Ingenieurwissenschaften und zugeordnete Tätigkeiten
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Eingeladener Vortrag
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We report on the development of ultra-small core-shell silver nanoparticles synthesized by an up-scaled modification of the polyol process. It is foreseen to use these thoroughly characterized particles as reference material to compare the catalytic and biological properties of functionalized silver nanoparticles. Small-angle X-ray scattering (SAXS) analysis reveal a narrow size distribution of the silver cores with a mean radius of RC = 3.0 nm and a distribution width of 0.6 nm. Dynamic light scattering (DLS) provides a hydrodynamic radius of RH = 10.0 nm and a PDI of 0.09. The particles’ surface is covered with poly(acrylic acid) (PAA) forming a shell with a thickness of 7.0 nm, which provides colloidal stability lasting for more than six months at ambient conditions. The PAA can be easily exchanged by biomolecules to modify the surface functionality. Replacements of PAA with glutathione (GSH) and bovine serum albumin (BSA) have been performed as examples. We demonstrate that the particles effectively catalyze the reduction of 4-nitrophenol to 4-aminophenol with sodium borohydride. The tunable catalytic activity of (436 ± 24) L g-1 s-1 is the highest reported in literature for silver nanoparticles.
The implementation of new 2-D materials based technologies in production processes requires the development of quality management tools. These have to be underpinned by appropriate measurements. Consequently there is a need for the development of the metrology for measurement methods, the development of certified reference materials (CRM) and finally standardization. This chain represents the ideal way to practically useful standards. The presentation will give an overview on the main players in the field and summarize the recent status of activities. At the highest level the metrology of chemical characterization of 2D materials is in the scope of the International Meter Convention, specifically the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM). Pre-standardization is an activity field of the Versailles Project on Advanced Materials and Standards (VAMAS). Standardization is mainly addressed by addressed ISO Technical Committees. A summary on available CRMs relevant to the characterization of nano materials has been prepared by BAM. Examples from the work of BAM’s Division 6.1 “Surface Analysis and Interfacial Chemistry” showcasing the characterization of chemically modified graphene surfaces are given and specific needs for the development of metrology are addressed.
In the discussion the audience is invited to define specific needs which will be streamlined to the respective bodies!
Tribological profile of hydraulic oils by using SRV. The determination of a set of critical, tribological by using different SRV-based test methods. The SRV-based concept of tribological profile generates the wear volumes on two triboelements (specimen), the extreme pressure properties and friction under different contact pressures.
Thus, the benchmark and validation of hydraulic oils bear on a wider range of tribological properties.
The RR2016 extends with six hydraulic oils to other base oil types including biodegradable fluids, which were all tested according to ASTM D7043 in order to consolidate the correlation between SRV and V104C.
Actions from the meeting in April 2016: 1. Four SAC test methods are in place and were revised: SH/T 0721 (Grease, coefficient of friction and wear), SH/T 0784 (Grease, pass load/O.K. load), SH/T 0847 (Oil, coefficient of friction and wear) and SH/T 0882 released by 11-2014 (Oil, pass load/O.K. load). 2. New test method to evaluate anti-fretting properties of greases based was approved by SAC TC280 and will be released. 3. SAC TC280 accepted the project “Simulation of synchronizer by using SRV”. Draft text to be submitted by 03-2017. Discussions on a parallel ASTM test method. 4. A procedure for “Wear Volume” is under development for SAC TC280.
One-part-geopolymers, produced by addition of water to a mixture of solid silica and sodium alumi-nate, are a less exhaustively studied approach to form geopolymeric binders. Depending on the silica source, the reaction products show significant amounts of zeolite Na-A besides amorphous compounds. Previously, 29Si MAS NMR has been used to analyze the chemical structure of such one-part geopolymers, having crystalline structures and amorphous phases (Q2, Q3, Q4).
In this work, pure zeolites and three different one-part-geopolymers cured for 1 day were investigated by 29Si-27Al TRAPDOR NMR. It was used to identify aluminum phases in overlapping silicon sites. Zeolites Na-X (Si/Al=1.4) and Na-Y (Si/Al=2.7) served as model systems to measure the TRAPDOR effect of the structural units Q4(mAl). Both materials show several Q4(mAl) signals, which are all separated by their chemical shifts. The more aluminum surrounds the silicon tetrahedron the higher are the normalized TRAPDOR difference signals (S0/∆S). The intensity ratios between Q4(mAl) to Q4({m-1}Al) of these signals is fixed but vary slightly between both zeolites. These results are transferred to the complex geopolymer structure.
3D Charakterisierung wasserstoffunterstüzter Risse in Stahl mittels Synchrotron-Refraktions-CT
(2016)
Die Fehlertoleranz moderner hochfester Stähle gegenüber Prozessfehlern beim Fügen nimmt stetig ab und erfordert eine immer kritischere Beurteilung der Ergebnisse aus den vorhandenen Prüfverfahren. Deren Aussagekraft ist häufig zu gering und daher muss zum einen das wissenschaftliche Verständnis der Mikrokaltriss-Entstehung in diesen Stählen vertieft werden und zum anderen müssen die Prüfmethoden und Bewertungskriterien angepasst werden. Dies erfordert ein besseres Verständnis insbesondere der Kopplung von Eigenspannungen, Wasserstoffgehalten und der Wirkung äußerer Kräfte auf die Rissentstehung und das Risswachstum.
Erstmals soll mittels 3D-Synchrotron-Refraktions-Topographie an der BAMline am BESSY die Rissentstehung in mit Wasserstoff beladenen Zugproben charakterisiert werden. Diese Kenntnisse sollen in weiteren Untersuchungen auf Schweißnähte übertragen werden.
3D Crack analysis in hydrogen charged lean duplex stainless steel with synchrotron refraction CT
(2016)
Hydrogen in metals can cause a degradation of the mechanical properties, the so-called hydrogen embrittlement. In combination with internal stresses, hydrogen assisted cracking (HAC) can occur. This phenomenon is not completely understood yet. To better characterise the cracking behaviour, it is important to gain information about the evolution of the 3D crack network. For this purpose samples of lean duplex stainless steel were loaded with hydrogen by means of electrochemical charging and investigated by means of synchrotron refraction CT and SEM fractography after uniaxial tensile loading. Synchrotron refraction CT is an analyser-based imaging (ABI) technique. It uses a Si (111) single crystal as analyser, which is placed into the beam path between sample and detector. According to Bragg’s law only incident x-rays within a narrow range around the Bragg-angle are diffracted from the analyser into the detector. Hence, the analyser acts as an angular filter for the transmitted beam. This filtering allows to turn the refraction and scattering of x-rays into image contrast. Refraction occurs at all interfaces, where the density of the material changes and is more sensitive to density changes than the attenuation. Therefore, it is possible to detect smaller cracks than with classical x-ray imaging techniques, like CT, with comparable spacial resolution. It also visualises the 3D structure of the cracks and gains quantitative information about their morphology and distribution. Since cracks introduced by HAC are usually very small and have a small opening displacement, synchrotron refraction CT is expected to be well suited for imaging this cracking mechanism and can be a valuable tool to characterise the formation and the evolution of a 3D crack network.
Hydrogen in metals can cause a degradation of the mechanical properties, the so-called hydrogen embrittlement. In combination with internal stresses, hydrogen assisted cracking (HAC) can occur. This phenomenon is not completely understood yet. To better characterise the cracking behaviour, it is important to gain information about the evolution of the 3D crack network. For this purpose samples of lean duplex stainless steel were loaded with hydrogen by means of electrochemical charging and investigated by means of synchrotron refraction CT and SEM fractography after uniaxial tensile loading. Synchrotron refraction CT is an analyser-based imaging (ABI) technique. It uses a Si (111) single crystal as analyser, which is placed into the beam path between sample and detector. According to Bragg’s law only incident x-rays within a narrow range around the Bragg-angle are diffracted from the analyser into the detector. Hence, the analyser acts as an angular filter for the transmitted beam. This filtering allows to turn the refraction and scattering of x-rays into image contrast. Refraction occurs at all interfaces, where the density of the material changes and is more sensitive to density changes than the attenuation. Therefore, it is possible to detect smaller cracks than with classical x-ray imaging techniques, like CT, with comparable spacial resolution. It also visualises the 3D structure of the cracks and gains quantitative information about their morphology and distribution. Since cracks introduced by HAC are usually very small and have a small opening displacement, synchrotron refraction CT is expected to be well suited for imaging this cracking mechanism and can be a valuable tool to characterise the formation and the evolution of a 3D crack network.
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.
Components in the Aerospace, Power and Automotive engineering sectors are frequently subjected to cyclic stresses induced by thermal fluctuations and mechanical loads. For the design of such components, reliable material property data are required which need to be acquired using well accepted and reproducible test procedures for thermo-mechanical fatigue (TMF) loading. Available materials TMF property data are limited so that there is a need for further TMF data generated by TMF testing. The TMF behaviour of materials is often desired to be simulated in models which describe the cyclic stress-strain behaviour, the fatigue life and the cyclic crack growth behaviour. There is a continuous need for the development and amendment of such models. Models can be validated by using materials in industrial applications which are subjected to TMF loading.
The adsorption behavior of Platinum nanoparticles was studied for the as-received catalyst (under inert gas), under hydrogen and CO atmosphere using our newly designed in-situ cell. X-ray Absorption Spectroscopy (XAS) and Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS) experiments were performed simultaneously with high data quality. Structural information and the type of adsorbate could be revealed via Extended X-ray Absorption Fine Structure (EXAFS) analysis, Δμ X-ray Absorption Near Edge Structure analysis (Δμ XANES) and in-situ DRIFTS. The as-received catalyst showed sub-surface oxygen and O(n-fold). Under CO atmosphere only CO(atop) was found. Reversible adsorbate induced changes of the Pt nanoparticle structure were derived from changes in the Pt-Pt coordination number and the corresponding bond distance. Under reducing conditions (H2, CO) a significant increase in both values occurred. Temperature dependent desorption of CO revealed a gradual shift from Pt-CO to Pt-O. Reoxidation was clearly assigned to strong metal support interaction from the SiO2 support.
With increased usage of highly demanded, modern materials on safety
relevant parts (e.g. railway wheel sets, generator shafts, turbine disks, medical
implants, etc.) comprehensive analyses regarding the quality of the material are
requested. This gives a focus to non-destructive methods using ultrasound immersion
tank testing for classifying the degree of purity. Two autonomous standards,
ASTM E588 and SEP 1927, have been established for the definition, execution and
evaluation for this high resolution ultrasonic measurements on steel products.
The propagation of ultrasonic waves and the resulting sound field are strongly
dependent on the acoustical properties of the inspected material and the geometry
of probes and specimen. The definition of the measurement setup and the evaluation
methods appear to differ significantly in the given standards. ASTM E588 and
SEP 1927 prescribe the requirement for surface roughness and probe selection, are
using threshold based methods for cleanliness detection, but differ in computation
for the degree of purity. This has been the motivation for a comparison between
both standards with the main focus on amplitude depth dependency and overall spatial
resolution taking the influence of different material characteristics, geometry of
the specimen and sound fields into account.
A performance comparison between the use of non-focusing and focusing probes
respective to the threshold based detection will be presented in this contribution. In
addition, the usage of complex reconstruction algorithms (e.g. SAFT, echo tomography)
is compared with the traditional approaches of inclusion detection and
estimation of the degree of purity
Introducing a single silicon nanowire with a known orientation and dimensions to a specific layout location constitutes a major challenge. The challenge becomes even more formidable, if one chooses to realize the task in a monolithic fashion with an extreme topography, a characteristic of microsystems. The need for such a monolithic integration is fueled by the recent surge in the use of silicon nanowires as functional building blocks in various electromechanical and optoelectronic applications. This challenge is addressed in this work by introducing a top-down, silicon-on-insulator technology. The technology provides a pathway for obtaining well-controlled silicon nanowires along with microstructures up to a three-order-of-magnitude scale difference. A two-step etching process is developed, where the first shallow etch defines a nanoscale protrusion on the wafer surface. After applying a conformal protection on the protrusion, a deep etch step is carried out forming the surrounding microscale features. A minimum nanowire cross-section of 35 nm by 168 nm is demonstrated in the presence of an etch depth of 10 m. All cross-sectional features are characterized via transmission electron microscopy and linked to specific process steps. The technology allows control on all dimensional aspects along with the exact location and orientation of the silicon nanowire.
A few Aspects of the Current Understanding of DPF Materials Thermal and Mechanical Properties
(2016)
Bi-continuous porous ceramics for filtration applications possess a particularly complicated microstructure, whereby porosity and solid matter are intermingled. Moreover, they very often display a microcrack network, resulting from the strong anisotropy of the microscopic coefficient of thermal expansion (CTE). Mechanical, thermal, and filtration properties, they all strongly depend on the morphology of both solid matter and porosity, and on the degree of microcracking (also, the microcrack density), which is in its turn tightened to the grain size.
Recent industrial and academic research has enormously progressed in understanding the microstructure-property-performance relationships existing in these complicated materials:
- Using 3D computed tomography (CT) at different resolutions, and several X-ray refraction-based techniques, porosity and pore orientation could be quantitatively evaluated (in the example of cordierite).
- Neutron and X-ray Diffraction has been instrumental to disclose a) the non-linear character of the stress-strain response, and b) the negative CTE of these materials, and its consequences on the materials properties;
- Analytical and numerical models have been elaborated to rationalize these behaviours in terms of microcracking and microstructural features.
Here these results will be reviewed, and a outlook at (some of the) outstanding problems will be given.
A fast quantitative model for the energy spectra of radiation emitted by X-ray tubes is described, handling thin as well as thick plane targets of arbitrary materials. The developed model is based on fundamental interaction cross sections, describing electron and photon transport via numerical integration of discretized distributions. While the focus lies on bremsstrahlung production, modeling of characteristic radiation is fully integrated. The model does not include any free parameters. The validity of the model is shown through comparison with measurements and Monte Carlo simulations for several combinations of target material and acceleration potential between 30 kV and 450 kV.
In comparison to manual NDT methods, mechanized NDT is considered to be more reliable for a number of reasons, one of which being that the role of the inspectors and, therewith, the potential for human error, have been reduced. However, human-automation interaction research suggests that in spite of its numerous benefits, automation can lead to new yet unknown risks. One of those risks is inappropriate reliance on automation, which can result in automation misuse and disuse. The aim of this study was to investigate the potential inappropriate use of automation (specifically - the automated aids) in NDT addressing therewith the prevalent belief in the high reliability of automation held by the NDT community. To address this issue, 70 NDT trainees were asked to control the results of an eddy current data evaluation, allegedly provided by an automated aid, i.e. indication detection and sizing software. Seven errors were implemented into the task and it was measured to what extent the participants agreed with the aid. The results revealed signs of both misuse (agreeing with the aid even though it is incorrect) and disuse (disagreeing with the aid even though it is correct) of the aid that can affect the reliability with which inspections are carried out. Whereas misuse could be explained by a lower propensity to take risks and by a decreased verification behaviour-possibly due to bias towards automation and complacent behaviour-, disuse was assigned to problems in establishing the sizing criterion or to general difficulties in sizing. The implications of these results for the NDT praxis including suggestions for the decrease of automation bias are discussed.
The repair of earthen structures is not an easy task. Earth as a construction material has comparatively weak mechanical properties. It is also susceptible towards liquid water, were it can lose cohesion very quickly if certain moisture contents are exceeded. Repair concepts of structures built with such materials are therefore challenging. Historical earthen structures often exhibit damages in form of extensive cracking, which may have been caused by static or dynamic loads. Frequently these cracks are insufficiently or inappropriately repaired because of lack of knowledge and / or technology. In particular, the behaviour of crack repair by grouting poses a challenge in earthen materials and demands specific requirements for the grouting mortar, such as low water content, good water retention, low shrinkage. Grouting materials require additional specifications such as compatible strengths and Young’s modulus as well as good adhesion to the earthen substrates. In addition, grouts have to be sufficiently flowable to fill small cracks and voids without segregation or bleeding. Therefore, the rheological behaviour has to be well understood and controlled to gain the desired effects.The repair of cracks in earthen buildings is traditionally done by stuffing manually mortar into the gap. Naturally, this method is only usable for cracks with large widths. Another disadvantage is that cracks going through thicker walls cannot be completely reached by the tools used for stuffing the mortar into the crack. Lime based grouts for earthen materials were usually used for re-attachment of plasters but less for structural reasons.Due to the nature of earthen materials grouts based on formulated or hydraulic lime (according to the definition in EN 459-1) have to meet considerable demands on a variety of properties, which are related to compatibility, durability and in particular to the ability of being injected. The goal of this study was to create a grout, which can be used to re-establish structural continuity in cracked earthen masonry or other massive earth walls (rammed earth and cob) with the focus on grouting cracks. The grout material was based on hydrated lime (calcium hydroxide) with additions of pozzolana and lime stone filler.
The repair of earthen structures is not an easy task. Earth as a construction material has comparatively weak mechanical properties. It is also susceptible towards liquid water, were it can lose cohesion very quickly if certain moisture contents are exceeded. Repair concepts of structures built with such materials are therefore challenging. Historical earthen structures often exhibit damages in form of extensive cracking, which may have been caused by static or dynamic loads. Frequently these cracks are insufficiently or inappropriately repaired because of lack of knowledge and / or technology. In particular, the behaviour of crack repair by grouting poses a challenge in earthen materials and demands specific requirements for the grouting mortar, such as low water content, good water retention, low shrinkage. Grouting materials require additional specifications such as compatible strengths and Young’s modulus as well as good adhesion to the earthen substrates. In addition, grouts have to be sufficiently flowable to fill small cracks and voids without segregation or bleeding. Therefore, the rheological behaviour has to be well understood and controlled to gain the desired effects.
The repair of cracks in earthen buildings is traditionally done by stuffing manually mortar into the gap. Naturally, this method is only usable for cracks with large widths. Another disadvantage is that cracks going through thicker walls cannot be completely reached by the tools used for stuffing the mortar into the crack. Lime based grouts for earthen materials were usually used for re-attachment of plasters but less for structural reasons. Due to the nature of earthen materials grouts based on formulated or hydraulic lime (according to the definition in EN 459-1) have to meet considerable demands on a variety of properties, which are related to compatibility, durability and in particular to the ability of being injected. The goal of this study was to create a grout, which can be used to re-establish structural continuity in cracked earthen masonry or other massive earth walls (rammed earth and cob) with the focus on grouting cracks. The grout material was based on hydrated lime (calcium hydroxide) with additions of pozzolana and lime stone filler.
Strain hardening ultra high performance fibre reinforced cementitious composites (UH-PFRCC) exhibit increased strength, ductility, and energy absorption capacity when compared to their quasi-brittle, unreinforced counterparts. A mesoscale finite element model can depict the underlying causes for the structural response of UHPFRC and thus help to optimize the fibre content, the fibre dimensions, and the fibre orientation.
Furthermore, it facilitates the investigation of strain rate effects in UHPFRCC under dynamic loading. The mesoscale model can either be used directly or as a representative volume element for a macroscale model.
This work proposes a two-dimensional and a three- dimensional mesoscale finite element model to simulate the structural response of strain hardening UHPFRCC. The mesoscale model employs an implicit gradient enhanced damage model, proposed by Peerlings et al., for the cement matrix and a local bond stress-slip model, proposed by Elige-hausen, Popov, and Bertero, for the bond between the cement matrix and the steel fibres. The steel fibres are modeled discretely as one-dimensional truss elements that are coupled to the cement matrix via bond elements. The implementation of hooked end fibres is realized in the constitutive equations of the bond elements.
The tensile stress-strain response of UHPFRCC is a consequence of local matrix cracking and bond failure. Both phenomena can be depicted when modeling the cement matrix, the steel fibres, and the fibre-to-matrix bond explicitly. In this work, the parameters for the constitutive equations of each constituent are determined through uniaxial Tension tests, bending tests, and fibre pullout tests. Additionally, UHPFRCC specimens are simulated with the same parameters and compared to experimental results.
A Multi-scale temporal integration scheme for viscoplatic solids subjected to fatigue deterioration
(2016)
Using a continuum mechanics framework for lifetime prediction requires numerical integration of evolving damage until the onset of failure. The primary challenge for the simulation of structural fatigue failure is caused by the enormous computational costs due to cycle by cycle temporal integration throughout the whole loading history, which is in the order of 10^3 - 10^7 cycles. As a consequence, most approaches circumvent this problem and use an empirical method such as Wöhler curves. They are well suited for approximation of the lifetime, but they are not capable to capture a realistic degradation of the material with a redistribution of the stresses. The main objective of the paper is to provide a technique for the long time response of a finite element (FE) model while reducing computational costs.
A multi-scale temporal integration scheme is proposed, which adapts the conventional FE method for realistic modeling of deterioration in a structure subjected to cyclic loading. For a particular case of two-scale temporal homogenization, the displacement field is assumed to satisfy scale separation: a short time scale arises from the oscillatory loading and a long time scale is due to the slow response relating to yielding and damage evolution. The original boundary value Problem (BVP) is approximated by the time-Independent BVPs on the short time scale. Alternation of the displacement field on the long time scale is correlated with the damage evolution by means of the adaptive cycle jump method. The significant acceleration of FE simulations is demonstrated for a constitutive damage model where the progressive damage accumulation under fatigue loading is driven by viscoplastic deformation.
A multiproxy approach to evaluate biocidal treatments on biodeteriorated majolica glazed tiles
(2016)
The Fishing House located on the grounds of the Marquis of Pombal Palace, Oeiras, Portugal, was built in the 18th century. During this epoch, Portuguese gardens, such as the one surrounding the Fishing House, were commonly ornamented with glazed wall tile claddings. Currently, some of these outdoor tile panels are covered with dark colored biofilms, contributing to undesirable aesthetic changes and eventually inducing chemical and physical damage to the tile surfaces. Phylogenetic analyses revealed that the investigated biofilms are mainly composed of green algae, cyanobacteria and dematiaceous fungi. With the aim of mitigating biodeterioration, four different biocides (TiO2 nanoparticles, Biotin® T, Preventol® RI 80 and Albilex Biostat®) were applied in situ to the glazed wall tiles. Their efficacy was monitored by visual examination, epifluorescence microscopy and DNA-based analysis. Significant changes in the microbial community composition were observed 4 months after treatment with Preventol® RI 80 and Biotin® T. Although the original community was inactivated after these treatments, an early stage of re-colonization was detected 6 months after the biocide application. TiO2 nanoparticles showed promising results due to their self-cleaning effect, causing the detachment of the biofilm from the tile surface, which remained clean 6 and even 24 months after biocide application.
A new tank design for Hazmat
(2016)
Initial studies have shown pre-deformed honeycomb structure
pressure vessels to have comparable burst pressure to straight steel vessels.
It was shown that honeycomp structured tanks have a higher energy absorption than straight steel tanks.
Future studies will investigate optimization of the deformed plate, to determine if increased payloads or a reduced wall thickness can be achieved.
In the last decades, numerical simulations of fresh concrete flow have gained importance in concrete industry. They showed a potential to become a tool for prediction of concrete casting and to help engineers to avoid expensive mistakes on site. A promising field for application of numerical modelling is casting of Self-Compacting Concrete (SCC), since the main area of application of SCC are complex and highly-reinforced building elements. Simulations of fresh concrete flow involve complex mathematical models and time-consuming computations. In case of casting simulations, the simulation time is additionally significantly increased because each reinforcement bar occurring in succession has to be considered one by one. This is particularly problematic in case of SCC casting, since this type of concrete is typically used for heavily-reinforced structural members. With the aim to decrease simulation time and to come closer to a practical simulation tool, we proposed an innovative modelling approach that models a zone with arrays of the reinforcement bars as a porous medium (PM). By defining characteristic parameters of the PM, its influence on the flow can be defined. This approach simplifies the geometry to be modelled and significantly decreases the computational time. The present contribution provides a brief description the proposed numerical model and of the conducted validation studies. The applicability of the model on fresh concrete is verified through the comparison between experimental measurements and numerical simulations.
An automatic sample changer chamber for total reflection X-ray fluorescence (TXRF) and X-ray absorption near-edge structure (XANES) analysis in TXRF geometry was successfully set up at the BAMline at BESSY II. TXRF and TXRF-XANES are valuable tools for elemental determination and speciation, especially where sample amounts are limited (<1 mg) and concentrations are low (ng ml⁻¹ to μg ml⁻¹). TXRF requires a well defined geometry regarding the reflecting surface of a sample carrier and the synchrotron beam. The newly installed chamber allows for reliable sample positioning, remote sample changing and evacuation of the fluorescence beam path. The chamber was successfully used showing accurate determination of elemental amounts in the certified reference material NISTwater 1640. Low limits of detection of less than 100 fg absolute (10 pg ml⁻¹) for Ni were found. TXRF-XANES on different Re species was applied. An unknown species of Re was found to be Re in the +7 oxidation state.
Plastic products used in geotechnical engineering, so-called geosynthetics, are often made of polyolefins (polyethylene or polypropylene) and stabilized against oxidative degradation by antioxidants (AO). Three types of AO “packages” are used: (P1) phenols and phosphites/sulfides, (P2) hindered amines (HAS) with a marginal stabilization P1 of the basic resin, (P3) a combination of packages P1 and P2 with comparable amounts of phenol and HAS. We report about long-lasting oven aging and water immersion tests at 80 °C of 29 different polyolefin based products (geomembranes, geonets and geotextiles). Pronounced differences in the degradation behavior were found depending solely on the type of AO package. In case of P1, the oxidative degradation is prevented by the AO. Autocatalytic oxidation only begins after depletion of AO and may lead to catastrophic failure depending on the environmental conditions. In case of P2, degradation starts right from the beginning. However, it is decelerated and proceeds gradually. In case of P3, the degradation behavior seems to be a superposition of the characteristics obtained for P1 and P2. Plotting the fractional loss of the AO in P1 and P2 as function of the square root of aging time, we identified two regimes of AO depletion. We suggest to attribute this observation to the different mechanisms of AO depletion.
Testing of the oxidative resistance of polyolefin based geosynthetics in
autoclaves at high oxygen pressure has been suggested as an alternative method to
conventional forced-air oven aging. The intention is to shorten considerably the testing
time and to ensure that aging is performed under the condition of rate-controlled
and not diffusion-limited oxidation. We compare data from high pressure autoclave
tests (HPAT) with data from oven aging and water immersion tests at 80 °C. For this,
the stabilization of the samples has to be taken into account. Polyolefin based geosynthetics
are usually stabilized by two types of “packages” of antioxidants (AO), designated
here as P1 and P2. P1 consists of phenols and phosphites, P2 of hindered amine
stabilizers (HAS) in addition to a marginal stabilization P1 of the resin for the manufacturing
process. Phenolic and phosphite AO are quickly consumed in the HPAT.
Failure time is tremendously reduced compared to forced-air oven aging or water
immersion. The results are discussed within the framework of a basic autoxidation
scheme (Wise et al., 1997). The reduction is much greater than expected from theoretical
considerations. Therefore, a direct and degrading reaction of oxygen with the AO
has to be assumed. In case of HAS, the time dependence of the degradation of tensile
properties in the HPAT is significantly different from the dependence observed in
conventional forced-air oven aging and their effectiveness is likewise strongly reduced.
A conclusive interpretation of HPAT results needs a better understanding of
what happens to the AO at high oxygen pressure.
South Africa and recently Nigeria are the only net exporter of cement in Africa, yet cements are imported into the country mainly on the basis of price competitiveness. This poses potential for scatter in the properties of the cements in the South African market as pricing seems to be the only determining factor that affects Portland cements imported. A survey of cements of grade 42.5N in the South African cement market was carried out to identify major players in the industry. The identified cements, which included four locally produced and one imported cement were then analysed for both chemical composition and physical properties in line with the Eurocode EN 196. Tests carried out include loss on ignition, chloride content, sulphate content, specific surface (Blaine), standard consistence, initial setting time, final setting time, soundness and flexural and compressive strength at 2, 7 and 28 days. The testing program was initiated as part of on-going Africa-wide cement testing competency program in partnership with BAM and PTB in Germany. The performance of the identified cements from the different local manufacturers and the imported cement were analysed and are presented in this paper. These results reveal some similarities and differences in the properties. Particularly of interest is the marked difference in the 28 days compressive strength of the cements. This paper shows that there is need for further tests across the cement industry as some of the cements failed to meet certain requirement as set by EN 196. The paper also recommends the use of proficiency testing schemes in the cement industry of the country to ensure the cement laboratories are providing results of high quality and at the same time act as a check to make sure these laboratories are not failing to meet standard requirements.
The objective of the present work was the investigation and demonstration of the potential of sol-gel alumina layers as corrosion protection of commercial power plant steels under oxyfuel conditions. The starting points of this work were modified Yoldas-sols which were developed in the BAM-department 5.6. These sols were suitable for the spin-coating method only. The application of coatings on tubes by spin-coating is impossible. Therefore, the chemical composition of the modified Yoldas-sol had to be adapted to the dip- and spray-coating techniques.
Exclusively the sol with the composition s-0.52-6-1.5 with a nitrate/aluminium ratio of 0.52; a solid content of 6 wt.% and a PVP (binder) content of 1.5 wt.% could fulfill the necessary criteria: long-term stability; formation of a dense, crack-free and well adhered layer on polished metal surfaces; as well as high protective abilities against corrosion in H2O-CO2-O2-SO2.
The commercial power plant steel X20CrMoV12-1 (X20) and the steel X12Cr13 were successfully coated with the sol s-0.52-6-1.5 by means of the dip-coating method. An at least 400 nm thick alumina layer (δ-Al2O3) is necessary to ensure the corrosion protection of these steels. The corrosion of the coated samples compared to that of the uncoated ones was significantly reduced, even after 1000 h of exposure in a H2O-CO2-O2-SO2 atmosphere at 600°C. Sulfur and carbon were not detected at the substrate surface or beneath the coating. Hence the transport of the flue gas components SO2 and CO2 into as well as through the alumina layer could be hindered. The diffusion of the alloying elements (Cr, Mn, Si) into the alumina layer resulted in the formation of mixed oxides like δ-(Al,Cr)2O3. Formation of such phases considerably contributed to the corrosion protection.
The long-term stability of the sol s-0.52-6-1.5 and the high protective abilities of the alumina layer on commercial power plant steels provide a good basis for an industrial application.
There is an increasing interest in optical reporters like semiconductor quantum dots and upconversion nanophosphors with emission > 1000 nm for bioanalysis, medical diagnostics, and safety barcodes and hence, in reliable fluorescence measurements in this wavelength region, e.g., for the comparison of material performance and the rational design of new nanomaterials with improved properties. Here, we present the design of an integrating sphere setup for the absolute measurement of emission spectra and quantum yields in the wavelength region of 650 to 1600 nm and its calibration as well as examples for potential fluorescence standards from different reporter classes for the control of the reliability of such measurements.
Nanocrystalline fluorophores like semiconductor quantum dots and rods and recently also lanthanide-based upconversion phosphors with emission in the visible (vis), near-infrared (NIR), and IR (infrared) region are increasingly being used in bioimaging studies and fluorescence assays as well as in photovoltaics and solid state lighting. The assessment and comparison of material performance as well as the development of rational design strategies for improved systems require spectroscopic tools, which enable the determination of the signal-relevant optical properties like photoluminescence quantum yields and brightness values. In the case of nonlinear fluorescence as shown by upconversion materials, such measurements must be also performed as function of excitation power density. In this work, we report on methods for the absolute determination of the photoluminescence quantum yield and brightness of fluorescent particles in dispersion and as powders based on integrating sphere spectroscopy and underline the importance of such measurements for the understanding of the photophysics of such nanocrystals.
The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread equally holds for industrial and academic research, and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Additionally, I will present a new technique in our portfolio, Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load.
The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread holds equally for industrial and academic research, and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread holds equally for industrial and academic research, and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
Adaption of Heat Control Concepts for Welding Stress Optimization in High-strength Steel Components
(2016)
High-strength structural steels from 690 MPa are increasingly applied at present. Major reasons are lightweight design trends and potential cost reductions. The structural design of welds and their manufacturing become more challenging with increasing material strength. By reasons of a higher yield ratio of these steels, the development of high residual stresses has to be avoided, since they are detrimental to the components safety and performance. Local restraint stresses and welding loads due to external shrinkage restraints occur. Frequently, this leads to critical tensile residual stresses in the weld and HAZ. In this study, influences of welding process parameters and restraint conditions on the residual stress state in welded components of high-strength steels were investigated. Multilayer GMAW tests under free shrinkage and experiments under well-defined restraints in special in-house developed testing facilities were accomplished. The tests permitted analyses of the resulting local residual stresses measured by means of X-ray diffraction and global reaction stress build-up while welding and cooling. Significant effects were found for heat control, seam configuration and restraint condition. Besides high restraints, elevated preheating and interpass temperatures lead to increased welding stresses. An adaption of welding parameters considering heat control, weld run sequence and seam configuration proved to be beneficial.
Adhesion and corrosive delamination of epoxy films on chemically etched ZnMgAl-alloy coatings
(2016)
The effect of alkaline and acidic pretreatment steps on the surface chemical
composition and adhesion properties of ZnMgAl-alloy coated steel was
investigated by means of spectroscopic methods, scanning Kelvin probe (SKP)
and peel test measurements.The spectroscopic results indicate that the surface
film composition can be adjusted by the wet-chemical treatment. To study the
corresponding surface adhesive properties, the samples were coated with an
epoxy amine adhesive. Peel tests under humid conditions indicated an
increased interaction between the acidic pre-treated surface and the adhesive.
The results of the SKP analysis show that the acidic cleaned substrates have the
highest resistance to delamination, which can be explained by the shift of the
interfacial electrode potential.
Adhesion is a key functionality for any kind of coating/substrate system. For optical applications, metallic and dielectric coatings are of major interest, in particular for crucial materials such as silver and gold on glass or metals and dielectrics on polymers. Adhesive strength is defined as the tensile force per area upon delamination. There are only two tensile testing procedures available, the single-sample pull-off test in a tensile testing machine and the multiple-sample test within a centrifuge. Both tests require bonded test stamps on top of the coating. After testing, a microscopic inspection is required in order to determine the failure pattern according to ISO 10365 such as adhesive failure (AF), delamination failure (DF), and cohesive failure (CF). There are remarkable effects of the substrate thickness and the plasto-elastic properties of the substrate on the measured adhesive strength. This fact is in general unavoidable as adhesion is a system property and testing of adhesion is a destructive stress test of the entire coating/substrate system. Various material combinations such as Al on polypropylene (PP), SiO₂ on CR39 polymer, protected layers of Au and Ag on glass have been investigated. Delamination failure (DF) could be divided into DF-R (delamination of metallic reflector) and DF-D (delamination of dielectric protection). Plasto-elastic properties and different thicknesses of the substrate yield to an uneven bending of these substrates during the test. As a result, unavoidable material-induced shear forces are produced, e.g. in dependence on substrate thickness, which is simulated by means of “inverse” the filmdoctor software usually applied to compressive stress conditions. From the first results this might give access to the adhesive strength as calculated independent of the substrate thickness.
The process window and range of functional properties of NbC is wide, because micro-hardness, hot hardness, sliding wear resistance, elastic modulus and toughness can be tailored by the C/Nb ratio, because Nb4C3, Nb6C5 and other short and long range ordered phases occur in the region of homogeneity of NbCx (0,75≤ x ≤1.0) in the binary Phase diagram, and by the type of binder. Further improvements enable the addition of secondary carbides. Supporting results from literature and different grades with varying C/Nb ratio or binder types were illuminated. Thus, the NbC system offers to producers a wider process window, than WC. The impact of these tailored properties on sliding wear and cutting performance was illuminated by tribological and machining results. NbC can be synthesized by carbothermal conversion of Nb2O5 or be metallurgically grown in melts and leached out as coarse NbC cubes. NbC provides comparably lower friction in many relevant tribo-contacts and displays low wear. NbC and Nb2O5 have so far no REACH classification related to human toxicology and are not listed as substances of very high concern contrary to WO3 and Co3O4.
Welded plate girders are used in heavy steel construction, industrial buildings and bride construction. Residual stresses are present in all plate structures. They are mainly caused by welding. In addition, they influence the load bearing capacity of these welded components. However, Eurocode (EC) does not provide any specific residual stress patterns for consideration of residual stress impact on load capacity. Hence, the decision for a particular problem has to be made by the designer. Many codes, including EC 3, permit the use of non-linear finite element analysis (FEA) for the design of structures. This contribution gives an overview on recent research topics: modeling, experimental measuring and evaluation of residual stresses as well as welding simulation tools and simplified methodologies for assessment of weld residual stresses.
Advancements in pressure-assisted sintering technology for low temperature co-fired ceramics (LTCC)
(2016)
Steadily increasing demands on design and dimensional accuracy of ceramic multilayer modules, as well as the processing of new materials, require continuous improvements of manufacturing technology, especially thermal processes. The capabilities of pressure-assisted sintering (PAS) for the manufacturing of highly integrated low temperature co-fired ceramics (LTCC) multilayer have been considerably extended in the last years by procedural and device-related advancements. A lambda probe has been integrated in a sintering press prototype to monitor and control the process atmosphere. Thereby, the development of oxygen partial pressure during binder burnout of real modules can be observed. On the other hand, the oxygen partial pressure can be regulated during densification, for example to prevent diffusion of silver from circuit paths into the surrounding LTCC. Thin-film capable surfaces can be produced without post-processing by using setter plates made of glass-like carbon in an advanced PAS process under nitrogen. A newly developed advancement of this approach enables in-situ hot-embossing of LTCC during PAS by using structured glass-like carbon molds. The prototype press is further extended by a sensitive displacement transducer for monitoring the thickness shrinkage of real modules with an edge length of up to 8 inch.
Welcome to the 2nd International Conference on Advances in Cement and Concrete Technology in Africa (ACCTA 2016), January 27– 29, 2016, held at White Sands Hotel, Dar es Salaam, Tanzania.
The first ACCTA conference that took place in January 2013 in Johannesburg was a result of an African-European collaborative research project. Due to the success of this conference, it was announced that a triennial international conference is necessary, with the next conference scheduled to take place once again in Johannesburg. Within the organisation of the conference, unfortunately some unforeseeable events arose, which would lead to either a delay of the conference in Johannesburg until 2018 or a change of venue. The great response from the international scientific community supported the option to maintain the originally scheduled date. With the support of the local organisation committee from the University of Dar es Salaam and the contributions from the University of the Witwatersrand and the University of Zagreb the conference was shifted to Dar es Salaam.
Despite the new boundary framework, we are extremely happy that it was possible to arrange an outstanding and excellent scientific programme. Therefore we would like to thank in particular the keynote speakers and all members of the international scientific community, as well as other delegates that supported the conference by their contributions and attendance. This shows us how significantly important the African cement and concrete market is for the entire global community.
Africa can become a spearhead for the future of construction with cement and concrete. The continent exhibits an enormous construction potential and due to the relatively short history of building with these materials, innovations can be adopted and adapted unbiased and without influence of stakeholders, traditions, and complicated networks of regulations. This is a fertile ground for the existing promising generation of engineers and decision makers for re-inventing cement and concrete in the best possible way.
There is no global optimum solution for concrete. The best solution in Africa is not the best solution in Europe or another part of the world, and the best solution in one particular African country is diverging from the best solution in another African country depending upon resources, supply chains, infrastructure, construction needs, traditions, available manpower, skills and technologies. Nevertheless, we can globally support our objectives to build future oriented and sustainable construction solutions by mutually learning from each other. In order to tackle the future challenges and build more sustainably and innovatively with concrete, we need to enhance interdisciplinary and cross-national skills and create networks between experts and decision makers globally.
ACCTA offers this kind of platform, and we are happy to announce that the conference reaches a high impact in the world. Delegates and speakers come from more than 40 countries in the world originating from all continents. Besides the technical content there will be plenary discussions on the most relevant topics of future binder technologies and standards and product safety with outstanding expert panellists.
We want to wish all delegates a successful conference and hope that this book can be a significant contribution for a future oriented and better concrete technology; in Africa and the entire world. Welcome to Dar es Salaam, Tanzania.
BAM is the federal institute for materials research and testing in Germany. One of our tasks is to evaluate the safety of casks designed for transport and/or storage of radioactive waste. As elastomeric seals are used in the containers as safety-relevant parts, it is our goal to be able to evaluate the service lifetime of the seals with regard to the requirements for long-term safety (40 years and more) of the containers. For this reason, an accelerated ageing programme with selected rubbers often used for seals (HNBR, EPDM and FKM) was started. Ageing was performed at four different temperatures (75 °C, 100 °C, 125 °C and 150 °C) for up to 2 years. For assessing properties related to the sealability, O-rings were aged in compression by 25 % (corresponding to the compression during service) between plates. For comparison, uncompressed O-rings were aged as well. The aged materials were characterized with conventional polymer analysis methods such as hardness and tensile tests, but also with more seal-specific methods such as compression stress relaxation (CSR, reflecting the loss of sealing force of a compressed seal over time), and compression set (CS, representing the recovery behaviour of a seal after release from compression). CS is chosen as the property for lifetime prediction as it is both sensitive to degradation and related to the seal performance. CS data is extrapolated to 60 °C, which yields lifetimes of approximately 5 years for HNBR and 64 years for EPDM for a criterion of 85 % CS respectively, and approx. 40 years for FKM for a criterion of 65 % CS (the highest value measured so far).
BAM is the federal institute for materials research and testing in Germany. One of our tasks is to evaluate the safety of casks designed for transport and/or storage of radioactive waste. As elastomeric seals are used in the containers as safety-relevant parts, it is our goal to be able to evaluate the service lifetime of the seals with regard to the requirements for long-term safety (40 years and more) of the containers. For this reason, an accelerated ageing programme with selected rubbers often used for seals (HNBR, EPDM and FKM) was started. Ageing was performed at four different temperatures (75 °C, 100 °C, 125 °C and 150 °C) for up to 2 years. For assessing properties related to the sealability, O-rings were aged in compression by 25 % (corresponding to the compression during service) between plates. For comparison, uncompressed O-rings were aged as well. The aged materials were characterized with conventional polymer analysis methods such as hardness and tensile tests, but also with more seal-specific methods such as compression stress relaxation (CSR, reflecting the loss of sealing force of a compressed seal over time), and compression set (CS, representing the recovery behaviour of a seal after release from compression). CS is chosen as the property for lifetime prediction as it is both sensitive to degradation and related to the seal performance. CS data is extrapolated to 60 °C, which yields lifetimes of approximately 5 years for HNBR and 64 years for EPDM for a criterion of 85 % CS respectively, and approx. 40 years for FKM for a criterion of 65 % CS (the highest value measured so far).
HNBR, EPDM and FKM O-rings were aged uncompressed and compressed at 75 °C, 100 °C, 125 °C and 150 °C for up to 1 year. HNBR exhibited the strongest ageing effects with high increases of hardness and glass transition temperature. Furthermore, heterogeneous ageing caused by diffusion-limited oxidation effects had a significant influence for HNBR at ageing temperatures of 125 °C and 150 °C. EPDM showed similar property changes as HNBR, but less pronounced. FKM displayed only minor ageing effects. O-rings aged in compression exhibited considerable compression set (CS). CS data was used for a time-temperature shift and resulting master curve construction. Leakage rate measurements showed that O-rings can remain leak tight under static conditions even if material properties have already deteriorated strongly.
Im Chemikalienrecht ergeben sich laufend Änderungen durch die regelmäßige Überar-beitung des UN-GHS. Konsequenzen hat dies auch für andere Vorschriften, die auf Einstufungen von gefährlichen Stoffen Bezug nehmen. Aber auch andere Vorschriften und Regelwerke unterliegen Änderungen durch Anpassungen an den Stand der Tech-nik. In diesem Beitrag werden für die chemische Sicherheitstechnik wichtige aktuelle Änderungen im Chemikalienrecht und nationalen Arbeitsschutzvorschriften vorgestellt.
Die 6. überarbeitete Fassung des GHS von 2015 enthält eine neue Gefahrenkategorie zur Einstufung von pyrophoren Gasen und eine neue Gefahrenklasse zur Einstufung von desensibilisierten explosiven Stoffen. Außerdem wurden Anforderungen an das Si-cherheitsdatenblatt bezüglich der physikalisch-chemischen Eigenschaften neu gefasst und um Informationen für die Ersteller von Sicherheitsdatenblättern ergänzt. Die 7. überarbeitete Fassung des GHS, die zurzeit in Arbeit ist und Anfang 2017 erschei-nen wird, wird voraussichtlich neue Kriterien und eine geänderte Einteilung für ent-zündbare Gase beinhalten sowie einen neuen Anhang zur Staubexplosionsgefahren.
Bei den nationalen Arbeitsschutzvorschriften haben sich Änderungen anlässlich der Verschiebung der Vorschriften zum betrieblichen Explosionsschutz von der Betriebssi-cherheitsverordnung in die Gefahrstoffverordnung ergeben. Im Nachgang werden auch die technischen Regeln zum Explosionsschutz überabeitet. Die technischen Re-geln für Tätigkeiten mit Gasen sind um Regelungen zu Acetylen ergänzt worden. Wei-tere Ergänzungen zu Füllanlagen für ortsfeste Druckanlagen für Gase und zu Flüssig-gas liegen gegenwärtig den zuständigen Ausschüssen zur Verabschiedung vor.
Im Chemikalienrecht ergeben sich laufend Änderungen durch die regelmäßige Überarbeitung
des UN-GHS. Konsequenzen hat dies auch für andere Vorschriften, die auf
Einstufungen von gefährlichen Stoffen Bezug nehmen. Aber auch andere Vorschriften
und Regelwerke unterliegen Änderungen durch Anpassungen an den Stand der Technik.
In diesem Beitrag werden für die chemische Sicherheitstechnik wichtige aktuelle
Änderungen im Chemikalienrecht und nationalen Arbeitsschutzvorschriften vorgestellt.
Die 6. überarbeitete Fassung des GHS von 2015 enthält eine neue Gefahrenkategorie
zur Einstufung von pyrophoren Gasen und eine neue Gefahrenklasse zur Einstufung
von desensibilisierten explosiven Stoffen. Außerdem wurden Anforderungen an das Sicherheitsdatenblatt
bezüglich der physikalisch-chemischen Eigenschaften neu gefasst
und um Informationen für die Ersteller von Sicherheitsdatenblättern ergänzt. Die 7.
überarbeitete Fassung des GHS, die zurzeit in Arbeit ist und Anfang 2017 erscheinen
wird, wird voraussichtlich neue Kriterien und eine geänderte Einteilung für entzündbare
Gase beinhalten sowie einen neuen Anhang zur Staubexplosionsgefahren.
Bei den nationalen Arbeitsschutzvorschriften haben sich Änderungen anlässlich der
Verschiebung der Vorschriften zum betrieblichen Explosionsschutz von der Betriebssicherheitsverordnung
in die Gefahrstoffverordnung ergeben. Im Nachgang werden
auch die technischen Regeln zum Explosionsschutz überabeitet. Die technischen Regeln
für Tätigkeiten mit Gasen sind um Regelungen zu Acetylen ergänzt worden. Weitere
Ergänzungen zu Füllanlagen für ortsfeste Druckanlagen für Gase und zu Flüssiggas
liegen gegenwärtig den zuständigen Ausschüssen zur Verabschiedung vor.
Zur Vermeidung der schädigenden Alkali-Kieselsäure-Reaktion in Betonbauwerken wird die Alkalireaktivität von Gesteinskörnungen im Vorhinein getestet. Der 60°C-Betonversuch ermöglicht eine vergleichsweise schnelle Einschätzung nach fünf-monatiger Testzeit. Dazu wird die Dehnung von Betonprüfkörpern, die mit der zu testenden Gesteinskörnung hergestellt wurden, manuell alle 28 Tage gemessen. Ein alternatives, an der BAM in den vergangen Jahren entwickeltes Verfahren setzt Dehnungssensoren ein, um kontinuierlich und online zu messen. Die Dehnungskurven sind eine gute Grundlage sowohl für die Prognose vom Expansionsverhalten während des Tests als auch für die Validierung von Expansionsmodellen.
A significant number of German concrete motorway pavements have shown damage only a few years after construction. The alkali-silica-reaction (ASR) is often one of the reasons for this damage. German guidelines and regulations focus on the optimisation of the concrete composition to avoid damage due to ASR. Moreover, diverse research projects have dealt with the development and optimisation of ASR performance test methods with and without external alkali supply.
However, the influence of other parameters on the occurrence and intensity of a damaging ASR had not yet been taken into account. Such parameters include, e.g., insufficient curing and the modifications of concrete’s porosity due to the use of slip form pavers. Likewise, the increased traffic loading had not yet been considered. The Federal Institute for Materials Research and Testing (BAM) assesses these parameters and processes in a number of projects. These projects aim primarily to increase the durability of the concrete pavements, in particular by improving preventive measures that may be taken before or after the construction of concrete pavements. This paper gives a short overview of BAM’s projects concerning ASR in concrete pavements. Furthermore, results regarding the influence of the cyclic traffic loading on ASR are presented.
A significant number of German concrete motorway pavements have shown damage only a few years after construction. The alkali-silica-reaction (ASR) is often one of the reasons for this damage. German guidelines and regulations focus on the optimisation of the concrete composition to avoid damage due to ASR. Moreover, diverse research projects have dealt with the development and optimisation of ASR performance test methods with and without external alkali supply. However, the influence of other parameters on the occurrence and intensity of a damaging ASR had not yet been taken into account. Such parameters include, e.g., insufficient curing and the modifications of concrete’s porosity due to the use of slip form pavers. Likewise, the increased traffic loading had not yet been considered. The Federal Institute for Materials Research and Testing (BAM) assesses these parameters and processes in a number of projects. These projects aim primarily to increase the durability of the concrete pavements, in particular by improving preventive measures that may be taken before or after the construction of concrete pavements. This paper gives a short overview of BAM’s projects concerning ASR in concrete pavements. Furthermore, results regarding the influence of the cyclic traffic loading on ASR are presented.
Durch faseroptische Sensoren können Bauteile im Einsatz kontinuierlich überwacht und frühzeitig Informationen über Materialveränderungen gewonnen werden. Mittels einer magnetostriktiven Aktorschicht, welche den Sensor umhüllt, kann nun auch die korrekte Sensorfunktion jederzeit kontrolliert werden. Als Aktorschicht eignet sich galvanisch abgeschiedenes reines Nickel oder Nickel-Eisen in der Zusammensetzung 50:50. Um diese haftfest mit dem Sensor zu verbinden wurde ein ECD/PVD-Kombinationsschichtsystem entwickelt. Die mechanischen Eigenschaften der ECD-Schicht können sowohl mit einer auf die Fasergeometrie angepassten instrumentierten Eindringprüfung als auch einem 2-Punkt-Biegeversuch bestimmt werden.
Durch den Einsatz von eingebetteten faseroptischen Sensoren können Bauteile überwacht und frühzeitig Informationen über Materialveränderungen gewonnen werden. Um die Zuverlässigkeit eines solchen Sensors gewährleisten zu können, ist es wichtig, die korrekte Funktion des Sensors im Verbund mit einer Werkstoff-Matrix on-line und in-situ überwachen zu können. Im Rahmen des DFG-Projekts FAMOS² (FAser-basierter Magneto-Optischer SchichtSensor) wurde ein selbstdiagnose-fähiger Schichtsensor entwickelt, welcher mit Hilfe einer magnetostriktiven Aktorschicht validiert werden kann. Durch eine Kombination aus PVD (physical vapour deposition) und ECD (electro-chemical deposition) wird die Aktorschicht auf faseroptischen Sensoren haftfest abgeschieden. Ein äußeres Magnetfeldes dehnt die Aktorschicht und damit auch die Faser reversibel. Diese Dehnung führt zu einer Verschiebung der Bragg-Wellenlänge, welche direkt mit der Stärke des zu messenden Magnetfeldes korreliert. Ein etwa 100 Nanometer dünnes PVD-Schichtsystem aus Chrom und Kupfer dient zunächst als Haftvermittler zwischen Glasfaser und ECD-Schicht. Um eine rotationssymmetrische Schichtabscheidung zu erhalten, erfolgt während der PVD-Beschichtung eine Rotation der Faser. In einem klassischen Watts-Elektrolyten wird dann im zweiten Schritt die eigentliche etwa 30 Mikrometer dicke ECD-Aktorschicht auf die PVD-Schicht abgeschieden. Reine Ni-Schichten werden mit NiFe-Legierungen verglichen.
Die Geometrie der Faser stellt für die Herstellung und Charakterisierung der Schichten auf der einen Seite eine besondere Herausforderung dar, bietet aber zugleich auch neue experimentelle Möglichkeiten. So kann ggf. die Entstehung von Spannungen in der Schicht während der ECD-Abscheidung in-situ verfolgt werden, indem die Wellenlängenverschiebung aufgrund der Dehnung des Bragg-Gitters optisch gemessen wird. Die Anpassung der Beschichtungsverfahren an die Fasergeometrie sowie die Charakterisierung und die Eigenschaften der ECD-Schicht werden diskutiert. Insbesondere wird auf den Elastizitätsmodul der Aktorschicht eingegangen, wobei Werte aus der Nanoindentation und dem 2-Punkt-Biegeversuch mit der beschichteten Faser als Biegebalken verglichen werden.
Alumina thin films
(2016)
This chapter gives an overview over preparation, properties and applications of alumina thin films. The preparation of polymeric and colloidal alumina sols and their deposition on diverse substrate materials with different geometries are described first. Consideration of properties (surface tension, particle size, viscosity, aging of the sols and their optimization by using certain additives) is included, too. A description of post-treatments of the coatings, which initiate phase transformations and also determine their microstructure, completes the part on coating preparation. Data on adhesion, thickness, surface roughness and mechanical, textural as well as optical properties of alumina thin films are provided in a further paragraph. In a third main part experience concerning possible applications, such as (i) membranes for catalysis, separation and filtration, (ii) barrier layers against electrochemical and high temperature corrosion or inter-diffusion of ions between different phases, (iii) mechanical protection, (iv) sensor construction, (v) improvement of optical properties, as well as (vi) achieving water repellency is summarized.
In this work a novel iterative method for isothermal cure kinetic modelling of an epoxy resin system using differential scanning calorimetry (DSC) technique is presented. To reach the isothermal cure temperature, the sample has to be heated up from ambient temperature. This is commonly done with very high heat-up rates to minimise the time the sample reacts at temperatures other than the desired one. However, during heat up with high heating the amount of released energy rates cannot be measured directly because the shape of baseline is unknown. This means that the cure state at the beginning of the isothermal stage is unknown. For fast curing systems this unknown cure state causes significant inaccuracies in cure kinetics modelling.
The presented iterative approach attempts to estimate the released enthalpy during heat-up of an isothermal run through an iterative numerical modelling of the heat-up phase. In each iteration the algorithm starts by estimating the enthalpy released during heat-up based on the recorded temperature profile and the calibrated model of the previous iteration. At the same time, it estimates the degree of cure at the end of the heat-up phase. Once the initial cure state is known the total heat of enthalpy can be recalculated for the current iteration. Subsequently the degree of cure and curing rate are re-evaluated with the newly estimated total enthalpy and used for determining the kinetics parameters. This is done by simultaneous fitting of the selected model to all experimental heat flow curves using a non-linear nonrestricted multivariable fitting method. The model with these new parameters is used again to estimate the released enthalpy and cure degree during the heat-up phase. The described loop is repeated until a predefined convergence criterion is satisfied.
For modelling the reaction kinetics, the Kamal–Sourour equation accompanied with Rabinowitch approach to consider the diffusion effects is used. The diffusion reaction rate is modelled by the free volume model proposed by Huguenin and Klein. DiBenedetto model is applied to predict the Evolution of glass transition temperature against the degree of cure. In order to compensate the effect of the Initial values in the model’s calibration, the algorithm is implemented in a routine, which assesses the quality of the fitting and consequently selects the cure kinetics parameter. The described algorithm and the Routine are implemented in MATLAB. This paper demonstrates the application of this approach for using cure kinetics modelling to predict the degree of cure and the glass transition temperature. It supports the obtained results with validation tests using isothermal, dynamic and combined temperature profiles.
Die Schädigung von Gefahrgutbehältern während ihres Transports durch Korrosion und Ermüdungsrisswachstum sind Ursache von Unfällen, die Menschenleben gefährden, die Umwelt schädigen und hohe Sachschäden verursachen. Um solchen Unfällen vorzubeugen, werden präventive Intervallprüfungen durchgeführt. Diese sind jedoch kostenintensiv, unter anderem durch die Standzeit der Transportmittel. Eine Alternative bietet die Idee einer kontinuierlichen Zustandsüberwachung mittels Schallemissionsprüfung (SEP). So sollen Materialfehler sofort nach dem Entstehen entdeckt und repariert werden können. Die Schallemissionsprüfung ist eine online Methode der Familie der zerstörungsfreien Prüfung. Schallemission (SE) wird durch Veränderungen im Material erzeugt und durch elastische Wellen als Körperschall transportiert. Erzeugt das Schallemissionsereignis genug Energie, damit sich eine elastische Welle bis zum Rand eines Bauteils ausbreiten kann, entsteht dort eine Oberflächenverschiebung im Pikometer-Bereich, die mithilfe von piezoelektrischen Sensoren detektiert werden kann. Der Sensor gibt ein elektrisches Signal aus. Aus diesem transienten SE-Signal lassen sich SE-Parameter wie die Maximalamplitude oder die Frequenz extrahieren. Durch Methoden der Signalanalyse können Signalgruppen in der Zeit- und Frequenzebene untersucht werden. Durch Wellenmodenanalysen lassen sich beispielsweise Aussagen über die Art der Quelle machen. Diese Methoden werden angewendet, um aus dem SE-Signal Rückschlüsse auf die Quelle der Schallemission zu ziehen. Werden definierte Schadensmechanismen erkannt, können Hinweise auf den Schadenszustand des Bauteils gegeben werden. Durch Schallemission, die durch den Rissfortschritt erzeugt wird, kann beispielsweise ein Zusammenhang zur Rissfortschrittsrate und zum Spannungsintensitätsfaktor geschlossen werden. Eine neue Entwicklung im Bereich der Schallemissionsprüfung ist die Mustererkennung von SESignalen. Aus den Signalen werden spezifische Merkmale extrahiert, die sie ihren Schadensmechanismen zuordnen sollen. Für die Schadensmechanismen Korrosion und Ermüdungsrisswachstum findet in dieser Arbeit eine vergleichende Analyse von SE-Signalen statt. Die Schadensmechanismen werden anwendungsnah auf großen Platten in der Wärmeeinflusszone einer Schweißnaht generiert und ihre SE-Signale definiert aufgenommen. Dafür werden Resonanzsensoren verwendet, die auf der einen Seite durch ihre Frequenzabhängigkeit sehr empfindlich die kleinste Oberflächenbewegungen reagieren und somit auch für die Anwendung in einer Zustandsüberwachung geeignet sind, jedoch andererseits frequenzbasierte Methoden der Signalanalyse erschweren. Es werden reines Ermüdungsrisswachstum, Ermüdungsrisswachstum unter dem Einfluss von Korrosion sowie reine Oberflächenkorrosion generiert. Die Signalgruppen der Schadensmechanismen werden anhand ihrer Parameter verglichen; anhand von Wellenmodenanalysen können erste Unterschiede, trotz des starken Sensoreinflusses im Frequenzbereich, festgestellt werden. Der Schadenszustand der Proben wird durch bruchmechanische Kenngrößen in Zusammenhang mit SE-Parametern der Signalgruppen gebracht. Ferner findet eine Mustererkennung der SE-Signale statt. Dafür werden zwei Methoden des überwachten Lernens verwendet: eine automatisierte Merkmalsauswahl mithilfe eines kommerziellen Mustererkennungssystems, bei dem hauptsächlich frequenzabhängige Merkmale generiert werden sowie eine parameterbasierte Mustererkennung. Bei der parameterbasierten Mustererkennung wird die Einteilung in Signalklassen aufgrund der Häufigkeitsverteilung der SE-Parameter aus den Signalen der untersuchen Schadensmechanismen vorgenommen. Dabei ergeben beide Methoden, insbesondere für die Schädigung durch Korrosion, eine gute Zuordnung der SE-Signale in die richtige Schädigungsklasse. Abschließend findet unter Berücksichtigung der Nachweisbarkeit von SE-Ereignissen und der Klassifizierbarkeit von SE-Signalen eine Einschätzung zu Chancen und Risiken der permanenten Zustandsüberwachung mittels Schallemissionsprüfung statt. Dazu werden unter anderem eigene Messungen an Tankfahrzeugen hinzugezogen sowie Ergebnisse aus zyklischer und statischer Belastung verglichen. Es wird eine Abschätzung zur Wahl der Überwachungsmethode an Gefahrgutbehältern gegeben.
This study presents diagnostic techniques to assess the structural vulnerability of earthen buildings. Medieval structures at Ambel (near Zaragoza, Spain), once a preceptory or monastic house belonging to the Military Orders, provide a useful case study. After more than a thousand years of construction, failure and repair from the 10th century to the present day, Ambel preceptory today is characterised by marked inhomogeneities: construction materials and structural typologies are juxtaposed, with structural discontinuities at the interfaces between construction phases. This paper argues that, while static analysis is an essential prerequisite before a suitable maintenance program can be defined, no evaluation of the structural behaviour of any historic building can ignore an understanding of the building’s history.
The aim of all the effort devoted to NDE reliability is to evaluate the reliability accurately, reliably and efficiently, in accordance with the specific requirements of industrial application taking into account the very different nature of influencing factors. The set up of the Modular Reliability Model in 1997 was a big step forward in the understanding of influencing mechanisms in terms of the three different main elements, i.e. the intrinsic capability (IC), the application parameters (AP) and the human factors (HF). The intrinsic capability stands for the pure physical-technological process of the signal detection caused by the waves or the rays from a material defect in the presence of noise (caused by the material and the devices). This intrinsic capability is the upper bound of the possible reliability. Already when measuring this intrinsic capability for thick walled components the original one-parameter POD should be extended to a multi-parameter POD, where, in addition to the defect size, a number of additional physical parameters, such as the grain size distribution (or attenuation), defect depth, and angle or surface roughness, must be considered. For real life cycle assessments it is necessary to evaluate the signal response from real defects. The industrial application factors, e.g. coupling conditions, limited accessibility, heat and environmental vibrations, diminish the reliability. The amount of reduction can be determined quantitatively, if the underlying conditions are controlled. In case they are not controlled it is necessary to count for a (unknown) fluctuation in the reliability in the field anyway. The third group of important influencing factors are the human factors, which do not only cover the individual performance capability of the inspectors but also the design of the working place, the procedure, the teamwork quality, interaction with systems, the organization, and finally, the relationship between the companies involved in the inspection process and to which extend the responsible parties are aware of it. Both the internal and external organizational context, affect not only the HF but also the IC and AP. After having analysed the single factors separately it is necessary to look how everything is interconnected. When comparing an “ideal inspection” with a “real inspection” it is worthwhile to look at the existing practices, rules and standards. How do they really support reliable testing? With respect to the industrial end user, it needs to be shown how the level of reliability of NDE, influenced by the different factors and their interaction, has an impact on acceptance or rejection of safety critical parts. The approach of analysis and synthesis will be illustrated by examples of the reliability investigation of the inspection of copper canisters for nuclear fuel deposit in Sweden and Finland and German Railway inspections (hollow axle testing).
Most VVOC were rarely considered in the evaluation of construction products. (Salthammer, 2014) In Germany this will change because the latest version of the German AgBB scheme for health evaluation (2015) now include VVOC, e.g. ethyl acetate and ethanol. In this study selected compounds were tested with the procedure described in ISO 16017 and a method for measuring VVOC with thermal desorption was developed.
Three different adsorbents Tenax TA, Carbograph 5TD and Carbopack X were tested to analyse VVOC according to ISO 16017. For the tested VVOC, Carbograph 5TD showed the best results under the chosen analytical conditions.
Most VVOC were rarely considered in the evaluation of construction products. (Salthammer, 2014) In Germany this will change because the latest version of the German AgBB scheme for health evaluation (2015) now include VVOC, e.g. ethyl acetate and ethanol. In this study selected compounds were tested with the procedure described in ISO 16017 and a method for measuring VVOC with thermal desorption was developed.
Three different adsorbents Tenax TA, Carbograph 5TD and Carbopack X were tested to analyse VVOC according to ISO 16017. For the tested VVOC, Carbograph 5TD showed the best results under the chosen analytical conditions.
Analytische bruchmechanische Ermittlung der Schwingfestigkeit von Schweißverbindungen (IBESS-A3)
(2016)
Ziel des DFG-AiF-Forschungsclusters IBESS war die Entwicklung einer Methodik zur bruchmechanischen Ermittlung von Wöhlerkurven in Schweißverbindungen. Dem vorliegenden Teilprojekt A3 kamen dabei zwei Aufgaben zu: die Entwicklung einer analytischen bruchmechanischen Methodik und die Koordinierung des insgesamt acht Partner umfassenden Clusters. Dieser Bericht fasst die Ergebnisse der erstgenannten Aufgabe zusammen. Die bruchmechanische Methode ist durch folgende Aspekte charakterisiert. (a) Sie beschreibt sowohl Kurz- als auch Langrisswachstum. Ersteres umfasst mechanisch und physikalisch kurze Risse. Mechanisch kurze Risse weisen Abmessungen in der Größenordnung der plastischen Zone auf, weshalb sie zwar bruchmechanisch, nicht jedoch auf der Basis des linear-elastischen K-Konzepts charakterisiert werden können. Im Projekt wurde entsprechend eine Methode zur Bestimmung eines „plastizitätskorrigierten“ zyklischen K-Faktors entwickelt, die auf dem zyklischen J-Integral beruht. Physikalisch kurz bedeutet, dass die Rissschließeffekte im Ausgangsstadium der Rissentwicklung zunächst noch nicht vorhanden sind, dann jedoch graduell aufgebaut werden, bis sie mit Erreichen des Langrissstadiums eine risstiefenunabhängig konstante Größe erreichen. Beschrieben wird dieser Effekt durch die Anwendung der sogenannten zyklischen R-Kurve, der Funktion des Schwellenwerts gegen Rissausbreitung von der Risstiefe. Mittels Rissarrestbetrachtungen des kurzen Risses werden (b) die Ausgangsrissgröße für die weitere Bruchmechanikanalyse und (c) die für N = 107 definierte Dauerfestigkeit der Bauteile bestimmt. Die Analyse erfolgt (d) statistisch, Schwankungen der lokalen Nahtgeometrie entlang des Nahtübergangs über ein Modell äquidistanter Abschnitte einbezogen werden. (e) Eigenspannungen werden sowohl im unbehandelten Schweißzustand als auch nach zyklischer Belastung berücksichtigt. Das Modell wird an insgesamt 33 Wöhlerkurven validiert, die an drei Schweißverbindungsformen (Stumpfstoß, Kreuzstoß, Längssteife) mit je zwei unterschiedlichen Ausführungen, zwei Werkstoffen (S355NL und S960QL), sowie im spannungsarmgeglühten und ungeglühten Zustand experimentell ermittelt wurden.
This paper presents a mode-tracing approach for elastic guided waves based on analytically computed derivatives and includes a study of interesting phenomena in the dispersion curve representation. Numerical simulation is done by means of the Scaled Boundary Finite Element Method (SBFEM). Two approaches are used to identify the characteristics of the resulting wave modes: Taylor approximation and Padé approximation. Higher order differentials of the underlying eigenvalue problem are the basis for these approaches. Remarkable phenomena in potentially critical frequency regions are identified and the tracing approach is adapted to these regions. Additionally, a stabilization of the solution process is suggested.
Analyzing the reliability of non-destructive tests using the modular modell - a practical approach
(2016)
Non-destructive testing is an important tool to guarantee the safety of railway traffic.
The infrastructure with tracks, switches and sleepers is regularly tested, the
locomotives and wagons with their wheels, bogies and axles as well. Many years of experience and some events lead in Germany to a good practice in testing the railway components. Now, European authorities are drafting a system of common requirements and standards for the European Railway Market. The German practice combines an intensive training of the NDT-personnel including sufficient time for practical exercises with organizational measures of the companies, responsible for rolling stock and infrastructure. Through the example of UT-testing of railway axles it will be shown, how training and organizational measures influence the reliability of such testing.
In dieser Studie wurde die Heißrissanfälligkeit beim Laserstrahlschweißen für die Werkstoffe 1.4376, 1.4301 und 1.4828 mit Hilfe des CTW Test quantifiziert. Bei den Versuchen konnten Erstarrungsrisse in den Proben generiert werden. Zusätzlich können mit der Bildkorrelations-Technik die lokalen Dehnungen und Dehnungsraten während des Heißrisstests gemessen wer den. In Verbindung mit einem externen Diodenlaser zum Beleuchten der zu messende Oberfläche und lnterferenzfiltern an den Kameras konnten die DIC Messungen ohne optische Störungen durchgeführt werden.
Die Ergebnisse zeigen, dass die Heißrissbildung bei einer externen Belastung von 3 % für die Stahlsorte 1.4376 zu erwarten ist. Für die Stahls orte 1.4301 beträgt dieser Grenzwert 2 % und 1,5 % für die Stahlgüte 1.4828. Außerdem ist zu beobachten, dass die Gesamtrisslänge mit zu nehmender äußerer Zugbeanspruchung steigt
Anwendung der Reverse-Time Migration auf Ultraschall-Echo-Daten in der zerstörungsfreien Prüfung
(2016)
Das Ultraschall-Echo-Verfahren ist eine klassische zerstörungsfreie Prüftechnik zur Bestimmung der Bauteilgeometrie sowie zur Lokalisierung von Einbauteilen und Fehlstellen. Der aktuelle Stand der Technik bei den Abbildungsverfahren ist die SAFT-Rekonstruktion (Synthetic Aperture Focusing Technique). Diese Gruppe von Verfahren weist u.a. Schwierigkeiten bei der Darstellung von steilen Grenzflächen auf und verarbeitet nur die primären Reflexionen am abzubildendem Objekt korrekt. Als Alternative werden seit einiger Zeit Migrationsmethoden aus dem Bereich der Geophysik evaluiert. Am Beispiel eines Stahlbetonfundamentes wurden in einer Vorarbeit die Kirchhoff-Migration und die Reverse-Time-Migration (RTM) getestet.
Die strahlenbasierten Algorithmen der Kirchhoff-Migration und SAFT-Rekonstruktion sind eng miteinander verwandt. Die RTM hingegen basiert auf der numerischen Lösung der vollständigen Wellengleichung. Durch Kreuzkorrelation von zeitlich vorwärts- und rückwärtsmodellierten Wellenfeldern erzeugt die RTM die migrierte Abbildung. Für die Durchführung der RTM wurde ein 2D akustischer Code verwendet.
Beide Migrationsmethoden wurden an auf Basis der akustischen Wellengleichung generierten synthetischen 2D-Daten sowie an realen Ultraschallmessdaten getestet. Letztere wurden mit Scherwellenprüfköpfen an der Fundamentplatte aufgenommen. Ein Vergleich der Migrationsergebnisse mit den Ergebnissen der SAFT-Rekonstruktion zeigte besonders für die RTM eine deutliche Verbesserung in der Abbildung der Bauteilgeometrie. Die Vorstudie an der Fundamentplatte lieferte somit den Nachweis, dass geophysikalische Migrationsverfahren auf reale Ultraschall-Messdaten anwendbar sind. Jedoch zeigten sich vereinzelt starke Artefakte und systembedingt Schwierigkeiten bei der Abbildung dreidimensionaler Strukturen.
Nunmehr wird vom akustischen Code auf einen elastischen Code umgestellt, da die eigentlichen Ultraschallmessungen mit elastischen Wellen erfolgen. In einem ersten Schritt wurde dies mit dem Softwarepaket Madagascar realisiert und an einem einfachen 2D-Modell getestet. Dabei fanden verschiedene Quellanregungen Anwendung. Des Weiteren wurden zwei Abbildungsbedingungen evaluiert. Ergebnisse der Kreuzkorrelation der Verschiebungskomponenten der zeitlich vorwärts-und rückwärtsmodellierten Wellenfelder wurden mit Resultaten der Kreuzkorrelation der Skalar- und Vektorpotentiale beider Wellenfelder verglichen.
Due to its simplicity, speed and ability to obtain a particle number size distribution, single particle ICP-MS (spICP-MS) has emerged as an important tool for the analysis of nanoparticles (NPs). However, when NPs are suspended in a complex, unknown solution, matrix effects can occur affecting the instrument’s sensitivity. As a result, an over- or underestimation of the particle size is possible.
In this work, a proof-of-concept study of the combination of isotopic dilution analysis (IDA) and spICP-MS compensating for possible matrix effects is presented. As an example, an isotopically enriched 109Ag standard solution was added to silver NPs (Ag NP) suspensions. Different NP suspensions with mean particle diameters between 30 and 80 nm were chosen. The mixtures were analyzed using a quadrupole ICP-MS instrument. Both Ag isotopes (107Ag and 109Ag) were monitored during one experiment. The result show a good agreement with the diameters obtained using conventional spICP-MS.
In a second step, the Ag NPs were suspended in a simulated seawater matrix. Using conventional spICP-MS, a great reduction in the signal intensities and consequently in the particle sizes, was monitored. The application of the IDA-spICP-MS approach on these samples was able to obtain similar diameters compared to the samples without matrix.
In this study, the feasibility of using non-contact Infrared thermography as a potential tool to monitor the CMT welding process is explored. The presence of internal defects such as porosity, lack of filler material deposition and formation of improper weld bead produce perturbations in the surface temperature which can be identified using an Infrared thermography technique. We present recent results obtained from online monitoring of the the dissimilar joining using CMT weld brazing of Aluminum and Steel using a transmission mode measurement approach. The effect of loss of zinc coating on the weldability of the cold metal transfer joining of aluminum to galvanised steel was investigated. A correlation between measured online thermal indications with the weld anomalies is successfully attempted and the results are compared with the conventional post-weld NDT inspection methods.
The corrosion of stainless steel components is a problem of global scale, economically as well as in regards to the safety of industrial equipment and facilities. With microorganisms involved (microbial influenced corrosion, MIC), the problem becomes more complex. Iron reducing bacteria (IRB) for example accelerate the corrosion of iron based materials like stainless steel via the reduction of iron oxides in the passive layer. When co-cultivated with iron oxidizing bacteria, IRBs can induce deep, heterogeneously distributed pits on stainless steel surfaces. The analysis of localized corrosion – or pitting corrosion – is of great relevance since it can lead to unpredictable material failure. In general, macroscopic electrochemical methods are not capable of providing information about the spatial heterogeneity of a sample and thus need to be complemented by multi-electrode based techniques or scanning electrochemical methods.
The aim of this work is to develop methods for the analysis of localized corrosion, on stainless steel surfaces induced by IRB biofilms. The greatest challenge is to address the complexity of two heterogeneous systems at the metal/biofilm interface. First there is the variation in the passive layer composition and microstructure. Secondly, the microbial biofilm with its heterogeneous tree-dimensional structure resulting in local differential aeration cells and electrochemical parameters. To be able to differentiate between individual effects, artificial biofilms mimicking the physical properties of a natural biofilm are used in this study as model systems. This artificial biofilm is applied on a multi-electrode probe to identify local anodic sites during exposure experiments. The detailed analysis of active sites by means of scanning electrochemical microscopy (SECM) allows the investigation of local properties within the biofilm and its immediate vicinity.
The presented analytical approach delivers promising results in clarifying how localized corrosion of stainless steels develops chronologically and spatially in the presence of IRBs. Furthermore, our results on model systems provide the basis for the application of the methodology for the investigation of natural or multi-species biofilms in the future.
The paper deals with the prediction of the fatigue Limit of notched specimens. Some authors in the literature have shown that this issue can be solved by employing an approach based on critical distances, others used elastic fracture mechanics. In this paper the fatigue limit of notched specimens is given by the non-propagating condition of mechanically small surface cracks. According to the so-called cyclic R-curve method, the crack driving force of a growing small crack is compared to its resistance force, which incorporates the gradual build-up of crack closure. The fatigue limit is determined by that applied nominal stress, for which the tangency condition of crack driving and resistance force is satisfied. The approach has been modified to incorporate plasticity effects in the mechanically short crack Regime and it has been applied to a mild and a high-strength steel, in case of an infinite plate with circular hole under remote tensile stress. The method has been successfully applied to the evaluation of fatigue notch-sensitivity in case of surface roughness.
Luminescence-based detection methods, ranging from fluorescence spectroscopy for photophysical and mechanistic studies over sensing applications, chromatographic separation techniques and the microarray technology with fluorescence detection to fluorescence microscopy, flow cytometry, single molecule spectroscopy, and molecular imaging to integrating sphere spectroscopy, are among the most widely used methods in the life and material sciences. This is due to e.g., their unique sensitivity enabling the detection of single molecules, potential for multiplexing, ease of combination with spatial resolution, and suitability for remote sensing. Many of these advantages are closely linked to the choice of suitable molecular and nanoscale fluorescent reporters, typically required for signal generation. This includes organic dyes without and with sensor function, fluorophore-encoded polymeric and silica nanoparticles as well as nanocrystalline systems like semiconductor quantum dots and upconversion phosphors, emitting in the visible (vis), near-infrared (NIR), and IR (infrared). Current challenges present the environment sensitivity of most fluorophores, rendering fluorescence spectra, measured intensities/fluorescence quantum yields, and fluorescence decay kinetics matrix-dependent, and instrument-specific distortions of measured fluorescence signals that need to be considered for quantification and comparability of data, particularly fluorescence spectra.
Here, current applications of luminescence-based methods and different types of reporters will be presented. In this context, suitable spectroscopic tools for the characteri-zation of the optical properties of fluorescent reporters and fluorophore-encoded microparticles, analytical tools for the determination of the surface chemistry of different types of particles, and different multiplexing strategies will be discussed.
One of the unique advantages of polymer optical fibres (POF) is that they can be used to measure very high strain values up to 100 % and beyond exceeding the strain limits of silica fibre-based sensor principles. In this paper the distributed strain measurement capabilities of POF based on backscatter change evaluation are summarized and distributed backscatter measurement technologies are intro-duced. Application examples in the structural health monitoring (SHM) field are presented: a promising approach is the integration into technical textiles for high-strain measurement in earthwork structures and crack detection in buildings. The potential of POF for future applications in SHM such as distributed relative humidity sensing is discussed.
One of the unique advantages of polymer optical fibres (POF) is that they can be used to measure very high strain values up to 100 % and beyond exceeding the strain limits of silica fibre-based sensor principles. In this paper the distributed strain measurement capabilities of POF based on backscatter change evaluation are summarized and distributed backscatter measurement technologies are intro-duced. Application examples in the structural health monitoring (SHM) field are presented: a promising approach is the integration into technical textiles for high-strain measurement in earthwork structures and crack detection in buildings. The potential of POF for future applications in SHM such as distributed relative humidity sensing is discussed.
Many engineering structures are made of composite materials or metal foam. To simulate the deformational behaviour of these structures often requires a high number of discretisation elements. This in turn yields a very large system of linear equations that are extremely time and memory consuming or practically impossible to solve. It is therefore desirable to find an approach to overcome this obstacle.
Many engineering structures are made of composite materials or metal foam. To simulate the deformational behaviour of these structures often requires a high number of discretisation elements. This in turn yields a very large system of linear
equations that are extremely time and memory consuming or practically impossible to solve. It is therefore desirable to find an approach to overcome this obstacle.
Many engineering structures are made of composite materials or metal foam. To simulate the deformational behaviour of these structures often requires a high number of discretisation elements. This in turn yields a very large system of linear equations that are extremely time and memory consuming or practically impossible to solve. It is therefore desirable to find an approach to overcome this obstacle.
Aufbau einer Wissensbasis zu Bruchflächen und Gefüge in der fraktographischen online-Datenbank
(2016)
In einer fraktographischen online-Datenbank werden Informationen zum Bruchverhalten von technischen Werkstoffen zusammengetragen. Primäres Ziel ist die kontrollierte Erzeugung von Brüchen und deren anschließende Analyse, aber auch Beispiele aus Schadensfällen werden eingestellt. Die makroskopischen und mikroskopischen Merkmale von Bruchflächen, die Art der Beanspruchung und die dazugehörigen Werkstoffgefüge werden in Datensätzen zusammengefasst, die der interessierten Fachöffentlichkeit zu Verfügung stehen.
The concrete prism test at 60°C facilitates accelerated testing of alkali-silica reactivity of aggregates within five months. Manual measurement is usually conducted to determine expansion of test specimen every 28 days. This conventional procedure gives only limited insight to expansion behaviour of ASR-affected prisms. Due to the large time intervals, expansion exceeding the critical value of 0.3 mm/m is likely to be noticed late. Continuous recording applied in this work resolves this problem and delivers beneficial information on the shape of the expansion curve.
Different types of aggregate have been tested applying continuous and manual measurement to the concrete specimens.
Models of ASR-induced expansion, available in the open literature, so far are validated with discontinuous data hardly tracing the modelled curve. Continuous measurement improves validation and further model development.
Reliability of NDT depends not only on the intrinsic capability of the measuring systems and on the application factors (the conditions under which NDT is applied), but also—and to a great extent—on human factors and the organisational context under which each inspection is carried out.
Adoption of a systematic approach to the identification and prevention of risks.
Critical defects could be missed, even if the inspection process is semi-automated. The causes of that risk lie in the technology, people and in the organisation. Currently installed preventive measures are insufficient to prevent from risks New preventive measures could be installed, e.g. further automation, installing alarms, implementing human redundancy, developing software and hardware solutions, optimising procedures, etc.
Human factors studies are not only essential for the operation but also during the development process.
Over the past couple of decades Non-Destructive Testing (NDT) has seen a significant increase in the use of automation. In addition to increased reliability, objectivity, consistency, repeatability, productivity, and so on, automating parts of the process is expected to decrease the potential for human error. However, the literature on human-automation interaction suggests that automation is not only associated with benefits, but also with new risks and risk sources. First, this paper will present the methodology used to identify—for the first time—possible risks associated with mechanised data acquisition and corresponding data evaluation. Moreover, it will highlight possible risks, their causes, consequences, and ways of preventing them. Second, those preventive measures will be further analysed by examining new risks that can arise from their implementation, i.e. potential for failure that can arise from (a) working with automated defect-detection and sizing aids, (b) implementing human redundancy, and (c) improvement of the inspection procedures without due consideration of the procedure users. And third, some optimisations strategies will be provided. The purpose of this work is to show that mechanised testing is associated with potential for failure and that the sources of those risks go beyond single inspectors and need to be looked at in the interaction of people with other systems, i.e. the technology, the team and, most importantly, the organisation.
Es wird ein Versuchsstand zum automatisierten MSG-Engspaltschweißen mit integrierter Lasersensorik zur Prozessteuerung und -überwachung vorgestellt. Die Funktion einer Lichtbogensensorik zur automatischen Steuerung der mechanischen Elektrodenauslenkung wird erläutert und verschiedene Anwendungsfälle an Beispielen demonstriert. Die zusätzliche Füllgradregelung beim Mehrlagenschweißen mit veränderlichem Nahtquerschnitt auf Basis der optischen Messtechnik wird zudem vorgestellt.
Average phase stress concentrations in multiphase metal matrix composites under compressive loading
(2016)
We develop a model to predict average over individual phases stress concentrations in a multiphase metal matrix composite under compressive loading. The model accounts for matrix plasticity through variation of the shear modulus with applied stress and for frac- ture of filler through change in the shape of the particles. Three micromechanical models are compared –non interaction approximation, Mori–Tanaka–Benveniste (MTB) scheme, and Maxwell scheme. Comparison with the experimental measurements of Cabeza et al. (2016) shows that Maxwell scheme generally predicts the stress concentration with satis- factory accuracy. Results of MTB scheme vary depending on the loading case and ignoring of the interaction leads to substantial overestimation of the stresses.
We introduce azobenzene-functionalized polyelectrolyte multilayers as efficient, inexpensive optoacoustic transducers for hyper-sound strain waves in the GHz range. By picosecond transient reflectivity measurements we study the creation of nanoscale strain waves, their reflection from interfaces, damping by scattering from nanoparticles and propagation in soft and hard adjacent materials like polymer layers, quartz and mica. The amplitude of the generated strain ε∼5×10−4 is calibrated by ultrafast X-ray diffraction.
Bedingungen für den schadensfreien Einsatz:
Die Passivschicht muss sich vollständig ausbilden können. Dabei sind von Bedeutung:
- Oberflächenausbildung, mechanische Bearbeitung
- Elementverteilung, Ausscheidungen
- Umformung, Wärmeeinbringung
- schweißtechnische Verarbeitung, Anlauffarben
- chemische Nachbehandlung bzw. Konditionierung
Die Repassivierung von Defektstellen unter Einsatzbedingungen muss möglich sein. Dabei sind zu berücksichtigen:
- Legierungszusammensetzung
- kritische Betriebszustände
- prozessbedingte Besonderheiten, Stagnation
- Reinigungsprozesse
In the course of miniaturizing modern technology down to the molecular scale, understanding the materials behavior has to be investigated and deviations from the bulk that might arises from confinement effects has to be understood. Here, a combination of nano-sized relaxation spectroscopies (Broadband dielectric spectroscopy (BDS) and Specific heat spectroscopy (SHS); employing AC nanochip calorimetry) were utilized to investigate the glassy dynamics of ultra-thin films of blends of Poly (vinyl methyl ether) (PVME) / Polystyrene (PS) 50:50 wt-%, which are miscible bulk (thicknesses: 8nm - 200nm, film thickness was controlled by ellipsometry, film topography by AFM). Both methods are sensitive to different probes; where SHS senses entropy fluctuations while BDS measures dipole fluctuations. For BDS measurements, a recently developed nano-structured electrode sample arrangement is employed; where ultra-thin films are spin-coated on an ultra-flat highly conductive silicon wafer, sandwiched between a wafer with nanostructured SiO2 nano-spacers with heights between 35 nm and 70 nm. The method was applied for film thicknesses up to 50 nm. For thicker films, the samples were prepared between crossed electrodes. It was proven that, for 50 nm films, both contact methods will lead to identical results. By measuring the dynamic Tg in dependence of the film thickness, SHS showed that the Tg of the whole film was strongly influenced by a nanometer-thick surface layer at the polymer/air interface due to a self-assembling process [1]. The dynamic Tg obtained from the SHS measurements decrease with decreasing film thickness, evidencing the importance of a mobile surface layer at the polymer/air interface for the glass transition of the whole film. Compared to the SHS results, the BDS measurements show a completely different behavior. At high temperatures, the temperature dependence of the relaxation times of the films follows that of bulk-like PS/PVME; obeying the VFT-law. With decreasing temperature, the temperature dependence deviates from the VFT to an Arrhenius law; where the apparent activation energy decreases with decreasing film thickness. This is the first example where confinement induced changes were observed by BDS for ultra-thin films. All results were analyzed in details in a comprehensive discussion.
Dieses Dokument fasst den Projekfortschritt des BAM-Projektes "Ermittlung geeigneter Wärmeführungen zur Wasserstoffreduktion beim Schweißen höherfester Feinkornbaustähle mit modifiziertem Sprühlichtbogen" im Rahmen des Fachausschusses 1 "Schweißmetallurgie & Werkstoffverhalten" des DVS e. V. zusammen.
Dieses Dokument fasst den Projekfortschritt des BAM-Projektes "Ermittlung geeigneter Wärmeführungen zur Wasserstoffreduktion
beim Schweißen höherfester Feinkornbaustähle mit modifiziertem
Sprühlichtbogen" im Rahmen des Fachausschusses 1 "Schweißmetallurgie & Werkstoffverhalten" des DVS e. V. zusammen.
Die Entwicklung von Wasserstoffbarrieren aus Glas erfordert die genaue Messung geringster H2-Permeabililtäten. Bisherige Untersuchungen haben gezeigt, dass die VHE-Pulvermethode diesbezüglich eine besonders hohe Empfindlichkeit bietet. Hierbei wird die isotherme Gasabgabe aus sphärischen Partikeln im Rahmen klassischer Diffusionsmodelle gefittet und daraus der Diffusionskoeffizient bestimmt. Für die Untersuchung von Gläsern mit möglichst geringer H2-Permeabilität ist jedoch eine Validierung der Genauigkeit der Methode notwendig. Vor diesem Hintergrund erfolgte die numerische Modellierung der H2-Abgabe mit Hilfe des Programms COMSOL Multiphysics®. Im Poster wird der Einfluss der Korngrößenverteilung der Glaspulverpartikel, der Partikelform sowie der Effekt einer nichthomogenen H2-Startverteilung auf die mittels Pulvermethode ermittelten Diffusionskoeffizienten diskutiert.
Die stetig zunehmenden Anforderungen an Kraftstoffverbrauch, Schadstoffemission, sowie passive Sicherheit haben die Automobilindustrie vor Herausforderungen gestellt, die nur durch einen konsequenten Einsatz moderner hochfester Stahlwerkstoffe zu bewältigen sind. Obgleich eine generelle Eignung dieser Stähle für das Widerstandspunktschweißen (WPS) gegeben ist, kann es durch verschiedene externe Einflüsse im betrieblichen Umfeld zur Rissbildung in der Schweißverbindung kommen. Der Einfluss dieser Risse auf die mechanischen Eigenschaften ist derzeit nicht hinreichend genau erfasst, so dass häufig die Vorgabe einer rissfreien Schweißverbindung besteht. Die Kenntnis der Rissanfälligkeit der verarbeiteten Materialkombinationen sowie von ungünstigen Schweißparametern ist daher für viele Unternehmen von erheblicher wirtschaftlicher Bedeutung. Im Rahmen des FOSTA Projekts P921 „Entwicklung eines Verfahrens zur Bestimmung der Rissanfälligkeit von hochfesten Stählen beim Widerstandspunktschweißen“ wurde ein Ansatz zur Bestimmung der Rissanfälligkeit von WPS-Verbindungen hochfester Stähle entwickelt. Mittels einer hydraulischen Vorrichtung unter Zugbelastung wurden geschweißte, rissbehaftete Proben optisch ausgewertet. Das Verfahren ist geeignet, um ein Werkstoffranking bezüglich der Rissanfälligkeit beim Widerstandspunktschweißen für Werkstoffe aufzustellen.
Beton ist als Massenbaustoff vielseitig einsetzbar. Eine der neuesten Entwicklungen ist Ultrahochleistungsbeton (UHPC). Seine besonderen Eigenschaften ermöglichen eine zusätzliche Funktionalisierung der Oberflächen, da annähernd beliebige Mikrostrukturen exakt abgeformt werden können. So lassen sich beispielsweise Fassadenelemente aus UHPC bereits bei ihrer Herstellung im Betonfertigteilwerk mit selbstreinigenden Oberflächen ausrüsten. Eine andere Möglichkeit ist eine Anwendung als Datenspeicher. Wie das Beispiel der Schallplatte aus UHPC zeigt, lassen sich Muster, die hier die Schallinformationen enthalten, exakt von einer Matrize kopieren.
Beton ist als Massenbaustoff vielseitig einsetzbar. Eine der neuesten Entwicklungen ist Ultrahochleistungsbeton (UHPC). Seine besonderen Eigenschaften ermöglichen eine zusätzliche Funktionalisierung der Oberflächen, da annähernd beliebige Mikrostrukturen exakt abgeformt werden können. So lassen sich beispielsweise Fassadenelemente aus UHPC bereits bei ihrer Herstellung im Betonfertigteilwerk mit selbstreinigenden Oberflächen ausrüsten. Eine andere Möglichkeit ist eine Anwendung als Datenspeicher. Wie das Beispiel der Schallplatte aus UHPC zeigt, lassen sich Muster, die hier die Schallinformationen enthalten, exakt von einer Matrize kopieren.
3-Punkt Biegeversuche an Si-basierten Mikro/Nanodrähten wurden im REM mittels Mikromanipulator mit Kraftmessspitze durchgeführt. Die Kraft wurde nach Kalibrierung der Messspitze direkt abgegriffen. Die Auslenkung des Drahtes wurde durch eine Videosequenz im REM aufgenommen und anschließend über die Bildkorrelation ausgewertet. Kraft-Weg-Kurven konnten erstellt werden, um die elastischen Eigenschaften der Drähte zu ermitteln. Die Daten wurden mit FEM-Simulationen und Literatur verglichen. Bruchmechanische Eigenschaften wurden ebenfalls in guter Übereinstimmung mit anderen Verfahren quantifiziert.