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Eingeladener Vortrag
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Hydrogen-assisted cracking (HAC) represents a significant failure risk for (high strength) creep resistant low-alloyed steel components in fossil-fired power plant applications at temperatures of up to and above 200 °C. This particularly applies to respective start-up and shut-down processes associated with alternating service-conditions in terms of load flexible power plants. For quantitative determination of localized crack critical hydrogen concentrations, the temperature dependent hydrogen diffusion coefficients have to be determined as exactly as possible.
However, available literature provides a wide range of hydrogen diffusion coefficients for low alloyed steels with similar microstructures. Additionally, the available diffusion data seem not to be very reliable and their scatter increases with decreasing temperature. One reason is that the experimental boundary conditions can have a major impact on the determination of respective effective diffusion coefficients. Hence, the scope of this study is to evaluate the influence of the experimental boundary conditions on the derived diffusion coefficients. In addition, different methods for calculating diffusion coefficients are discussed. To elucidate such influences and to draw a line to practical application, the diffusion and trapping behavior in the creep resistant steel 7CrMoVTiB10 10 has been studied.
For such purpose, hydrogen charged specimens were isothermally degassed at different temperatures using carrier gas hot extraction (CGHE). Based on experimental data, a numerical model has been developed by which the hydrogen transport behavior and the respective hydrogen distribution during CGHE can be assessed.
It is demonstrated that the specimen heating rate has a large influence on the calculated diffusion coefficients under assumption of isothermal degassing which elsewhere has been underestimated in the assessment of diffusion data in creep-resistant steels. The numerical results suggest that calculation methods for diffusion coefficients are limited if compared to experimental results. It also turned out that the sample preparation time before CGHE can enormously influence determined diffusion coefficients. Consequently, non-homogeneous hydrogen concentration profiles have to be anticipated in the simulations to arrive at characteristic effusion curves consistent to respective CGHE experiments. In turn, validated diffusion coefficients are now available for the low-alloyed Cr-Mo-V steel which might be helpful to calculate appropriate hydrogen removal heat treatment procedures, for instance.
Modeling of Hydrogen-Assisted Cracking (HAC) in Duplex Stainless Steels (DSS):
- Hydrogen causes significant degradation in DSS and consequently HAC
- Mechanisms of HAC have not been fully understood in two-phase microstructures
- Mesoscale numerical modeling for HAC in DSS was created, coupled to the macroscale, enabling simulation of HAC in both phases independent from predefined crack paths
Hydrogen-assisted cracking (HAC) represents a significant failure risk for (high strength) creep resistant low-alloyed steel components in fossil-fired power plant applications at temperatures of up to and above 200 °C. This particularly applies to respective start-up and shut-down processes associated with alternating service-conditions in terms of load flexible power plants. For quantitative determination of localized crack critical hydrogen concentrations, the temperature dependent hydrogen diffusion coefficients have to be determined as exactly as possible.
However, available literature provides a wide range of hydrogen diffusion coefficients for low alloyed steels with similar microstructures. Additionally, the available diffusion data seem not to be very reliable and their scatter increases with decreasing temperature. One reason is that the experimental boundary conditions can have a major impact on the determination of respective effective diffusion coefficients. Hence, the scope of this study is to evaluate the influence of the experimental boundary conditions on the derived diffusion coefficients. In addition, different methods for calculating diffusion coefficients are discussed. To elucidate such influences and to draw a line to practical application, the diffusion and trapping behavior in the creep resistant steel 7CrMoVTiB10 10 has been studied.
For such purpose, hydrogen charged specimens were isothermally degassed at different temperatures using carrier gas hot extraction (CGHE). Based on experimental data, a numerical model has been developed by which the hydrogen transport behavior and the respective hydrogen distribution during CGHE can be assessed.
It is demonstrated that the specimen heating rate has a large influence on the calculated diffusion coefficients under assumption of isothermal degassing which elsewhere has been underestimated in the assessment of diffusion data in creep-resistant steels. The numerical results suggest that calculation methods for diffusion coefficients are limited if compared to experimental results. It also turned out that the sample preparation time before CGHE can enormously influence determined diffusion coefficients. Consequently, non-homogeneous hydrogen concentration profiles have to be anticipated in the simulations to arrive at characteristic effusion curves consistent to respective CGHE experiments. In turn, validated diffusion coefficients are now available for the low-alloyed Cr-Mo-V steel, which can be helpful to calculate appropriate hydrogen removal heat treatment procedures.
The chemical industry has expressed great interest in using polyethylene terephthalate (PET) as material for packagings for the transport of dangerous goods. Due to the high strength and stiffness of PET, the wall thickness and weight of packagings can be reduced. This is a relevant cost factor. PET is a semi-crystalline thermoplast which is produced by polycondensation of terephthalic acid and ethylene glycol.
According to the European dangerous goods regulations RID and ADR, samples of PET design types of packagings for dangerous goods must be pre-stored with the original filling good for six months at 23°C, before the design type tests can be carried out. For packagings made of polyethylene (PE) tests to prove the stress cracking resistance by using laboratory methods are possible to reduce time and costs. Therefore, standard liquids, simulating the different types of damaging effects on PE are defined in RID and ADR. However, there is no information and research available about the damaging mechanisms on PET in comparison to PE, especially regarding to stress cracking resistance and test methods.
The aim of this work is to compare the stress cracking resistance of PE and PET with the Full Notch Creep Test (FNCT), which was developed by chemical industry and is described in the standards EN ISO 16101 and EN 15507. It was investigated whether testing specimens made of PE and PET with a full coplanar notch around the middle of the specimens show weakening after the impact of a tensile force in a wetting solution (Lutensol® FSA 10) at 50°C in a test device on the basis of the FNCT.
The test results confirmed the suitability of the method for eight PE grades. Unfortunately, this method couldn’t be used for PET because the specimens broke during notching. In addition the molding of the sheets and the following temper process for twelve hours are very time-consuming, and the specimens broke during notching due to the high brittleness of PET.
Another possibility to provide evidence of stress cracking resistance of PE packagings is laid down in BAM’s Dangerous Goods Rule BAM-GGR 015. This test was carried out with PE and PET bottles to compare both materials. Therefore 1l test bottles were filled with a 5% wetting solution and mounted with a clamping tool for 28 days at 40°C. Tensile test specimens were cut out afterwards from the middle of the bottles in the deformed areas. Tensile strength and breaking elongation of PE specimens were determined in comparison to the PET specimens. The tensile properties of the PET specimens couldn’t be determined due to the strength and the stiffness of the material.
In conclusion the only way to provide information about the stress cracking resistance of PET was to perform stacking tests. 1l bottles made of PE and PET were filled with a 5% wetting solution and stored with a stacking load for 28 days at 40°C according to EN ISO 16495. Design types of PE and PET both passed the stacking tests.
Deuterium permeation and cracking in duplex steels as viewed by ToF-SIMS and HR-SEM with data fusion
(2016)
Better understanding of hydrogen assisted degradation and trapping mecha-nisms requires sufficient imaging techniques for respective hydrogen-microstructure interaction studies, in particular with multi-phase metallic micro-structures [1]. The present work is focusing on the elucidation of deuterium be-havior in two austenitic-ferritic duplex stainless steels (DSS) under the assumption that deuterium behaves in many ways similarly to hydrogen [2]. For case studies standard 2205 and lean 2101 DSSs were chosen due to the extensive use of these steels in industry [3]. The analyses were conducted by using a novel in-situ permeation and Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) imaging technique or by ex-situ ToF-SIMS imaging following electrochemical charging experiments. Another pioneering procedure was data fusion (including chemometry) of results of powerful laterally resolved chemical analysis and high resolution structural characterization techniques .
Results for the ex-situ observations showed a different influence of deuterium loading on the two steel grades as well as different damage mechanisms in each phase. Formation of sub-surface blisters between the ferrite and austenite were obtained in both the standard and the lean DSS. In both steels, an increased deuterium concentration was observed around deformed regions such as cracks, confirming that they originate from the presence of deuterium [4]. The formation of parallel cracks was obtained only in the austenite within the standard duplex whereas in the lean duplex the highest intensity of deuterium was obtained in the austenite along the ferrite-austenite interphase.
In comparison, application of the novel in-situ permeation technique enabled to register and record the deuterium permeation through the material and the respective saturation sequence of the two phases as well as the interfaces. Faster diffusion of the deuterium was observed in the ferrite and a direct proof for deuterium enrichment at the austenite-ferrite interface has been given [1]. The integration of the specified techniques gives a better insight into the processes leading to hydrogen induced failure. These two experimental techniques provide very valuable tools for elucidation of respective metallurgical failure mechanisms that can be used for the validation of respective numerical models for hydrogen assisted cracking (HAC).
A test campaign was launched to determine the mechanical properties of the HL-LHC 11 T Nb3Sn magnet components in order to accurately model the mechanical properties in Finite Element simulations that predict the stress and strain distribution in These magnets. Static and dynamic test methods have been applied for determining elastic materials behavior, and highly accurate Young’s moduli are obtained with the dynamic methods resonance and impulse excitation. These non-destructive methods also enable temperature dependent modulus measurements during in situ heat cycles.
In the presentation different zinc coatings are presented and investigated. Their naturally formed protective layers are electrochemically characterized and corrosion relevant values are determined by using a gel pad based on polysaccharide. The corrosion relevant values allow the differentiation of various zinc coating systems and can describe the current protective effect provided by the coating. It is shown that gel-type electrolytes influence protective layers and coatings considerably less than corresponding bulk electrolytes. From the results it is evident that gel-type electrolytes represent a viable and promising field in corrosion research.zeige mehr
Bei der Bewertung der Verlässlichkeit der im Labor gewonnenen Prüfergebnisse spielen Ringversuche eine entscheidende Rolle. Die Bundesanstalt für Materialforschung und -prüfung (BAM) unterstützt deshalb den weiteren Ausbau des Ringversuchsprogramms des im Jahr 2007 gegründeten Kompetenzzentrums zur Qualitätssicherung für Prüfungen von Gefahrgütern und Gefahrstoffen auf physikalische Gefahren (Centre for quality assurance for testing of dangerous goods and hazardous substances, CEQAT-DGHS).
Bei allen bisher untersuchten Prüfmethoden besteht ein Verbesserungsbedarf. Die RV müssen daher zunächst auf die Methodenentwicklung, -verbesserung und -validierung abzielen und nicht auf Leistungstests.
Ermüdungsverhalten, Lebensdauer und Schädigungsprozesse von P92 unter zyklischen Betriebsbedingungen
(2016)
Schnelle Lastwechsel mit hohen Temperaturgradienten führen zu thermischen und mechanischen Beanspruchungen v.a. in dickwandigen Bauteilen. Daraus ergibt sich ein komplexes Lastkollektiv, bei dem der Werkstoff sowohl durch Kriechermüdung als auch durch thermomechanische Ermüdung (TMF) geschädigt wird. Welche Auswirkungen hat eine gleichzeitige Änderung von Temperatur, mechanischer Beanspruchung und Arbeitsmedium auf die Schädigungsprozesse?
Application of 4Q-BSE detector and dedicated software enables 3D surface measurements of fracture samples in SEM. 3D surface measurement is independent from magnification and material invariant. Quantitative height measurements require careful detector adjustment and system calibration. Live 3D view allows a fast assessment of topographical features. In addition to SE and BSE imaging, 3D surface data help to analyse and interpret fracture samples.
In order to reduce CO2 emissions fossil fuelled power stations with high combustion efficiency are being developed. The increase of the operating temperature, a common way to improve combustion efficiency, leads to enhanced corrosion of heat exchange steel tubes in the power plants. Within the framework of the European project “Production of Coatings for New Efficient and Clean Coal Power Plant Materials” (POEMA)", high temperature corrosion protection coatings are now under investigation.
Thin porous sol-gel alumina films are promising candidate coating materials. Coatings were prepared by applying boehmite sols on grinded steel P92 and subsequent heat treatments at temperatures up to 650 °C. Thus a porous layer of worm-like particles was formed consisting of nano-crystallites and amorphous alumina. A dense interface with satisfying adhesion resulted from diffusion of chromium and iron ions out of the steel into the porous coating. However, the film locally exhibited some cracks caused by steep edges in the grinded steel surface. An appropriate substrate pretreatment should avoid this problem.
The protection of the steel relies on the barrier function of the alumina coating and the formation of a dense chromia layer at the steel surface.
We investigated the efficiency of phase gratings, i.e., the visibility upon variation of different parameters. Rotating around an axis parallel to the grid lines of the phase grating changes the grating’s shape and thereby the initial distribution of phase shifts. This yields high visibilities for shorter propagation distances than derived from box shapes. Tilting the grating in the scattering plane allows continuous tuning of the grating’s height that corresponds to an ideal phase shift for a particular photon energy. This opens the way for tuning the design energy suitable for the material under investigation. Our study included simulations for monochromatic sources with the sampling procedure for rectangular and triangular phase gratings.
In this study a metal-matrix-composite with aluminum matrix and Al2O3 particles was investigated with x-ray refraction topography and in-situ tensile loading. It could be observed that after reaching a certain load the specific surface increased steadily. However, the classical radiographs taken for comparison show no damage in the sample.
We investigated the efficiency of phase gratings, i.e., the visibility upon variation of different parameters. Rotating around an axis parallel to the grid lines of the phase grating changes the grating’s shape and thereby the initial distribution of phase shifts. This yields high visibilities for shorter propagation distances than derived from box shapes. Tilting the grating in the scattering plane allows continuous tuning of the grating’s height that corresponds to an ideal phase shift for a particular photon energy. This opens the way for tuning the design energy suitable for the material under investigation. Our study included simulations for monochromatic sources with the sampling procedure for rectangular and triangular phase gratings.
One of the alternative renewable fuels is biomass but it is a difficult fuel because of its diversity and complexity. It can contain high percentages of K and Cl responsible for corrosion together with sand that have additionally an abrasive effect during combustion. Because of permanently extending the surface reaction due to abrasion the corrosion of the materials increases. In particular in power plants, the superheater tubes are exposed to a corrosive abrasive attack that is one of the main sources of concern. The development of new alloys for multilayer surface, which combines corrosive and abrasive resistance is therefore of high importance. Those new technical approaches must be at the same time cost-effective to be an alternative to conventional materials. The aim of the presented investigation methods is to test and develop suitable alloys for coatings for the super heater tubes of biomass power plants. First results of abrasion investigations show improved abrasion resistance compared to the multi-component reference material Alloy 625.
Microbial induced corrosion (MIC) is a crucial problem in many technical plants as well as fuel tanks, leading to considerable damage and huge financial losses. Successful prevention of MIC requires the localization of first signs of corrosion as well as the identification of factors influencing the corrosion process. In this respect, also the determination of corrosion rates can be of interest for the possible prevention of MIC. Hence, there is a growing need for sensitive and preferably inexpensive tools that enable the early detection of MIC. Of special interest are methods, which provide spatially and time-resolved information and allow the study of changes on metal surfaces as prerequisites for a more detailed analysis of ongoing corrosion processes at a MIC-affected site.
Biofilm formation can lead to changes in pH, oxygen and chloride concentration as well as to the release of certain metal ions like Fe(II) and Mn(II) depending on the type of metal surface involved. Hence, optical methods enabling the detection of these analytes at very low concentration and monitoring of their changes can be used for MIC detection. Here, we propose to utilize polymeric nanosensors for MIC detection via the determination of the local pH value changes in different biofilms. Such nanosensors are known to have several advantages in imaging applications such as intracellular pH measurements including the ease of doping or labeling with a multitude of analyte-responsive and inert dye molecules for the realization of a high analyte sensitivity and ratiometric sensing. Moreover, they can be surface functionalized with target-specific ligands e.g., lectins, for the specific binding to the outer surface of certain types of bacteria. In this respect, different polymer architectures will be studied to identify an optimal candidate in terms of imaging performance in conjunction with several classes of pH-responsive fluorescent dyes like cyanines, aza-BODIPYs, and xanthenes, utilizing different mechanism of signal generation such as photo-induced electron transfer or protonation-induced changes in the spectral position of absorption and emission spectra.
Hard materials consist of a hard phase embedded in a metallic binder. In order to achieve high toughness and strength, it is necessary to have a perfect mixing of hard phase and binder, which is mainly achieved by ball milling. Niobium carbide (NbC) has a high potential to substitute tungsten carbide as hard material.
The publication presents the development of stable homogeneous and de-agglomerated NbC-dispersions. To prevent agglomeration of the powder, stable suspensions were achieved by surface treatments with the dispersants (PD and HD), which resulted in a charge reversal from a negative to a positive zeta potential. This surface-modified powder guaranteed a stable re-dispersion in the binder suspension. Nickel powder was added as metallic binder. This suspension was suited for 3D-printing. The green samples could be sintered in vacuum or Argon atmosphere.