Ingenieurwissenschaften und zugeordnete Tätigkeiten
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In coal-fired power plants using oxyfuel combustion process with carbon capture and sequestration, instead of air, a mixture of oxygen and recirculated flue gas is injected in the boiler. A series of steels were exposed to CO2-SO2-Ar-H2O gas mixtures at 600 °C for 1000 h to compare their high temperature corrosion behavior. During the corrosion process, carburization, decarburization and recrystallization were observed underneath the oxide scale depending on the gas mixture and alloy composition. The conditions that lead to carburization are not yet completely understood, but decarburization can be simulated using thermodynamic and kinetic models. In this work, the results of these simulations are compared with measured values for one of the alloys that displayed a decarburized region. Since the mobility of carbon in the scale is not known, two strategies were adopted: simulation of alloy-atmosphere contact; and estimation of the carbon flux to produce the observed decarburization. The second approach might give an insight on how permeable to carbon the scale is.
Visualization of surface modifications may be very challenging for coating/substrate systems of either almost identical optical constants, e.g. transparent films on substrates of the same material, or minor film thickness, substance quantity and affected area, e.g. ultra-thin or island films. Methods for visualization are optical microscopy (OM), imaging ellipsometry (IE), and referenced spectroscopic ellipsometry (RSE). Imaging ellipsometry operates at oblique incidence near Brewster angle of the bare, clean or unmodified substrate. In this configuration, reflected intensities are rather weak. However, the contrast to add-on and sub-off features may be superior. Referenced spectroscopic ellipsometry operates in a two-sample configuration but with much higher intensities. In many cases, both ellipsometric techniques reveal and visualize thin films, printed-pattern, laser-induced changes, and impurities better than optical microscopy. In particular for stratified homogeneous modifications, ellipsometric techniques give access to modelling and hence thickness determination. Modifications under investigation are polymer foil residue on silicon, laser-induced changes of ta-C:H coatings on 100Cr6 steel, imperfections of ta-C:H on thermal silicon oxide, degradation of glass, thin film tin oxide pattern on silicon, printed and dried pattern of liquids such as deionized water, cleaning agents, and dissolved silicone. © 2016 Elsevier B.V. All rights reserved.
In coal-fired power plants using oxyfuel combustion process with carbon capture and sequestration, instead of air, a mixture of oxygen and recirculated flue gas is injected in the boiler. A series of steels were exposed to CO2-SO2-Ar-H2O gas mixtures at 600 °C for 1000 h to compare their high temperature corrosion behavior. During the corrosion process, carburization, decarburization and recrystallization were observed underneath the oxide scale depending on the gas mixture and alloy composition. The conditions that lead to carburization are not yet completely understood, but decarburization can be simulated using thermodynamic and kinetic models. In this work, the results of these simulations are compared with measured values for one of the alloys that displayed a decarburized region. Since the mobility of carbon in the scale is not known, two strategies were adopted: simulation of alloy-atmosphere contact; and estimation of the carbon flux to produce the observed decarburization. The second approach might give an insight on how permeable to carbon the scale is.
Hydroxyapatite (HA) is a bioceramic material with excellent biological properties. However, these properties are strongly dependent of ist crystallinity degree, with high values of crystallinity associated to poor resorption rates and bioactivity. This work evaluates the properties of HA samples produced by two different free-forming conformation methods, CNC machining and 3D printing. In both cases, porous gypsum samples were produced and subsequently converted into HA in a reaction with di-ammonium hydrogen phosphate at 100°C and pH 8. A total conversion of the samples was achieved after 36 h independently of the conformation method used. The microstructure, however, before and after the conversion is showed to be dependent on the method used. After conversion the machined samples achieved a Maximum compressive strength of 3.5 MPaforporosities of circa 80%, while 3D printed samples achieved a tensile strength of 2.0 MPa by porosities of 61%.
It has been shown that selected types of substituents are able to vary the oxidative behavior of multi-walled carbon nanotubes. Such substituents investigated were sterically hindered secondary amino groups bonded in grafted piperidine units and covalently bonded bromine groups. Their interference and activity was preliminary determined in the model cumene and then in oil diesel fraction and low density polyethylene oxidation reactions. Results obtained indicate that chemical linking of amine moieties containing –NH groups directly to the carbon nanotubes core significantly increases their intrinsic anti-oxidative capacity while the grafting of Br-groups provokes the opposite functioning of the pristine samples. This inference was proved by thermogravimetric and differential thermal analysis of the polyethylene composites and experiments on profound aerobic oxidation of petroleum naphthenic fraction derived from the commercial Baku oils blend diesel cut.
Quality control requirements imposed on assays used in clinical diagnostics and point-of-care-diagnostic testing (POCT), utilizing amplification reactions performed at elevated temperatures of 35 to 95 °C are very stringent. As the temperature of a reaction vessel has a large impact on the specificity and sensitivity of the amplification reaction, simple tools for local in situ temperature sensing and monitoring are required for reaction and assay control. We describe here a platform of stem-and-loop structured DNA hairpins (molecular beacons, MBs), absorbing and emitting in the visible and red spectral region, rationally designed for precise temperature measurements in microfluidic assays for POCT, and their ap-plication for temperature measurements in a common DNA-based molecular biological assay utilizing thermophilic helicase-dependent amplification (tHDA). Spectroscopic studies of these MBs, rationally designed from DNA se-quences of different thermal stabilities, chosen not to interact with the DNA probes applied in the nucleic acid amplification assay, and temperature-dependent fluorescence measurements of MB-assay mixtures revealed the suitability of these MBs for temperature measurements directly in such an assay with a temperature resolution of about 0.5 °C without interferences from assay components. Combining two spectrally distinguishable MBs provides a broader response range and an increase in temperature sensitivity up to 0.1 °C. This approach will find future application for temperature monitoring and quality control in commercialized diagnostics assays using dried reagents and microfluidic chips as well as assays read out with tube and microplate readers and PCR detection systems for temperature measurements in the range of 35 to 95 °C.
Microstructure-property connections for porous ceramics: The possibilities offered by micromechanics
(2016)
Microstructure of porous ceramics is highly “irregular”: it comprises pores and microcracks of diverse shapes and orientations.
This makes their quantitative modeling challenging, and one
often resorts to empirical relations containing Fitting Parameters and having somewhat uncertain range of applicability. We review the substantial progress made in modeling of “irregular” microstructures that does not seem to have been sufficiently utilized in the context of ceramics. We discuss the possibilities offered by micromechanics in developing microstructure–property relations for porous microcracked ceramics. After an overview of relevant micromechanics topics, we focus on several issues of specific interest for ceramics: nonlinear stress–strain behavior, effective elastic properties, and thermally induced microcracking. We discuss extraction of microscale Parameters (such as strength of the intergranular cohesion, density of cracks and pores, etc.) from macroscopic data and identify the extent of uncertainty in this process. We also argue that there is no quantitative correlation between fracturing process and the loss of elastic stiffness.
Texture formation in amorphous Al86Ni6Y4.5La1.5Co2 splats by thermal and mechanical treatment
(2016)
The crystallization behavior of amorphous Al86Ni6Y4.5La1.5Co2 splats was analyzed by differential scanning calorimetry (DSC) and X-ray diffraction (XRD). Rietveld refinement was used to analyze the preferred orientation of fcc aluminum nanocrystals in the residual amorphous matrix after annealing. Fiber textures in [200] and [220] directions were found after heating to 360 C. The influence of cold rolling on the preferred crystal orientation was studied as a function of the thickness reduction of the specimen. It was found that cold rolling significantly increases the (220) texture, while the (200) texture remains unchanged. Based on the experimental results the formation of (220) and (200) texture during the crystallization of the amorphous splats was ascribed to two different processes, internal stresses induced during splat formation or cold-rolling.
3-Aminovinylquinoxalines are readily accessible from (hetero)aryl glyoxylic acids or heterocyclic π-nucleophiles by consecutive four- and fivecomponent syntheses in the sense of an activation-alkynylation-cyclocondensation-addition sequence or glyoxylation-alkynylation-cyclocondensation-addition sequence in good yields. The title compounds are highly fluorescent with pronounced emission solvatochromicity and protochromic fluorescence quenching. Time-resolved fluorescence spectroscopy furnishes radiative and nonradiative fluorescence decay rates in various solvent polarities. The electronic structure is corroborated by DFT and TD-DFT calculations rationalizing the observed spectroscopic effects.
Similar to the success story of digital photography a major upheaval has been observed in digital industrial radiology. This paper is split into 3 parts:
Part 1: Film Replacement and Backscatter Imaging: Computed radiography with phosphor imaging plates substitutes film applications. Digital Detector Arrays enable an extraordinary increase of contrast sensitivity in comparison to film radiography. The increased sensitivity of digital detectors enables the efficient usage for dimensional measurements and functionality tests substituting manual maintenance. The digital measurement of wall thickness and corrosion status is state of the art in petrochemical industry. Photon counting and energy discriminating detectors are applied up to 300 Kv provide increased thickness dynamic and material discrimination by synchronously acquisition of images of the high and low energy part of the spectrum. X-ray back scatter techniques have been applied in safety and security relevant applications with single sided access of source and detector. First inspections of CFRP in aerospace industry were successfully conducted with newly designed back scatter cameras. Numeric modeling is used to design X-Ray optics and inspection scenarios as well as conducting RT training.
Part 2: Computed tomography (CT)
Part 3: Micro Radiography and Micro CT.
Designing artificial macromolecules with absolute sequence order represents a considerable challenge. Here we report an advanced light-induced avenue to monodisperse sequencedefined functional linear macromolecules up to decamers via a unique photochemical approach. The versatility of the synthetic strategy—combining sequential and modular concepts—enables the synthesis of perfect macromolecules varying in chemical constitution and topology. Specific functions are placed at arbitrary positions along the chain via the successive addition of monomer units and blocks, leading to a library of functional homopolymers, alternating copolymers and block copolymers. The in-depth characterization of each sequence-defined chain confirms the precision nature of the macromolecules. Decoding of the functional information contained in the molecular structure is achieved via tandem mass spectrometry without recourse to their synthetic history, showing that the sequence information can be read.We submit that the presented photochemical strategy is a viable and advanced concept for coding individual monomer units along a macromolecular chain.
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.
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.
Electron Beam Melting (EBM) as a means of Additive Manufacturing (AM), is of interest for the fabrication of intricate geometries for cellular materials in areas where complex architectures are needed, e.g. biomedical implants. Most studies have focused on specific geometries and so the effect of the structure on mechanical performance is not well understood. Many kinds of micro- and macro-scale defects can arise in additively manufactured components, so assessment of their influence on properties is needed. In this work, lattices of Ti-6Al-4V having a cubic structure have been manufactured by EBM, and the effect of heat treatments above and below the β-transus temperature on microstructure and compression response have been investigated. The former modifies only slightly the α + β structure and mechanical performance whereas the latter leads to coarse alternating α and β lamellae packets and α at the prior grain boundaries with a 10% loss in yield strength. The variation in the compressive yield stress with strut diameter is in good accord with simple models based on compressive deformation rather than shearing or buckling. Internal pores for struts aligned with the build direction are found around the edges of the solid form, in regions which seem to be associated with the EB scan pattern. Struts normal to the build direction show more significant defects but their redundancy means that they do not compromise the compressive performance in the build direction. Using a particle size in the range 45–100 μm minimum weld-track sizes were experimentally and numerically identified to be 176 and 148 μm in depth respectively with a depth-to-width ratio of 0.55. This produced a beam pass of the order of 300 μm oversizing small features (struts of 0.4 and 0.6 mm nominal diameter) when a contour around the strut periphery was applied.
Measurement and numerical modeling of residual stresses in welded HSLA component-like I-girders
(2016)
The present contribution shows the residual stress results obtained from experiments with the sectioning method in comparison to global(structural) welding simulation models on component-like (i.e., large scale) I-girders made
of structural steel grades S355 and S690QL. Plates were welded by conventional gas metal arc welding using two different heat inputs. In addition, the base material was assumed to be stress-free. Based on these results, conclusions and recommendations for the design of welded I-girders are drawn.
In the second half of the 19th century, Roman and Portland cements played an essential role as active hydraulic binder material in building construction and façade ornamentation. Size and heterogeneous phase assemblage of unhydrated cement clinker remnants in historical cement stone differ significantly from those of remnants occurring in modern Portland cement clinker burnt in rotary kilns due to limitations of the production technology available in the 19th century (e.g., comminution and homogeneity of the feedstock, burning temperature and regime in the intermittently operated shaft kilns, grinding machinery). In the common analytical approach, thin sections and fracture surfaces of historical Roman and Portland cement mortars are characterised regarding their mineralogical composition and microstructure using optical and electron microscopic imaging techniques. Raman microspectroscopy can be additionally employed for petrographic examination, overcoming some limitations of the methods used so far. The determination of the phase content of residual cement clinker grains in the hydrated matrix allows for the differentiation of Roman and Portland cement binders. As marker phases, we propose the calcium aluminates CA, C12A7, C2AS and C3A – besides the commonly used calcium silicates C2S and C3S – because of their different formation temperatures and stability fields. This study focuses on the identification of different calcium aluminate and aluminoferrite phases in clinker remnants in samples of cast ornaments of three buildings in Switzerland raised between 1875 and 1893; the obtained Raman spectra are compared with fingerprint spectra of the corresponding pure, synthesised clinker phases collected with the same instrument for an unambiguous data interpretation. In addition to these phases, mainly minerals showing no hydraulic activity, such as, wollastonite CS, rankinite C3S2, free lime, portlandite, iron oxides, garnets, augite, albite and feldspathoids have been identified in the sampled historical cement stones by Raman microspectroscopy. As there is a strong relationship between coexisting clinker phases and the chemical composition of the raw meal as well as the burning and cooling history during clinkering, the results can help in understanding the physical and mechanical characteristics of historical cement mortars. This knowledge is fundamental for the choice and the formulation of appropriate repair materials with tailored properties employed in the field of restoration and preservation of the architectural heritage of the 19th and early 20th centuries.
The detection and characterization of surface cracks in steel specimens prior to damage is a technologically and economically highly significant task and is of utmost importance when it comes to safety-relevant structures. In steel production where steel billets at high temperatures have to be inspected while moving a number of well-established NDT methods cannot be applied. Laser thermography however is a promising candidate to serve as a fast, non-contact and remote tool in this case. We present a study that shows that the crack detection capabilities of laser thermography can be extended also to specimens at high temperature. A combination of inductive and laser heating allows to systematically study the contrast formation as well as the optimization of the important measurement parameters. The experiments are accompanied by FEM simulations that provide a better insight of the physical correlations and support the experimental developments. The aim of these studies is to develop a system with high inspection speed and detection performance to be in-line operated under the hostile environment of steel production lines.
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.
Online (passive) thermographic inspection of overlap joints of aluminium and zinc coated steel sheets made by cold metal Transfer weld brazing process was explored. Different experimental Trials were conducted for demonstrating the feasibility of thermographic inspection to detect the porosities, improper weld bead and to differentiate the pre weld temperature. The whole process was monitored using infrared cameras in different wavelength region.
Image analysis algorithms were developed to reconstruct the thermal images that contain the signatures of the weld defects and to extract the pre weld temperature and ist evolution with distance from the centre of the weld torch. Post-weld radiography lends strong Support to the observations.
Using channeling-enhanced energy-dispersive X-ray spectroscopy (EDX), we demonstrate polarity sensitive orientation determination of a non-centrosymmetric crystal in the scanning electron microscope. The authors observe a characteristic asymmetry in the channeling-enhanced, angle-dependent EDX data of a GaAs sample, which is in good agreement to simulations using the dynamical theory of diffraction for the incident electron beam. This allows us to assign the orientation of the GaAs crystal according to the non-centrosymmetric point group. The method shown here overcomes the limitation of a reduced point-group sensitivity of electron backscatter diffraction Patterns and electron channeling patterns for crystalline phases that contain atoms of approximately equal electron scattering cross sections.
Nondestructive flaw detection in polymeric materials is important but difficult to achieve. In this research, the application of magnetite nanoparticles (MNPs) in nondestructive flaw detection is studied and realized, to the best of our knowledge, for the first time. Superparamagnetic and highly magnetic (up to 63 emu/g) magnetite core-shell nanoparticles are prepared by grafting bromo-end group-functionalized poly(glycidyl methacrylate) (Br-PGMA) onto surface-modified Fe3O4 NPs. These Fe3O4-PGMA NPs are blended into bisphenol A diglycidylether (BADGE) based epoxy to form homogeneously distributed magnetic epoxy nanocomposites (MENCs) after curing. The core Fe3O4 of the Fe3O4-PGMA NPs endows the MENCs with magnetic property, which is crucial for nondestructive flaw detection of the materials, while the shell PGMA promotes colloidal stability and prevents NP aggregation during curing. The eddy current testing (ET) technique is firstly applied to detect flaws in the MENCs. Through the brightness contrast of the ET image, surficial and sub-surficial flaws in MENCs can be detected, even for MENCs with low content of Fe3O4-PGMA NPs (1 wt %). The incorporation of Fe3O4-PGMA NPs can be easily extended to other polymer and polymer-based composite systems and opens a new and very promising pathway toward MNP-based nondestructive flaw detection in polymeric materials.
Vertebroplasty or kyphoplasty of osteoporotic vertebral fractures bears the risk of pulmonary cement embolism (3.5%–23%) caused by leakage of commonly applied acrylic polymethylmethacrylate (PMMA) cement to spongious bone marrow or outside of the vertebrae. Ultraviscous cement and specific augmentation systems have been developed to reduce such adverse effects. Rapidly setting, resorbable, physiological calcium phosphate cement (CPC) may also represent a suitable alternative.
PURPOSE: This study aimed to compare the intravertebral extrusion of CPC and PMMA cement in an ex vivo and in vivo study in sheep.
STUDY DESIGN/SETTING: A prospective experimental animal study was carried out. METHODS: Defects (diameter 5 mm; 15 mm depth) were created by a ventrolateral percutane-ous approach in lumbar vertebrae of female Merino sheep (2–4 years) either ex vivo (n = 17) or in vivo (n = 6), and injected with: (1) CPC (L3); (2) CPC reinforced with 10% poly(l-lactide-co-glycolide) (PLGA) fibers (L4); or (3) PMMA cement (L5; Kyphon HV-R). Controls were untouched (L1) or empty defects (L2). The effects of the cement injections were assessed in vivo by blood gas analysis and ex vivo by computed tomography (CT), micro-CT (voxel size: 67 µm), histology, and biomechanical testing.
Im Rahmen des EU-Forschungsvorhabens [H]house wurden Holz, Lehm und Naturfasern in Bezug auf Feuchtesorption und Schadstoffe untersucht und mit konventionellen Materialien verglichen. Weiter entwickelte Innenwandsysteme und Innendämmungen wurden ebenfalls untersucht. Auf dieser Basis wurden Holz- und Lehm-Bausysteme ohne Lüftungsanlage entwickelt und angewendet.
Low-κ dielectric LTCC was developed, to realize successful co-firing with NiCuZn ferrite tapes. A critical high-temperature process in the production of highly integrated LTCC modules is the migration of silver from inner conductors into the LTCC glass phase. Intensive silver migration causes strong deformation of LTCC multilayers during firing in air.
Silver migration into the LTCC glass phase depends on oxygen content of the sintering atmosphere and can be minimized by sintering in nitrogen atmosphere. However, partial decomposition of NiCuZn-ferrite and formation of cuprite was observed during sintering in nitrogen and, consequently, the permeability of the ferrite decreases. As shown by a combined XRD/thermogravimetric study the co-firing of LTCC modules with silver metallization and integrated ferrite layer demands precise adjustment of oxygen partial pressure.
Ob in der Automobilindustrie, beim Rohrleitungs- oder beim Kraftwerksbau – anspruchsvolle und hochwertige Fügeverbindungen entscheiden oft über die Qualität des Endproduktes. Um z. B. das Verzugsverhalten von Karosseriebauteilen vorab einschätzen zu können, setzen Hersteller auf die numerische Simulation der geschweißten Komponenten. Besondere Aufmerksamkeit gilt hier den Fügestellen. Da diese oft nur wenige Millimeter klein sind, kommen konventionelle Prüfverfahren wie der Zugversuch hier jedoch nicht ohne weiteres in Frage.
Forscher des Fraunhofer IPK untersuchen deshalb eine alternative Methode, um die negativen Begleiterscheinungen des thermischen Schweißens im Vorfeld am PC zu analysieren und nötige Gegenmaßnahmen ableiten zu können.
Die Anwendung der additiven Fertigung nimmt stark zu. Eine neue Designfreiheit erlaubt es hier den Konstrukteurinnen und Konstrukteuren, die Bauteilfunktion in den Vordergrund der Entwicklungen zu stellen. Leichtbaustrukturen sowie Funktionsintegration machen es möglich, vormals Bauteile aus vielen Einzelkomponenten jetzt in einem einzigen Bauteil zu vereinigen. Experten am Fraunhofer IPK qualifizieren das Laser-Pulver-Auftragschweißen für die additive Fertigung und legen dabei besonderen Wert auf die Automatisierung des Verfahrens.
The interest in (micro)porous systems is greater than ever before with microporous polymers finding application in areas such as gas storage/separation and catalysis. In contrast to the vast majority of publications on microporous polymers seeking ever higher values for surface area or uptake capacity for a particular gas, this work presents a means to render a microporous system responsive to electromagnetic stimuli. The incorporation of a diarylethene (DAE) derivative in the backbone of a polymer of intrinsic microporosity (PIM) produces a microporous system that exhibits photochromism as proven by UV–vis absorption and NMR studies. In the resulting DAE-PIM, surface area is not a fixed unalterable property but can be influenced by the external and nondestructive stimulus light in a reversible manner. Furthermore, in combination with Matrimid, free-standing membranes can be produced that display light-switchable diffusivity and permeability for carbon dioxide and oxygen. In this way, material scientists are offered the potential to employ only one system that can assume several states with different properties for each.
Die Richtlinie 2014/28/EU für zivile Explosivstoffe verlangt die Verwendung einer eindeutigen Identifizierung jedes einzelnen Explosivstoffs. Das schon 2008 durch die Richtlinie 2008/43/EG eingesetzte Verfahren, ergänzt durch eine Empfehlung der Federation of European Explosives Manufacturers (FEEM), hat im Laufe der Implementierung verschiedene Probleme und Fragen aufgeworfen. Einige Probleme technischer Natur bezüglich der Code-Inhalte werden hier dargestellt. Dabei geht es um Abweichungen von den Vorgaben, die die Verarbeitung dieser eindeutigen Kennzeichnung erschweren. Es zeichnet sich jedoch auch ab, dass sich die Probleme allmählich verringern werden.
Laser beam processes are increasingly used in the field of additive manufacturing.
Prominent methods are either powderbed-based like Laser Metal Fusion (LMF), or utilizing a powder nozzle like Laser Metal Deposition (LMD). While LMF allows the manufacturing of complex structures, build rate, part volumes and material flexibility are limited. In contrast, LMD is able to operate with high deposition rates on existing parts, and materials can be changed easily during the process. However LMD shape complexity is limited. Utilizing their respective strengths, a combination of these two additive technologies has the potential to produce complex parts with high deposition rates and increased material flexibility. In this paper, combined manufacturing with additive technologies LMF and LMD is described. Its benefit for industry with emphasis on turbomachinery is shown. As reality test for the innovation, an industrial turbine blade is manufactured.
We discuss the dynamics of ultrashort pulsed laser excitation in bulk optical silica-based glasses (fused silica and borosilicate BK7) well-above the permanent modification threshold. We indicate subsequent structural and thermomechanical energy relaxation paths that translate into positive and negative refractive index changes, compression and rarefaction zones. If fast electronic decay occurs at low excitation levels in fused silica via self-trapping of excitons, for carrier densities in the vicinity of the critical value at the incident wavelength, persistent long-living absorptive states indicate the achievement of low viscosity matter states manifesting pressure relaxation, rarefaction, void opening and compaction in the neighboring domains. An intermediate ps-long excited carrier dynamics is observed for BK7 in the range corresponding to structural expansion and rarefaction. The amount of excitation and the strength of the subsequent hydrodynamic evolution is critically dependent on the pulse time envelope, indicative of potential optimization schemes.
Healable materials could play an important role in reducing the environmental footprint of our
modern technological society through extending the life cycles of consumer products and constructions. However, as most healing processes are carried out by heat alone, the ability to heal damage generally kills the parent material’s thermal and mechanical properties. Here we
present a dynamic covalent polymer network whose thermal healing ability can be switched ‘on’ and ‘off’ on demand by light, thereby providing local control over repair while retaining the advantageous macroscopic properties of static polymer networks. We employ a photoswitchable furan-based crosslinker, which reacts with short and mobile maleimidesubstituted poly(lauryl methacrylate) chains forming strong covalent bonds while simultaneously allowing the reversible, spatiotemporally resolved control over thermally induced de- and re-crosslinking. We reason that our system can be adapted to more complex materials and has the potential to impact applications in responsive coatings, photolithography and microfabrication.
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.
A reversed phase high performance liquid chromatography coupled to an inductively coupled plasma mass spectrometer (HPLC-ICP-MS) approach in combination with isotope dilution analysis (IDA) for the separation and parallel quantification of nanostructured and ionic silver (Ag) is presented. The main focus of this work was the determination of the ionic Ag concentration. For a sufficient stabilization of the ions without dissolving the nanoparticles (NPs), the eluent had to be initially optimized. The determined Ag ion concentration was in a good agreement with results obtained using ultrafiltration. Further, the mechanism of the NP separation in the HPLC column was investigated. Typical size exclusion effects were found by comparing results from columns with different pore sizes. Since the recovery rates decreased with increasing Ag NP size and large Ag NPs did not elute from the column, additional interactions of the particles with the stationary phase were assumed. Our results reveal that the presented method is not only applicable to Ag NPs, but also to gold and polystyrene NPs. Finally, IDA-HPLC-ICP-MS experiments in single particle mode were performed to determine the particle cut-off size. The comparison with conventional spICP-MS experiments resulted in a similar diameter and particle size distribution.
Atemluftflaschen aus Faserverbundwerkstoffen werden im Feuerwehrbetrieb hohen thermischen Belastungen ausgesetzt. Der thermisch sichere Bereich dieser Behälter ist jedoch heutzutage noch nicht einschätzbar. Deshalb haben es sich die Bundesanstalt für Materialforschung und -prüfung (BAM) im Austausch mit der Bergischen Universität Wuppertal zur Aufgabe gemacht, die Auswirkungen dieser Betriebslasten zu untersuchen. Die Erkenntnisse dieser Untersuchungsreihe werden genutzt, um einzuschätzen, ob es sicherheitstechnisch notwendig ist, besondere thermische Betriebsbedingungen in normativen Prüfkriterien zu berücksichtigen.
In einem ersten Schritt wurden Typ-III-Atemluftflaschen der Berliner Feuerwehr Umgebungsbedingungen des typischen Belastungsprofils der Brandbekämpfung (130 °C bis 250 °C, 10 Minuten) ausgesetzt, um die Erwärmung des Behältermaterials zu erfassen. Da die Größe der bestrahlten Oberfläche in einem Brandeinsatz nicht bekannt ist, erfolgte zusätzlich eine Variation der Strahlungsexposition. Strömungsprozesse, die in einem Brandeinsatz den Behälter von innen kühlen, wurden in diesem ersten Untersuchungsabschnitt noch nicht betrachtet.
Es konnte gezeigt werden, dass der Aluminium-Liner einer Typ-III-Atemluftflasche einen erheblichen Einfluss auf die Temperaturverteilung im Behältermaterial ausübt. Die hohe Leitfähigkeit des Aluminiums führt bei Verringerung der bestrahlten Behälteroberfläche zu hohen Temperaturgradienten innerhalb der Behälterwand. Die Materialtemperaturen in der Atemluftflasche konnten für das Belastungsprofil der Brandbekämpfung auf ein typisches Temperaturintervall eingegrenzt werden. Die Grenzen liefern Aussagen zur exponierten Behälteroberfläche und liegen zwischen einseitiger und Vollbestrahlung.
Ultrafast laser processing can be used to realize various morphological surface transformations, ranging from direct contour shaping to large-area-surface functionalization via the generation of “self-ordered” micro- and nanostructures as well as their hierarchical hybrids. Irradiation with high-intensity laser pulses excites materials into extreme conditions, which then return to equilibrium through these unique surface transformations. In combination with suitable top-down or bottom-up manufacturing strategies, such laser-tailored surface morphologies open up new avenues toward the control of optical, chemical, and mechanical surface properties, featuring various technical applications especially in the fields of photovoltaics, tribology, and medicine. This article reviews recent efforts in the fundamental understanding of the formation of laser-induced surface micro- and nanostructures and discusses some of their emerging capabilities.
Benzamide has been known for its polymorphism for almost 200 years.Three polymorphic forms are described. To date,itwas only possible to crystallizeametastable form in amixture together with the thermodynamically most stable form I. Acomplete transformation of form Iinto the metastable form III by mechanochemical treatment has been achieved. Catalytic amounts of nicotinamide seeds were used to activate the conversion by mechanochemical seeding. NMR experiments indicated that the nicotinamide molecules were incorporated statistically in the crystal lattice of benzamide form III during the conversion. The transformation pathway was evaluated using in situ powder X-ray diffraction.
The device performance of polycrystalline chalcogenide thin film solar cells is strongly influenced by different kinds of defects within the material. The presence of sodium or other alkali metals like potassium during the deposition process is well known to influence the electronic properties of the solar cell and thus to improve the efficiency of the final device. Structural analysis of neutron powder diffraction data collected at low temperatures and subsequent profile analysis by the LeBail and Rietveld method demonstrates the impact of sodium on the point defect characteristics in off stoichiometric CuInSe2. The analyzed materials are powder and thin film solar absorber material with addition of NaF and free of sodium. It is illustrated, the so called “sodium effect” cannot be reduced to one single origin. A range of effects, the reduction of InCu donors with a followed increase of VCu acceptors is possible. The main effect is an increased ordered character of the chalcopyrite crystal structure at off stoichiometric composition, when containing sodium.
Talbot-Lau interferometry provides X-ray imaging techniques with significant enhancement of the radiographic contrast of weakly absorbing objects. The grating based technique allows separation of absorption, refraction and small angle scattering effects. The different efficiency of rectangular and triangular shaped phase gratings at varying detector distances is investigated. The interference patterns (Talbot carpets) are modeled for parallel monochromatic radiation and measured by synchrotron radiation. In comparison to rectangular shapes of phase gratings much higher visibility is obtained for triangular shapes which yield enhanced contrast of a glass capillary test specimen.
The crystal structures and syntheses of four different copper(II) phenylphosphonates, the monophenylphosphonates α-, β-, and γ-Cu(O3PC6H5)·H2O (α-CuPhPmH (1) β-CuPhPmH (2) and γ-CuPhPmH (3)), and the diphosphonate Cu(HO3PC6H5)2·H2O (CuPhP2mH (4)), are presented. The compounds were synthesized from solution at room temperature, at elevated temperature, under hydrothermal conditions, and mechanochemical conditions. The structures of α-CuPhPmH (1) and CuPhP2mH (4) were solved from powder X-ray diffraction data. The structure of β-CuPhPmH (2) was solved by single crystal X-ray analysis. The structures were validated by extended X-ray absorption fine structure (EXAFS) and DTA analyses. Disorder of the crystal structure was elucidated by electron diffraction. The relationship between the compounds and their reaction pathways were investigated by in situ synchrotron measurements.
CO2 streams captured from power stations or industrial plants may contain impurities that impact the consecutive steps of the CO2 capture and storage (CCS) chain. As the basis for an optimization of CO2 purity over the whole CCS chain, impacts of different impurities were investigated at key steps including studies on (i) corrosion of metallic materials in CO2 streams and brine, (ii) fluid and interfacial properties as a function of pressure, temperature and CO2 stream composition and their implications for CO2 transport, injection and geological storage, (iii) costs of different pipeline design options, (iv) geochemical alterations at typical reservoir conditions and their implications for geomechanical rock properties. Major findings are synthesized for two exemplary single source-single sink CCS chain scenarios involving CO2 stream compositions typical for pre-combustion capture and oxyfuel combustion. Recommendations for material selection for compression, transport and injection were derived for various CO2 stream compositions. To reliably control corrosion, a limitation of water contents to 50 ppmv is recommended for pipeline transportation of all CO2 streams. At geological storage conditions, the presence of either O2, NOx or SO2 only weakly affected fluid-mineral/rock interactions that still impacted geomechanical rock properties.
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.
Conventional concrete and UHPC performance-damage relationships identified using computed tomography
(2016)
To make significant advances in concrete engineering, it will be necessary to understand the behavior of cementitious materials at the microscale. To achieve this goal, the nature of damage initiation and growth needs to be understood at very small scales. This Research program sought to increase that understanding through the collection of microscale data using X-ray computed tomography (CT). The tensile and compression behavior of both ultra-high performance concrete (UHPC) and conventional concrete were investigated as a part of this
program. Relationships were identified between mechanical performance parameters, such as stiffness degradation and work of load, and cracking parameters, such as crack volume and crack surface area, that could be quantified mathematically and implemented into future finite element analysis (FEA) models. The results of this Research program have the potential to improve the accuracy and resiliency of numerical models and to provide insight to the materials engineering community concerning the optimal use of UHPC.
Im Rahmen des Forschungsprojekts „FIT“ wurden Ermüdungsfestigkeitsuntersuchungen an geschweißten Konstruktionsdetails, die häufig in Gründungsstrukturen von OffshoreWindenergieanlagen (OWEA), aber auch im Stahlbrückenbau eingesetzt werden, durchgeführt. Der Schwerpunkt der Untersuchungen wurde auf einseitig geschweißte Kreishohlprofile (KHP) gelegt. Für einseitig stumpfgeschweißte Kreishohlprofile wurden die derzeitigen auf unzureichender Versuchsbasis erstellten Kerbfalleinstufungen geltender Regelwerke überprüft. Hierzu wurden umfangreiche experimentelle Untersuchungen zur Ermüdungsfestigkeit dieses Details durchgeführt. Die den Ermüdungswiderstand maßgeblich beeinflussenden Parameter, wie vorhandene geometrische Imperfektionen und Schweißnahtausbildung, wurden identifiziert, bewertet und deren Einfluss im Rahmen numerischer Berechnungen untersucht. Basierend auf diesen Ergebnissen wurde eine Kerbfallempfehlung erarbeitet, die eine zutreffende Lebensdauerabschätzung ermöglicht. Diese Kerbfallempfehlung soll als Grundlage für die zukünftige Aufnahme in Normen und Regelwerke dienen.
This paper is a case study of complete substitution of sodium-metasilicate in zeolite Na-A synthesis by an electrostatic filterash (FA) arising in high amounts during silane waste incineration process.The silicate abundant FA is a suitable material for reinsertion in zeolite chemistry. This is shown in the presented investigation by the development of a model reaction process at low temperatures (50–60 °C) and short times (1.5–4 h). The experiments were performed under addition of NaAlO2 and variation of the alkalinity and the reaction period. Characterization and fine tuning of the process was mainly done by studying the kinetics of FA digestion and zeolite crystallization by XRD and chemical analyses (ICP-OES) of solutions and solids. It could be shown that pure FA was mostly dissolved (98%) in 8 m NaOH already after 1 h. Addition of NaAlO2 and crystallization for further 60 min under optimized conditions at 50 °C yielded to a suitable product. It consists of zeolite Na-A (92% by mass) beside some hydrosodalite (8% by mass). According to this low temperature short time process this study is a contribution for the development of energy efficient recycling solutions.
The effect of a nanometer scale confinement (pore sizes 7.5 nm down to 2.5 nm) on the vibrational density of states (VDOS) and on the molecular dynamics of Poly(dimethyl siloxane) (PDMS) and Poly(-methyl phenyl siloxane) (PMPS) is studied by inelastic Neutron scattering. The high penetration depth of neutrons makes neutron scattering a suitable tool for the study of confined systems. Moreover, Neutrons are sensitive to light nuclei therefore the confined polymers can be investigated directly, more or less independently of the confining host. Resulting findings are firstly, a reduction of the low frequency contributions to the VDOS below the Boson Peak frequency for both polymers. Including literature data, this reduction can be regarded as a more general feature for glass-forming systems confined by hard walls. Secondly, clear deviations in the temperature dependence of the mean squared displacement of
the confined molecules compared to the bulk were found close to the thermal glass transition temperature, whereas localized methyl group rotations were only weakly influenced. Furthermore, the molecular dynamics is accessed. The combination of neutron Time-of-Flight with neutron backscattering, thus covering a broad dynamical range from sub ps to ns, reveal clear influence from confinement on the intermediate incoherent scattering function S(q,t). The latter was obtained by combining the inverse Fourier transform of the individual dynamical structure factors measured by the both methods. The time and q dependence of S(q,t) are discussed in detail for the local methyl group rotations and the segmental dynamics, considering both the interaction of the segments with the pore walls and possible geometrical confinement effects.
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.
Semi-probabilistic method for residual lifetime of aluminothermic welded rails with foot cracks
(2016)
One of the most frequent and dangerous failure modes in continuous welded rails is fatigue crack Propagation terminated by brittle fracture. Due to the brittleness of the weld material and HAZ and the scatter in its mechanical properties, a statistical approach is necessary. The paper deals with surface cracks at the foot base of aluminothermic welded rails, developing a probabilistic methodology for determining the day by day prospective failure probability. The investigations presented here comprise weld material characterization, simulation of fatigue crack propagation and finally the determination of the failure probability using the Monte Carlo method. The effect of various parameters, such as axle weight, Initial crack size, residual stresses, fatigue crack propagation threshold and date of inspection were analyzed.
The results show that, independent of the date of the last inspection, almost any failure event happens in wintertime. This is in accordance with practical experience. However, from the proposed analysis it is evident that the main parameter controlling rail fracture is not only the minimum local temperature, but the temperature range over the whole year. Finally, the results are compared to the standard rail classification method.
Die drei technischen Regeln zu Gasen sind ergänzt und grundlegend überarbeitet worden. Die Neufassungen der TRGS 407 "Tätigkeiten mit Gasen - Gefährdungsbeurteilung" und der TRBS 3145/TRGS 745 "Ortsbewegliche Druckgasbehälter - Füllen, Bereithalten, innerbetriebliche Beförderung, Entleeren" sind bereits im Gemeinsamen Ministerialblatt veröffentlicht und können auf der Internetseite der BAuA heruntergeladen werden. Die Neufassung der TRBS 3146/TRGS 746 "Ortsfeste Druckanlagen für Gase" wurde im Ausschuss für Gefahrstoffe und im Ausschuss für Betriebssicherheit verabschiedet und ihre Veröffentlichung wird in den nächsten Wochen erwartet. Aufgabe der neuen technischen Regeln für Gase war es, die Lücken, die durch das Außerkrafttreten des umfangreichen bisherigen Regelwerks für Gase (insbesondere TRG, TRB und TRAC) entstanden waren, mit einem neuen, schlankeren und an der Gefährdung orientierten Regelwerk zu schließen. Die 2013 und 2014 veröffentlichten ersten Fassungen der drei technischen Regeln waren allerdings noch zu vervollständigen. Die bisher noch nicht eingearbeiteten Regelungen zu Acetylen, zu Füllanlagen für ortsfeste Druckanlagen für Gase sowie einige spezifische Regelungen zu Flüssiggas sind nun in die technischen Regeln zu Gasen integriert worden. Außerdem wurde die Überarbeitung genutzt, um Rückmeldungen aus der Praxis, insbesondere zur Aufstellung von ortsbeweglichen Druckgasbehältern, in die Neufassungen einfließen zu lassen. Die umfangreichen Ergänzungen führten dann auch zu einer Neustrukturierung der technischen Regeln, die vor allem der Verbesserung der Anwenderfreundlichkeit dienen soll. Der vorliegende Beitrag stellt die neugefassten Technischen Regeln zu Gasen vor und geht dabei insbesondere auf die aktuellen Ergänzungen und Änderungen ein.
Molybdenum disulfide (MoS₂) is a well-known solid lubricant for tribosystems running in vacuum or dry gases. Problems arise due to its sensitivity to humidity, which is a drawback for its application under ambient conditions. However, by using a physical vapor deposition (PVD) process, deposition parameters can be optimized not only to gain a coatings structure with favorable frictional properties but also to minimize the sensitivity to attack by water molecules. Therefore, an improved tribological behavior even under moist conditions can be achieved. MoS₂coatings are also candidates for being applied at cryogenic temperatures. They already have proven their suitability, e.g., for sliding support elements between superconducting magnets of the nuclear fusion-experiment Wendelstein 7-X. However, these coatings were exclusively produced for this particular application and the utilization for more common tribosystems may be precluded due to cost considerations. In view of a wider range of applications, pure and Cr containing PVD-MoS₂ coatings with an optimized structure were tested under varying environments including hydrogen gas and cryogenic temperatures. Results of the most promising variant are presented in this paper.