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The ferritic steel 13CrMo4-5 due to good properties with relation to attractive price is frequently use in power plants industry. According EN10028-2 this steel can be used up to 570 °C because of its creep behavior but its corrosion resistance limits the use frequently to lower temperatures, depending on gas temperature and slag formation. The corrosion test were performed in environment containing mixture of gases like: O2, COx, SOx and ashes, with elements e.g. Na, Cl, Ca, Si, C, Fe, Al. Exposure time was respectively 240 h, 1000 h and 4500 h in temperature 600 °C. The oxide scale on the 13CrMo4-5 steel was significant thicker than for In686 coating and the difference increase according for longer exposure time.
The microstructure, chemical and phase composition of the oxide scales were investigated by means of a light microscope, the electron scanning and transmission microscopes (SEM,TEM) equipped with the EDS detectors.
Introduction/purpose:
Multi-principal-element alloys (MPEAs), also known as complex concentrated alloys (CCAs), have recently come to the attention of the scientific community due to some interesting and unexpected microstructures, and their potential for improving properties such as, e.g. mechanical strength and oxidation resistance in high temperature structural applications. The AlMo0.5NbTa0.5TiZr refractory (r)CCA is one such candidate, showing a two-phase microstructure after a two-stage heat treatment under argon atmosphere at a controlled cooling rate. Since the application conditions intended for this alloy require a long-term high temperature (> 700 °C) mechanical and oxidation resistance, it becomes necessary to assess the possible phase development in this regime.
Methods:
In this contribution, the CALPHAD method is used to calculate phase equilibria for the AlMo0.5NbTa0.5TiZr CCA in the presence and absence of oxygen. Equilibrium phase amount evolution with temperature and Scheil Model for solidification (e.g. Fig.1a and Fig.1b, respectively) are analyzed, which are obtained using the databases TCNI9 and TTNI7 and the Gibbs energy minimizer in the Thermo-Calc software.
Results:
The diagrams reveal that two BCC-based phases could form during alloy solidification, where one phase would be enriched with Mo, Nb and Ta while the other phase, with Al, Ti and Zr. Activity oxides diagrams show that a stable form of aluminum oxide (α-Al2O3, Pearson symbol: hR10, corundum) can be formed. Results obtained by both databases, as well as discrepancies between property phase and Scheil approaches are discussed on the base of experimental results.
Conclusions:
A modeling tool is used to support alloy characterization and development, providing also the possibility to feedback information to improve existing thermodynamic databases.
Die Abbildung von Bruchflächen im REM liefert hochaufgelöste Bilddaten, die für die mikrofraktografische Bewertung von Bruchmechanismen unerlässlich sind. Durch den Abbildungsprozess im REM gehen räumliche Informationen im Normalfall größtenteils verloren. Mit der Verwendung eines segmentierten Rückstreudetektors ist dagegen die Erzeugung eines 3D-Oberflächenmodells während der Bildaufnahme praktisch in Echtzeit möglich. Die hier beschriebene Untersuchung soll die Anwendbarkeit des Verfahrens auf Bruchflächen zeigen. Zukünftig können Topografiedaten dazu beitragen, Bruchflächen besser zu interpretieren.
3D coherence scanning interferometry (CSI) is anoptical, non-contact and rapide measurement technique using a defined bandwidth of white light at normal incidence. White light interference microscopy (WLIM) providest here-dimensional surface topometry data up to a resolution of 0.4 µm lateral and 0.1 nm vertical. Three operating modi, surface, films and advanced films, enable measurements of step heights, roughness, wear volume, cone angle, surface pattern and layer thickness. Traceability to SI system is ensured by certified standards (PTB/NIST) within a DAkkS DIN EN ISO/IEC 17025:2018 accredited lab.
Characterization of early crystallization stages in surface-crystallized diopside glass-ceramics
(2019)
Structure formation in glass-ceramics by means of surface crystallization is a challenging open question and remains elusive to definite answers. In several glass-ceramic systems, oriented crystal layers have been observed at the immediate surface, including diopside and some fresnoite systems. However, it is still open to debate, whether oriented surface crystallization is the result of oriented nucleation or growth selection effects. In the same vein, there is still discussion whether surface nucleation is governed by surface chemistry effects or by defects serving as active nucleation sites.
In order to help answer these questions, annealing experiments at 850°C have been performed on a MgO·CaO·2SiO2 glass, leading to the crystallization of diopside at the surface. Different annealing durations and surface treatment protocols (i.a. lapping with diamond slurries between 16 µm and 1 µm grain size) have been applied. Particular focus has been put on earliest crystallization stages, with crystal sizes down to about 200 nm. The resultant microstructure has been analyzed by electron backscatter diffraction (EBSD) and two different kinds of textures have been observed, with the a- or b-axis being perpendicular to the sample surface and the c-axis lying in the sample plane. Even at shortest annealing durations, a clear texture was present in the samples. Additionally, selected samples have been investigated with energy-dispersive x-ray spectroscopy in the scanning transmission electron microscope (STEM-EDX). The diopside crystals have been found to exhibit distinguished submicron structure variations and the glass around the crystals was shown to be depleted of Mg.
Fresnoite glass with excess SiO2 exhibits oriented surface crystallization, in contrast to the stoichiometric glass composition. Recent EBSD studies documented that the crystals in BTS (2BaO-TiO2-xSiO2, x=0-3) can occur in a distinct [101]-orientation perpendicular to the surface and claimed that this orientation is not a result of growth selection. During these previous studies, however, the effect of surface preparation and surrounding atmosphere during the crystallization experiments were not considered. As these parameters may influence crystal orientation, we studied the surface crystallization of a BTS glass (2BaO-TiO2–2.75SiO2) under controlled conditions with the help of light, electron and polarisation microscopy as well as EBSD. Heat treatments for one hour at 840°C of fractured BTS glass surfaces in air resulted in a large number of not-separable surface crystals. This large number of crystals can be caused by dust particles, which act as nucleation agents. As crystal growth velocity could further be influenced by humidity, our experiments are performed in a filtered and dried air atmosphere. The crystal morphology and orientation will be analysed in dependence of the sample preparation and a differing surrounding atmosphere.
The characteristics of TiO2 coatings can greatly influence their final performance in large-scale applications. In the present study self-assembly of TiO2 nanoparticles (NPs) in multiple layers was selected as a deposition procedure on various substrates. For this, the main prerequisite constitutes the surface modification of both NPs and substrate with e.g. silane coupling agents. A set of functionalized TiO2 NPs has been produced by reaction with either (3- aminopropyl)triethoxysilane (APTES) or (3-aminopropyl)phosphonic acid (APPA) to functionalize the NP surface with free amino-groups. Then, the complementary functionalized NP set can be obtained from an aliquot of the first one, through the conversion of free surface amino-groups to aldehydes by reaction with glutaraldehyde (GA). Several types of TiO2 NPs differing in size, shape and specific surface area have been functionalized. FTIR, TGA, SEM/EDS, XPS, Auger electron spectroscopy (AES) and ToF-SIMS analyses have been carried out to evaluate the degree of functionalization, all the analytical methods employed demonstrating successful functionalization of TiO2 NP surface with APTES or APPA and GA.
Using non-optimum combination of manufacturing parameters in selective laser melting (SLM) may lead to reduction of quality of component: defects generation, distortion of geometry and even cracking. Usually, the optimization of parameters is performed by changing volumetric energy density (Ev) and selecting parameters giving low porosity values. However, not only low porosity but also stable microstructure and low residual stresses will help to achieve advanced mechanical behavior of the component.
In present work, we investigated cuboid-shaped Ti-6Al-4V samples produced with different manufacturing parameters. The parameters leading to the same Ev were considered as well as parameters which are not included in Ev. Residual stresses in subsurface region were investigated by synchrotron X-ray diffraction, which allows to penetrate around 100 µm from the surface therefore overcome the problem of high roughness of SLM components without additional sample preparation. Only tensile stresses were found along the building direction, that can play critical role especially during cyclic loading. The pore shape and spatial distribution obtained by computed tomography varied for samples produced with the same Ev. However, by using some process parameters it was possible to decrease residual stresses and obtain uniform α+β Ti microstructure and relatively low porosity. Additionally, it was found that not included in Ev (e.g., base plate position, focus distance) should be considered as additional manufacturing parameters during SLM process.
Chromia forming high alloyed ferritic-austenitic steels are being used as boiler tube materials in biomass and coal-biomass co-fired power plants. Despite thermodynamic and kinetic boundary conditions, microstructural features such as grain orientation, grain sizes or surface deformation contribute to the oxidation resistance and formation of protective chromium-rich oxide layers. This study elucidates the impact of microstructure such as the grain size and number of carbide precipitates on high temperature oxidation at 650°C in 0.5% SO2 atmosphere. Cold-rolled Fe-16Cr-0.2C material was heat-treated to obtain two additional microstructures. After exposure to hot and reactive gases for 10 h < t < 1000 h layer thicknesses and microstructure of oxide scales are observed by scanning electron microscopy and Energy-dispersive X-ray spectroscopy. The two heat treated alloys showed reasonable oxidation resistance after 1000 h of exposure. The oxidation rate was substantially higher for the alloy with a duplex matrix after heat treatment compared to the fine-grained material.
Toxicological studies have shown that some types of carbon nanotubes may provoke asbestos-like effects including chronic inflammation and lung cancer. Inhaled carbon nanotubes may reach the deep lung tissue. Alveolar macrophages are responsible to remove such foreign objects from the alveoli in a process called phagocytosis. If a macrophage fails to uptake a nanotube completely, cell lesions may give rise to inflammation. It is currently assumed that short, flexible and long as well as granularly agglomerated (tangled) nanofibres are clearable by macrophages, whereas biodurable long and rigid nanotubes may persist in lung tissue. The flexural rigidity of nanofibres is therefore believed to be an important material property that governs fibre toxicity and needs to be investigated. The present work aims at determining the rigidity of nanofibres by detecting their resonance frequencies using a Dynamic Scanning Electron Microscope (DySEM) setup. By depositing and fixing a nanofibre to an oscillating support, it can be excited to vibrations and treated as a cantilevered beam. This way, its elastic modulus can be determined via Euler-Bernoulli’s beam theory. Multi-walled carbon nanotubes (MWCNTs) were deposited on high frequency piezoelectric quartz crystals mounted on a scanning electron microscope (SEM) holder. When introduced into the SEM chamber and connected to a frequency-sweeping waveform generator, the quartz crystal actuates the deposited fibre. A lock-in amplified processes the secondary electron detector signal resulting from the electron beam modulated by the vibrating nanofibre. Whenever a fibre resonance is detected, the SEM image of the fibre is stored to identify the fibre oscillation mode. The found resonance frequencies and modes allow determining the elastic modulus accordingly. Since the frequency spacing of resonances is predicted by Euler-Bernoulli, the mode number can be identified and elastic modulus values be averaged. A significant number of individual MWCNTs were classified according to their level of rigidity. The applicability and reliability of the method will be discussed.
Toxicological studies have shown that some types of carbon nanotubes may provoke asbestos-like effects including chronic inflammation and lung cancer. Inhaled carbon nanotubes may reach the deep lung tissue. Alveolar macrophages are responsible to remove such foreign objects from the alveoli in a process called phagocytosis. If a macrophage fails to uptake a nanotube completely, cell lesions may give rise to inflammation. It is currently assumed that short, flexible and long as well as granularly agglomerated (tangled) nanofibres are clearable by macrophages, whereas biodurable long and rigid nanotubes may persist in lung tissue. The flexural rigidity of nanofibres is therefore believed to be an important material property that governs fibre toxicity and needs to be investigated. The present work aims at determining the rigidity of nanofibres by detecting their resonance frequencies using a Dynamic Scanning Electron Microscope (DySEM) setup. By depositing and fixing a nanofibre to an oscillating support, it can be excited to vibrations and treated as a cantilevered beam. This way, its elastic modulus can be determined via Euler-Bernoulli’s beam theory. Multi-walled carbon nanotubes (MWCNTs) were deposited on high frequency piezoelectric quartz crystals mounted on a scanning electron microscope (SEM) holder. When introduced into the SEM chamber and connected to a frequency-sweeping waveform generator, the quartz crystal actuates the deposited fibre. A lock-in amplified processes the secondary electron detector signal resulting from the electron beam modulated by the vibrating nanofibre. Whenever a fibre resonance is detected, the SEM image of the fibre is stored to identify the fibre oscillation mode. The found resonance frequencies and modes allow determining the elastic modulus accordingly. Since the frequency spacing of resonances is predicted by Euler-Bernoulli, the mode number can be identified and elastic modulus values be averaged. A significant number of individual MWCNTs were classified according to their level of rigidity. The applicability and reliability of the method will be discussed.
Toxicological studies have shown that some types of carbon nanotubes may provoke asbestos-like effects including chronic inflammation and lung cancer. Inhaled carbon nanotubes may reach the deep lung tissue. Alveolar macrophages are responsible to remove such foreign objects from the alveoli in a process called phagocytosis. If a macrophage fails to uptake a nanotube completely, cell lesions give rise to inflammation. It is currently assumed that short, long and flexible, and granularly agglomerated (tangled) nanofibres are clearable by macrophages, whereas biodurable long and rigid nanotubes persist in the lung tissue. The flexural rigidity of nanofibres is therefore believed to an important material property that governs fibre toxicity and needs to be investigated. The present work aims at determining the rigidity of nanofibres by detecting their resonance frequencies using a Dynamic Scanning Electron Microscope (DySEM) setup. By depositing and fixing a nanofibre to an oscillating support, it can be excited to vibrations and treated as a cantilevered beam. This way, its elastic modulus can be determined via Euler-Bernoulli’s beam theory. Multi-walled carbon nanotubes (MWCNTs) were deposited on high frequency piezoelectric quartz crystals mounted on a scanning electron microscope (SEM) holder. When introduced into the SEM chamber and connected to a frequency-sweeping waveform generator, the quartz crystal actuates the deposited fibre. A lock-in amplified processes the secondary electron detector signal resulting from the electron beam modulated by the vibrating nanofibre. Whenever a fibre resonance is detected, the SEM image of the fibre is stored to identify the fibre oscillation mode. The found resonance frequencies and modes allow determining the elastic modulus according. Since the frequency spacing of resonances is predicted by Euler-Bernoulli, the mode number can be checked and elastic modulus values be averaged. A significant number of MWCNTs have been classified according to their level of rigidity. The applicability and reliability of the method will be discussed.
Quality Aspects of Additively Manufactured Medical Implants - Defect Detection in Lattice Parts
(2019)
Additive Manufacturing technologies are developing fast to enable a rapid and flexible production of parts. Tailoring products to individual needs is a big advantage of this technology, which makes it of special interest for the medical device industry and the direct manufacturing of final products. Due to the fast development, standards to assure reliability of the AM process and quality of the printed products are often lacking. The EU project Metrology for Additively Manufactured Medical Implants (MetAMMI) is aiming to fill this gap by investigating alternative and cost efficient non-destructive measurement methods.
Water as side effect of reinforcing boehmite filler Local changes in anhydride cured epoxy resin
(2019)
Nanocomposites offer wide opportunities for lightweight constructions and enable reduction of weight and volume. Beside macroscopic toughening nanoparticle reinforced polymers show a soft interface around boehmite (AlOOH) filler nanoparticles. A related strong interaction between boehmite and the anhydride cured resin system is widely suspected in literature but not determined by structural Analysis. Determination of the molecular structure is important to allow simulations approaching the real system and predict future reinforcing effects.
DRIFT (diffuse refletance infrared fourier transformed) spectra of the boehmite reinforced anhydride cured epoxy show significant changes in the molecular structure compared to the neat polymer. Further investigations of the interactions between the single components of the resin system and the boehmite filler pointed out reactions between released water released from the boehmite filler and the anhydride hardener or amine accelerator. This leads to the discussion of competing polymerisation mechanisms that highly influence the polymer properties. Ongoing experiments and literature research approve that this impact of water is able to locally change the stoichiometrie, alter the curing mechanism or support an inhomogeneous crosslink density.
Heating oil storage tanks made of polyethylene grades have been on the market in Germany since the early 1970s. To ensure safety, their replacement is recommended by tank manufacturers after a period of 30 years. Polyethylene is subject to ageing by alteration of the properties during its life cycle. The degree of degradation and the nature of the process mainly depend on the chemical alteration of the polyethylene, the wall thickness of the tank and the environmental conditions. There are no data available on the long-term behaviour of the polyethylene grades, especially after a service life of more than 30 years.
The aim of this investigation was to find a suitable test method to determine the factual degree of damage in comparison to the uncontaminated polyethylene grades. Material data of the used polyethylene grades are available because the BAM was the competent authority for the tests and expert reports for the approval of these tanks until the middle of the 1990s. Therefore, tank sections from the bottom, the shell and the roof of 22 individual storage tanks produced of polyethylene grades A and B have been examined by Melt Flow Rate (MFR) and Attenuated Total Reflectance (ATR). Their service life was in the range between 20 and 41 years.
The MFR measurements of the tank sections showed differences in the values depending on the weight which was used (5 kg or 21.6 kg). An increase of the MFR was determined for the samples of polyethylene grade A, whereas a reduction of the MFR values was measured for most samples of polyethylene grade B. This grade is mainly subject to the internal ageing by cross-linkages, increased degree of branched molecules and loss of the plasticizer.
ATR analysis exhibits an absorption band at 909 cm‒1 predominantly in samples of polyethylene grade A indicating chain scission and concomitantly formed terminal vinyl groups. This absorption band can be used for the characterization of the ageing of the polyethylene grades.
TIG welding process was monitored using LIBS for the in situ measurement of chemical compositions in austenitic stainless steels. This research aims to prototype a real-time chemical composition analysis system for welding applications and prove the feasibility of such a quality control loop.
The chemical compositions of the weld pool, considering the welding metallurgy, is the most critical parameter for any occurring weld defects, e.g. hot cracking. Hence, controlling the weld pool chemical composition allows governing of the weld pool solidification behavior by monitoring and adjusting the respective welding parameters, e.g. welding current.
LIBS measurements were conducted during a TIG-welding process. The effect of the welding plasma on the LIBS signal was thoroughly investigated by varying various LIBS settings, e.g. delay and exposure time. Quantification of the main alloying elements Cr and Ni in the weld pool during welding was achieved by univariate calibration procedure.
In special cases of angle beam ultrasonic measurement the applied transducer has to withstand extreme temperatures. Since the irradiation angle depends on the speed of sound in both the wedge material and the tested object, the developer must take into account the speed of Sound in a wedge material over the whole temperature range of transducers application.
In this joint project, standardized measurement methods for hybrid
mixtures are developed, which serve to determine safety
characteristics for explosion protection.
A hybrid mixture is a multi-phase System consisting of fuel gas or
vapor, as well as air and flammable dust. This combination can occur
for instance in drying processes or during heterogenous reaction
processes.
The influence of prestraining on the aging response of an Al-Cu-Li alloy is investigated by preparation of different strain states (3 %, 4 %, 6 %) of the initial aging state. The Brinell hardness of the subsequently aged samples (up to 60 h aging time) was measured and it was found that the increasing dislocation concentration in the 3 different initial states leads to faster hardness increases and slightly higher maximum hardness.