Ingenieurwissenschaften und zugeordnete Tätigkeiten
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Eingeladener Vortrag
- nein (429)
The manufacture of sintered glasses and glass-ceramics, glass matrix composites, and glass-bounded ceramics or pastes is often affected by gas bubble formation. Against this background, we studied sintering and foaming of barium silicate glass powders used as SOFC sealants using different powder milling procedures. Sintering was measured by means of heating microscopy backed up by XPD, differential thermal analysis, vacuum hot extraction (VHE), and optical and electron microscopy. Foaming increased significantly as milling progressed. For moderately milled glass powders, subsequent storage in air could also promote foaming. Although the powder compacts were uniaxially pressed and sintered in air, the milling atmosphere significantly affected foaming. The strength of this effect increased in the order Ar ≈ N2 < air < CO2. Conformingly, VHE studies revealed that the pores of foamed samples predominantly encapsulated CO2, even for powders milled in Ar and N2. Results of this study thus indicate that foaming is caused by carbonaceous species trapped on the glass powder surface. Foaming could be substantially reduced by milling in water and 10 wt% HCl.
Surface roughness, RZ, normal transmittance, ΤN, total transmittance, ΤT, and photovoltaic (PV) module efficiency, ηS, were measured for commercial solar glass plates and PV test modules identically sandblasted with different loads of quartz sand (200–400 μm), impact inclination angles, and sand particle speed. Measured data are presented versus the specific energy uptake during sand blasting, E (J/m2). Cracks, adhering particles, and scratch-like textures probably caused by plastic flow phenomena could be observed after sand blasting. Their characteristic size was much smaller than that of sand particles. After blasting and subsequent cleaning, the glass surface was still covered with adhering glass particles. These particles, cracks, and scratch-like textures could not be removed by cleaning. For sand blasting with α = 30° inclination angle and E = 30 000 J/m2, normal transmittance, total transmittance, and relative module efficiency decreased by 29%, 2% and ∽2%, respectively. This finding indicates that diffusive transmission of light substantially contributes to PV module efficiency and that the module efficiency decrease caused by sand erosion can be better estimated from total than by normal transmittance measurements.
The demand for improved castability and low angle grain boundary (LAGB) resistance has led to the addition of low contents of e.g., B, Hf, Zr or C, into large industrial gas turbine components made of Ni-base superalloy single crystals (SXs). Due to the long-term application of Ni-base superalloy SX components in the temperature regime > 1000 °C, the formation of carbides is highly probable, which could jeopardize mechanical properties, such as high cycle fatigue. In the present contribution, the effect of internal and external stresses on the nucleation and growth characteristics of M23C6 carbides is investigated. Creep experiments are performed on the Ni-base superalloy SX LEK 94, which shows a low C concentration (= 0.1 at. %), at 1020 °C under parallel and circularly notched tensile specimens at a nominal stress of 160 MPa in the crystallographic direction [001]. The carbides are then characterized via scanning (S) and transmission (T) electron microscopy (EM). Nucleation is enhanced in the dendritic cores, often as coalesced colonies, extending over micrometers within M-rich (M: Cr, Re, W, Mo) γ channels. Lath shapes with facets on {100} (parallel to growth direction) and {111} are common. These facets exist since early stages (Fig.1a) and later develop misfit dislocations (Fig.1b), preserving the orientation relationship {100}γ || {100}M23C6. Fig. 1c shows a region from the creep gage, where carbides interact with superdislocations in the γ’ phase. Possible mechanisms are discussed.
Geothermal brine is considered to be an aggressive
environment as it contains various dissolved salts.
Even though carbon steel is commonly used as a
construction material due to its machinability and
economical reason, it is susceptible to uniform and
localized corrosion in a high temperature and high
pressure system. Therefore, a coating system is
introduced to protect the carbon steel against
corrosion in such environment.
1. Carbon steel is susceptible to uniform corrosion in presence of oxygen, with corrosion rate of immersion at 150 °C of 0.39 mm/a.
2. Exposure test of carbon steel at 150°C and 10 bar (pressurized by Ar) results in pitting corrosion with depth of 19 µm and width 4 µm on average.
3. OCP measurement shows that the stability of measurement is reached after 40 hours of immersion in the solution.
4. EIS measurement is useful to observe the effect of temperature, immersion time, and coating composition on the corrosion processes of coated metals for use in geothermal application.
Ein neuartiger Modellierungsansatz für die Berechnung des transienten Temperaturfeldes beim Laserstrahlschweißen mit einer äquivalenten Wärmequelle wurde vorgestellt. Das numerische Modell wurde in zwei Studien unterteilt. Im ersten Teil wurde der Laserstrahlschweißprozess in einer stationären Schmelzbadsimulation untersucht. Die lokale Schmelzbadgeometrie und das Temperaturfeld wurden unter Berücksichtigung der Effekte der thermokapillaren und freien Konvektion, der latenten Wärme und der temperaturabhängigen Materialeigenschaften bis hin zur Verdampfungstemperatur ermittelt. Die Ergebnisse wurden benutzt, um eine äquivalente volumetrische Wärmequelle zu definieren. In der folgenden Studie wurde damit das transiente Temperaturfeld im geschweißten Bauteil berechnet. Die numerischen Ergebnisse wurden durch parallel laufende Experimente validiert.
Transient process simulation of heat transfer in laser beam welding with an equivalent heat source
(2017)
A multi-physics modelling framework developed for the prediction of the three-dimensional transient temperature field of the laser welding process is presented. The numerical model consists of two studies. In the first study, a steady-state CFD process simulation of full-penetration keyhole laser beam welding was performed. Considering the effects of latent heat, natural and thermo-capillary convection and temperature-dependent material properties up to evaporation temperature the local weld pool geometry and temperature field were obtained. These results were used in the second subsequent study, as an equivalent volumetric heat source, by the prediction of the transient thermal cycle during and after fusion welding. Here the energy input and the movement of the heat source were realized by a novel technique, making use of pointwise constraints and a moving mesh provided with helper lines and additional remeshing condition. The numerically calculated results were compared to experimentally observed weld pool shapes and time-temperature curves and show a very good agreement.
Der vorgestellte Modellierungsprozess dient zur Abschätzung einer geeigneten äquivalenten Wärmequelle und Berechnung des thermischen Verhaltens beim Laserstrahlschweißen. Die Methode Kombiniert die Vorteile von gägngigen Simulationsverfahren und reduziert die berücksichtigte Anzahl an physikalischen Aspekten und Kalibrierungsparameter. Durch die modellierten physikalischen Phänomene konnten die Informationen über die Strömung im Schmelzbad und dessen Einfluss auf die resultierende lokale Temperaturverteilung und folglich auf das transiente Temperaturfeld gewonnen werden. Dadurch wurde die Simulatioszeit(inkl. Kalibrierungsaufwand) auf weniger als einen Tag Rechenzeit verringert.
Ein neuer Ansatz bei elektrochemischen Korrosionsuntersuchungen kann durch den Einsatz von gelartigen Elektrolyten als Alternative zu wässrigen Prüfelektrolyten beschritten werden. Gelartige Elektrolyte ermöglichen minimalinvasive Untersuchungen an natürlich gebildeten Zinkdeckschichten. Dadurch können korrosionsrelevante Kennwerte ermittelt werden, die Aussagen zur Deckschichtbildung und zur Stabilität der gebildeten Deckschichten unter verschiedenen klimatischen Bedingungen erlauben. In diesem Beitrag wird anhand verschiedener Deckschichtzustände an Zink der Mehrwert von Untersuchungen mit gelartigen Elektrolyten für die Korrosionsforschung verdeutlicht.
Der Beitrag stellt eine neue Herangehensweise zur Bestimmung und Bewertung von Tafelfaktoren unter Verwendung gelartiger Elektrolyte und der Electrochemical Frequency Modulation (EFM) vor. Diese relativ neue elektrochemische Methode bietet die Möglichkeit, innerhalb einer Messung und in kurzen Messintervallen sowohl Polarisationswiderstände als auch Tafelfaktoren zu bestimmen. Ausgehend von einer umfassenden Parameterstudie wird gezeigt, dass ein direkter Zusammenhang zwischen den beiden Werten besteht, der mathematisch beschrieben werden kann. Die ermittelten B-Werte werden in diesem Beitrag vorgestellt und hinsichtlich ihrer Anwendbarkeit und Grenzen diskutiert.
Ein neuer Ansatz bei elektrochemischen Korrosionsuntersuchungen kann durch den Einsatz von gelartigen Elektrolyten als Alternative zu wässrigen Prüfelektrolyten beschritten werden. Gelartige Elektrolyte ermöglichen minimalinvasive Untersuchungen an natürlich gebildeten Zinkdeckschichten. Dadurch können korrosionsrelevante Kennwerte ermittelt werden, die Aussagen zur Deckschichtbildung und zur Stabilität der gebildeten Deckschichten erlauben. In diesem Beitrag wird anhand verschiedener Deckschichtzustände an Zink der Mehrwert von gelartigen Elektrolyten für die Korrosionsforschung verdeutlicht.
Ein neuer Ansatz bei elektrochemischen Korrosionsuntersuchungen kann durch den Einsatz von gelartigen Elektrolyten als Alternative zu wässrigen Prüfelektrolyten beschritten werden. Gelartige Elektrolyte ermöglichen minimalinvasive Untersuchungen an natürlich gebildeten Zinkdeckschichten. Dadurch können korrosionsrelevante Kennwerte ermittelt werden, die Aussagen zur Deckschichtbildung und zur Stabilität der gebildeten Deckschichten erlauben. Der Vortrag stellt das Promotionsthema vor und erläutert die Untersuchungsschwerpunkte.
Welding Technology
(2017)
Experimental determination and analysis of dynamic fracture toughness data of ductile cast iron
(2017)
Ductile Cast Iron materials (DCI) have become important structural materials. Neverthe-less, to draw maximum benefit from DCIs property potential, tailored testing methods must be provided. The established dynamic Jd-R and CTOD 5d-R curve procedures are based on material specifically developed, independent experimental techniques but pro-vide almost matching results. This can be seen as additional validation of the Jd procedure which was mandatory.
This technique is the first to provide a measurement of the full strain field locally in the immediate vicinity of the solidification front. Automatic identification of the cases that can be critical for the solidification crack formation the described procedure of the optical measurement allows the real material-dependent values of critical strain characterising the transition to hot cracking during laser welding processes to be determined. The local critical strain in vicinity of the solidification front has observed between 3.6 and 4.2%.
Im Arbeitskreis von Herrn Prof. Dr. Menzel (TU Braunschweig) wurde in Sievershausen ein Vortrag zum Thema „Self-healing and mechanically reinforced silicone rubber by the use of multifuctional capsules“ gehalten. Der Vortrag beginnt mit einer kurzen Motivation und einem Überblick über selbstheilende Materialien. Daraufhin werden die Ergebnisse zur Entwicklung eines selbstheilenden Silikonelastomers auf Basis von Kapseln, bestehend aus einem PDMS Kern und einer POS Hülle, dargestellt. Es folgt die Analytik, die auf DLS, TGA, UV/Vis und Fluoreszenzspektroskopie sowie SEM beruht. Der Vortrag endet mit einem Ausblick über zukünftige Arbeiten auf dem Gebiet.
Copolymers made of polycarbonate (PC) and polydimethylsiloxane (PDMS) are broadly applied in material science. High impact-stability and transparency are the marks of bisphenol-A polycarbonate. PDMS on the other hand excels in thermal stability, flame resistance and weatherability. Combining those favourable characteristics in a copolymer yields in a ductile but impact-resistant and flame retardant material. In order to understand the synthesis process and to improve the quality and characteristics of a copolymer, knowing its structure is essential. The challenge lies in the variety of heterogeneities like molecular mass-, block-size- and block-distribution.
This study addresses the structural characterization of PC-PDMS-copolymers using different liquid chromatographic techniques, including two dimensional combinations, hyphenated to MALDI-mass spectrometry and FTIR. The large difference in polarities of PC and PDMS is a challenge for liquid chromatography as well as ionization in MALDI. Nevertheless, we were able to differentiate between homopolymer and actual copolymer, clarify the presence of cyclic structures and gain information about the PDMS blocks
Im Rahmen eines BMWi Projekts der Fa. Innovent Jena, bei dem ein neuartiger optischer Sensor zur Bewertung der Oberflächenqualität und Reinheit von optischen Gläsern im Fokus stand, wurden die abbildende Ellipsometrie, die IR-Mikroskopie und die Weißlichtinterferenzmikroskopie als Referenzverfahren herangezogen. Mittels Brewster-Winkelmessungen konnten „Wolkenstrukturen“ identifiziert werden, die bei nachfolgenden Beschichtungsprozessen zu Schichtdefekten führen können. Außerdem wurden mittels Ellipsometrie Änderungen im Brechungsindex der Floatgläser (Luft- bzw. Zinnseite) nachgewiesen. Topographie Oberflächenmerkmale wie Welligkeit, Rauheit und Kreuzrillen konnten mittels Weißlichtinterferenzmikroskopie bzw. abbildender Ellipsometrie identifiziert werden.
Die Angabe der Messunsicherheit wird im Rahmen von Konformitätsbewertungen gefordert. Die Messunsicherheit gibt an, wie sicher der wahre Wert der Messgröße getroffen wird. Für ihre Ermittlung gibt es unterschiedliche Ansätze, allen voran der „Guide to the Expression of Uncertainty in Measurement“ (GUM). In der geplanten Auditoren- und Bewerterschulung sollen in einem Übersichtsvortrag "Uncertainty Budgets in Measurement and Testing for Surface Characterization: Ellipsometry, Hardness and Adhesion Testing" Herangehensweisen und Methoden zur Ermittlung der Messunsicherheit vorgestellt und anschließend anhand beispielhafter Anwendungen aus den Arbeitsbereichen der BAM erklärend untersetzt werden.
Mit dieser Schulung sollen die Auditoren und Bewerter der BAM befähigt werden, geltende Anforderungen zur Messunsicherheit handhaben und beurteilen zu können.
Der Vortrag widmet sich modifizierten Oberflächen zur Erhöhung der Kratzbeständigkeit sowie entspre-chenden Prüfmethoden und bewertet deren Praxis-tauglichkeit. Nach einer Übersicht zu Begriffen und Definitionen wird die wirtschaftliche Bedeutung der Kratzbeständigkeit aufgezeigt. Neben generellen Anforderungen an Mess-und Prüfverfahren hinsicht-lich Einsatzbereichen, Messunsicherheit und Validie-rung werden diverse Verfahren zur Erzeugung und Bewertung Einzel- und Vielfach-Kratzern nebst ent-sprechenden Normen vorgestellt. Die analytische Charakterisierung, werkstofftechnische Gesichts-punkte und eine Zusammenstellung aktuell gültiger Normen zur Kratzbeständigkeit schließen den Vortrag ab.
The talk addresses layer-based sensors for monitoring applications. In particular, sensor principles surface plasmon resonance (SPR), air-coupled ultrasonic, and magneto-optical coupling are discussed. Optical sensors on planar substrates are prepared by sol-gel, CVD- and PVD deposition techniques, ultrasonic sensors on planar and curved substrates are made by means of PVD processes, and magnetostrictive coatings for magneto-optical sensors are deposited on fibre-based Bragg gratings (FBGs) using PVD and ECD techniques. For all kinds of sensors design and function are explained and discussed, i.e. regarding sensitivity. It is shown that a) SPR enhanced ellipsometry is a promising tool for gas monitoring of hazardous gases, that b) thermos-acoustic and piezo-electric pulse-echo techniques are relevant for damage inspection of hidden volume defects of CFRPs, and that c) magnetostrictive-optical sensors with self-calibrating (magnetic reference field) function are useful for structural health monitoring in terms of strain sensors.
Der Vortrag widmet sich den Normenentwicklungen auf den Gebieten der
• Chemische Oberflächenanalyse und Rastersondenmikroskopie
• Elektronenmikroskopie und Mikrobereichsanalyse
• Prüfverfahren (zu Nanotechnologien)
• Hardness Testing
• Oberflächenmesstechnik im Mikro- und Nanobereich
• Kohlenstoff- und keramische Hartstoffschichten
• Mess- und Prüfverfahren für Schichten und Schichtsysteme
• Dünne Schichten für die Optik
• Coating Qualification Tests
Zur Erhöhung der Haft- und Klebfestigkeit von Niedrigenergie-Polymeren wie PTFE, PP und PE werden plasmabasierte Aktivierungen (Realisierung von dangling bonds) und Modifizierungen (Realisierung von functional groups) verwendet. Die Effizienz dieser Modifizierungen liegt für technisch raue Oberflächen bei ca. 10%, d. h. nur jedes zehnte C-Atom wird aktiviert oder modifi-ziert, weil sowohl LP- (Low Pressure) als auch AP- (Atmospheric Pressure) Plasmen nicht topo-graphietreu wirksam werden. Zudem ist die Lebensdauer der Aktivierung bzw. Modifizierung oft sehr kurz, liegt im Bereich von wenigen Minuten bis zu mehreren Stunden, d.h. zeitnahe Beschich-tung oder Verklebung in Prozessfolge sind unabdingbar.
Im Projekt „HARFE - Haftung, Reproduzierbarkeit, Festigkeit“ soll untersucht werden, in wie weit diese Defizite mittels Atomlagenabscheidung (ALD: Atomic Layer Deposition) vorbeschichteten Polymeren minimiert werden können. ALD-Prozesse sind zum einen topographietreu, zum anderen sowohl ohne als auch mit Plasmaunterstützung realisierbar.
Interlaboratory comparison: optical property classification of carbon-based films by ellipsometry
(2017)
The paper addresses the “INTERLABORATORY COMPARISON: OPTICAL PROPERTY CLASSIFICATION OF CARBON-BASED FILMS BY ELLIPSOMETRY” and the following points are discussed in more detail: Established classification for mechanical properties, Complementary classification for optical properties, Ellipsometry for determination of optical constants n-k plane as material fingerprint, Samples, participants & set-ups (samples: Japan, participants: Japan, Germany, France, set-ups: Japan, Germany, USA) and Results of interlaboratory comparison: thickness, n & k.
THz time domain spectroscopy (TDS) operates with short electromagnetic pulses. The sensitivity of the pulses to optical material property changes makes THz-TDS attractive for the detection of flaws in dielectric materials. Unfortunately, the X-ray computed tomography (CT) model holds only for THz-TDS reconstruction if minor refraction index differences between the inhomogeneities and the surrounding material matrix exist. A Time Domain SAFT algorithm has been developed to overcome the restrictions. THz time domain measurement on representative sample sets with inherent artefacts were performed to use them for the image reconstructions. The results will be presented and compared with optical surface images of the used test objects to evaluate the SAFT algorithm in relation to the reconstruction quality.
THz applications for NDT
(2017)
Electromagnetic waves in the frequency range between 0.1 and 10 THz are described as THz-radiation (T-ray). The ability to penetrate dielectric materials, to operate contactless and to be non-ionizing as well as be-ing insensitive to ambient temperatures makes THz technologies for NDT applications attractive especially where other techniques are not available or less suitable. Today T-rays are applied in non-destructive testing for quality control and condition monitoring issues. The operation is based on the combination of both transmission and/or reflection measurements and specially developed reconstruction procedures. Firstly, THz-TDS measurements will be presented to demonstrate the opportunities for spectroscopy and imaging of polymer materials. A SAFT algorithm and an Optical Layer-Model will be presented and discussed in more detail to demonstrate the opportunities of image reconstruction for visualization of the inner structures of op-tically and far infra-red opaque polymer composites.
Borosilicate glass has a wide range of technical applications due to its high chemical durability and thermal-shock resistivity. Here the effect of H2O on 16 Na2O, 10 B2O3,74 SiO2 glass is studied over a wide range of water contents from 0 to 8 wt.%. MIR spectra give evidence for the coexistence of strongly and weakly H-bonded hydrous species. Evaluation of NIR bands at 5200 cm-1 (molecular H2O), 4700 cm-1 (B-OH), and 4500 cm-1 (Si-OH) reveal that OH groups dominate up to ~6 wt.% H2O, with B-OH/Si-OH of ≈ 0.8. The incorporation of low amounts of H2O has strong impact on structure. NMR spectra of nominally dry glasses indicate a significant fraction (12 %) of 3-coordinated boron, but almost all boron is 4-coordinated after addition of 3 wt.% H2O. Raman spectra show that hydration results preferentially in transformation of Q4 to Q2 while Q3 remain unchanged, probably stabilized by bonding to BO4 tetrahedra. Viscosity measurements and differential thermal analysis give consistent results, confirming strong decrease of the glass transition temperature with addition of water from 849 K (dry) to 540 K (5 wt% H2O). An additional relaxation mechanism in hydrous glasses is inferred from dynamic mechanical analysis and is assigned to cooperative processes involving hydrous species. It is postulated that this relaxation mechanism plays an important role in crack growth kinetics.
Borosilicate glass has a wide range of technical applications due to its high chemical durability and thermal-shock resistivity. Here the effect of H2O on 16 Na2O, 10 B2O3,74 SiO2 glass is studied over a wide range of water contents from 0 to 8 wt.%. MIR spectra give evidence for the coexistence of strongly and weakly H-bonded hydrous species. Evaluation of NIR bands at 5200 cm-1 (molecular H2O), 4700 cm-1 (B-OH), and 4500 cm-1 (Si-OH) reveal that OH groups dominate up to ~6 wt.% H2O, with B-OH/Si-OH of ≈ 0.8. The incorporation of low amounts of H2O has strong impact on structure. NMR spectra of nominally dry glasses indicate a significant fraction (12 %) of 3-coordinated boron, but almost all boron is 4-coordinated after addition of 3 wt.% H2O. Raman spectra show that hydration results preferentially in transformation of Q4 to Q2 while Q3 remain unchanged, probably stabilized by bonding to BO4 tetrahedra. Viscosity measurements and differential thermal analysis give consistent results, confirming strong decrease of the glass transition temperature with addition of water from 849 K (dry) to 540 K (5 wt% H2O). An additional relaxation mechanism in hydrous glasses is inferred from dynamic mechanical analysis and is assigned to cooperative processes involving hydrous species. It is postulated that this relaxation mechanism plays an important role in crack growth kinetics.
Thickness determination in active thermography for one and multilayer semitransparent materials
(2017)
Flash thermography is a well-known non-destructive testing technique and has proven to be a valuable tool to examine material defects and to determine thermal material parameters and the thickness of test specimens. However, its application to semitransparent materials is quite new and challenging, especially for semitransparent multilayer materials like glass fiber reinforced polymer (GFRP). Here, in order to deduce the thickness of coated and uncoated semitransparent specimens as well as the depth of defects in such specimens by means of flash thermography, we apply an analytical model based on the quadrupole method by Maillet et al. to calculate the temperature development during the flash thermography experiment.
The model considers semitransparency of the sample and thermal losses at its surface. It supports the use of an arbitrary temporal shape of the heating pulse to properly describe the measurement conditions for different heat sources. By fitting the results of the analytical model to experimental data it is possible to determine the thickness of the specimen, provided the thermal material parameters are known, e.g., by calibration experiments with samples of the same material with known thickness.
We will show that thickness determination of semitransparent test specimens is possible both for transmission and reflection configuration, with and without a blackened sample surface at either front or back side of the sample. As an example, Figure 1 shows the experimentally obtained temperature differences of the surface of a blackened GFRP sample in transmission configuration with the coating facing the flash lamp (usual configuration, (a)) or the infrared camera (unusual configuration, (b)). Using the proposed method, the thickness of the sample can be determined for both configurations.
Impulsthermografie ist ein bekanntes zerstörungsfreies Prüfverfahren, welches sehr gut geeignet ist, um geometrische Eigenschaften von Materialfehler, thermische Materialparameter sowie die Dicke von Objekten zu bestimmen. Die Anwendung auf semitransparente Materialien ist jedoch recht neu und anspruchsvoll, insbesondere für semitransparente Mehrschichtmaterialien wie glasfaserverstärkte Kunststoffe (GFK). Um die Dicke beschichteter und unbeschichteter semitransparenten Proben mittels Impuls-Thermografie bestimmen zu können, verwenden wir ein analytisches Modell, welches auf der Quadrupol-Methode basiert.
Unser 1D-Modell berücksichtigt:
• die Semitransparenz der Probe,
• die Wärmeverluste an den Seitenflächen,
• beliebige zeitlichen Form des Heizimpulses (um die Messbedingungen für verschiedene Wärmequellen korrekt zu beschreiben),
• mögliche Flächenabsorption an der Vorder- oder Rückseite (für beschichtete Proben),
• und Mehrschichtsysteme.
Durch Anpassung der Ergebnisse des analytischen Modells an experimentelle Daten ist es möglich, die Dicke der Probe zu bestimmen, sofern die thermischen Materialparameter bekannt sind. Diese können z.B. durch Kalibrierungsmessungen an Proben desselben Materials mit bekannter Dicke bestimmt werden.
UCST-type thermoresponsive polymers (i.e. that phase separate from solution upon cooling) present a tremendous potential not only in aqueous media where they can be used in drug delivery, diagnostic and microfluidic applications, but also in water/alcohol mixtures, where they can be used for instance in sensing systems for alcohol-soluble drugs. However, only a few thermoresponsive polymers have been reported that present an UCST in a relevant temperature range and “green” solvents such as water or ethanol.
In this context, acrylamide-based monomers can be very useful building blocks for designing novel non-ionic UCST-type polymers because of their hydrophilic nature (with the appropriate side chain) and propensity to form hydrogen bonds. We will present our latest results on the UCST-type thermoresponsive behaviour of acrylamide- and 2,6-diaminopyridine-based homopolymers and copolymers in water or water/alcohol mixtures, and give some insights about the rational design of UCST polymers relying on H-bonding.
The demand for high-performance materials has strongly increased over the last decade. One way to improve their performance is to introduce material gradients as found in Nature (for example squid beaks, spider fangs, mussel byssal threads).
One path towards the achievement of such material gradients is the synthesis of hybrid (gradient) copolymers, for instance based on silane and organic monomers. Since not all gradient copolymers can be synthesized by utilising the reactivity ratios of the monomers, forced gradients have to be used. However, in order to obtain gradient copolymers at high conversions, living or pseudo-living copolymerizations have to be performed and so far only few hybrid (organic / inorganic) gradient copolymers have been reported. In this contribution we will present the synthesis of a novel organic / inorganic hybrid copolymer via controlled radical polymerization.
UCST-type thermoresponsive polymers (i.e. that phase separate from solution upon cooling) present a tremendous potential not only in aqueous media where they can be used in drug delivery, diagnostic and microfluidic applications but also in water/alcohol mixtures, where they can be used for instance in sensing systems for alcohol-soluble drugs. However, only a few thermoresponsive polymers have been reported that present an UCST in a relevant temperature range and “green” solvents such as water or ethanol.
In this context, acrylamide-based monomers can be very useful building blocks for designing novel non-ionic UCST-type polymers because of their hydrophilic nature (with the right side chain) and propensity to form hydrogen bonds. We will present our latest results on the UCST-type thermoresponsive behaviour of acrylamide- and 2,6-diaminopyridine-based homopolymers and copolymers in water or water/alcohol mixtures, and give some insights about the rational design of UCST polymers relying on H-bonding.
Unilamellar vesicles self-assembled in water from natural and synthetic phospholipids (liposomes), amphiphilic block copolymers (polymersomes), and more recently amphiphilic Janus dendrimers (dendrimersomes) as hollow soft structures in the nano size regime have attracted increasing interest as they can mimic primitive and contemporary biological membranes, and can be configured into biomimetic nanocapsules with application in nanomedicine such as gene, proteins and drug carriers or theranostics. Compared to other amphiphilic structures, the molecular structure of Janus dendrimers can be precisely controlled: by using the vast range of tools from organic chemistry their size, architecture, density, generation as well as the number of endgroups of the individual dendrons can be modified as desired. Unfortunately, the controlled production of the supramolecular aggregates made thereof is still a challenging task. Conventional batch-based techniques such as the solvent injection method or the film hydration method typically go along with a lack of control over mixing and thus over size, morphology and size distribution. The micromixer technology is a promising method for the controlled preparation of supramolecular assemblies as it allows control of mixing at microscale level. In addition, such microfluidic systems benefit from a high mixing efficiency, a low mixing time as well as from a reproducible and continuous synthesis.
Herein, we report on the microfluidic-controlled self-assembly of Janus dendrimers as dendrimersomes and the impact of the mixing parameters on the self-assembly process.
UCST-type thermoresponsive polymers (i.e. that phase separate from solution upon cooling) present a tremendous potential not only in aqueous media where they can be used in drug delivery, diagnostic and microfluidic applications, but also in water/alcohol mixtures, where they can be used for instance in sensing systems for alcohol-soluble drugs. However, only a few thermoresponsive polymers have been reported that present an UCST in a relevant temperature range and “green” solvents such as water or ethanol.
In this context, acrylamide-based monomers can be very useful building blocks for designing novel non-ionic UCST-type polymers because of their hydrophilic nature (with the appropriate side chain) and propensity to form hydrogen bonds. We will present our latest results on the UCST-type thermoresponsive behaviour of acrylamide- and 2,6-diaminopyridine-based homopolymers and copolymers in water or water/alcohol mixtures, and give some insights about the rational design of UCST polymers relying on H-bonding.
Vesicles self-assembled in water from natural and synthetic phospholipids (liposomes), amphiphilic block copolymers (polymersomes), and more recently amphiphilic Janus dendrimers (dendrimersomes) -5 as hollow soft structures in the nano size regime have attracted increasing interest as they can mimic primitive and contemporary biological membranes, and can be configured into biomimetic nanocapsules with application in nanomedicine such as gene, proteins and drug carriers or theranostics.
Compared to other amphiphilic structures, the molecular structure of Janus dendrimers can be precisely controlled: by using the vast range of tools from organic chemistry their size, architecture, density, generation as well as the number of end groups of the individual dendrons can be modified as desired.
Unfortunately, the controlled production of the supramolecular aggregates made thereof is still a challenging task. Conventional batch-based techniques such as the solvent injection method or the film hydration method typically go along with a lack of control over mixing and thus over size, morphology and size distribution. The micromixer technology is a promising method for the controlled preparation of supramolecular assemblies as it allows control of mixing at microscale level. In addition, such microfluidic systems benefit from a high mixing efficiency, a low mixing time as well as from a reproducible and continuous synthesis.
Herein, we report on the microfluidic-controlled self-assembly of Janus dendrimers as dendrimersomes and the impact of the mixing parameters on the self-assembly process.
Vesicles self-assembled in water from natural and synthetic phospholipids (liposomes), amphiphilic block copolymers (polymersomes), and more recently amphiphilic Janus dendrimers (dendrimersomes) as hollow soft structures in the nano size regime have attracted increasing interest as they can mimic primitive and contemporary biological membranes, and can be configured into biomimetic nanocapsules with application in nanomedicine such as gene, proteins and drug carriers or theranostics.
Compared to other amphiphilic structures, the molecular structure of Janus dendrimers can be precisely controlled: by using the vast range of tools from organic chemistry their size, architecture, density, generation as well as the number of end groups of the individual dendrons can be modified as desired.
Unfortunately, the controlled production of the supramolecular aggregates made thereof is still a challenging task. Conventional batch-based techniques such as the solvent injection method or the film hydration method typically go along with a lack of control over mixing and thus over size, morphology and size distribution. The micromixer technology is a promising method for the controlled preparation of supramolecular assemblies as it allows control of mixing at microscale level. In addition, such microfluidic systems benefit from a high mixing efficiency, a low mixing time as well as from a reproducible and continuous synthesis.
Herein, we report on the microfluidic-controlled self-assembly of Janus dendrimers as dendrimersomes and the impact of the mixing parameters on the self-assembly process.
Thermoresponsive polymers are of great importance in numerous applications such as bioseparation, drug delivery, diagnostic and microfluidic applications. Only few thermoresponsive polymers that present an upper critical solution temperature (UCST), i.e. phase separate from solution upon cooling, in a relevant temperature range and green solvents such as water or ethanol have been reported.
In this work two novel functional polymers of based on a 2,6-diaminopyridine motif, namely poly(N-(6-aminopyridin-2-yl)acrylamide) (PNAPAAm) and poly(N-(6-acetamidopyridin-2-yl)acrylamide) (PNAcAPAAm), were synthesized by free radical polymerization. The obtained polymers displayed UCST-type reversible thermoresponsive behaviour in water/alcohol mixtures. Insights into this phenomenon will be given based on visual observations, temperature-dependent turbidimetry and dynamic light scattering as well as 1H-NMR measurements. The UCST phase transition behaviour of the polymers was tunable by varying either the concentration of the polymer solution, the nature of the alcohol or the composition of the solvent mixture. The cloud point temperature of PNAcAPAAm was found to decrease with increasing alcohol content (MeOH, EtOH and iPrOH) in water/alcohol mixtures. Past a critical amount of EtOH or iPrOH in water the cloud point temperature of PNAcAPAAm increased by further addition of EtOH or iPrOH. These polymers with UCST behavior below 60°C in water/alcohol mixtures show great promises for the preparation of smart materials for sensing.
The sources of human error
(2017)
Perfect flawless performance does not exist. Yet we expect people in organisations with high safety and reliability demand to perform at their best so that the systems designed, operated and maintained by people do not fail. Still, even the best guarded systems fail. The goal of the study of human factors is avoiding the negative effects of the interaction between humans and technology as well as decreasing them to increase the well-being of people, functioning of the systems, and safety. This is achieved by identifying human performance problems, by applying human knowledge to the design of the system, and by utilizing gained knowledge to other similar situations that exist currently or will occur in the future.
This presentation will outline the definition, classification and misconceptions about human error and discuss the differences between traditional and contemporary understanding and prevention of human error. Practical examples from own research, highlighting the importance of identifying risks and appropriately dealing with them, will be given.
Dass die Zuverlässigkeit der ZfP eine sehr wichtige Rolle bei der Bewertung sicherheitsrelevanter Systeme spielt, ist bekannt. Laut dem modularen Zuverlässigkeitsmodell für zerstörungsfreie Prüfprozesse hängt die Zuverlässigkeit von der innewohnenden (physikalisch-technischen) Fähigkeit der Prüfsystems, den Anwendungsparametern, den menschlichen Faktoren und dem organisatorischen Kontext ab. Seit Einführung des Modells während des ersten Workshops zur Zuverlässigkeit der ZfP (European-American Workshop on Reliability of NDE) wurde das Modell in weiteren fünf Workshops stetig weiterentwickelt, diskutiert und an den Stand der Wissenschaft angepasst. Das Ziel dieser Publikation ist es, den aktuellen Stand der Diskussion und die neusten Fragestellungen der internationalen Zuverlässigkeitsgemeinschaft vorzustellen. Im Einzelnen werden die Entwicklung fortgeschrittener Modelle zur Bewertung der Probability of Detection (POD), Bewertungsansätze im Bereich Structural Health Monitoring und Fragestellungen zu den menschlichen Faktoren dargestellt. Besonderer Wert wurde sowohl auf die Entwicklung, als auch auf die Anwendung der Ansätze in der industriellen Praxis gelegt.
Die Grundlagen der Metallographie wurden in der zweiten Hälfte des 19. Jahrhunderts von Henry Clifton Sorby in England und Adolf Martens in Deutschland gelegt. Den verfügbaren Quellen nach erfolgten diese Arbeiten unabhängig voneinander. In diesem Beitrag werden die Beiträge von Adolf Martens und Emil Heyn zur Etablierung der Metallographie als ein eigenständiges Fach im Rahmen der Metallkunde dargestellt. Dabei werden Aspekte der Werkstoffprüfung, der Fraktographie und der Schadensanalyse einbezogen. Abschließend wird die führende Rolle dieser Pioniere der Metallkunde bei der Gründung der Deutschen Gesellschaft für Materialkunde (DGM) sowie des Deutschen Verbands für Materialforschung und -prüfung (DVM) gewürdigt.
Integration of screen-printed tunable BST thick films in LTCC modules for microwave applications
(2017)
Reconfigurable microwave components play an important role in modern communication systems to meet the increasing demands for functionality and flexibility of the systems. Various technologies, such as semiconductor technology, microelectromechanical systems (MEMS) or ferroelectric thin and thick films, are suitable for the realization of tunable microwave components. Ferroelectric materials are characterized by high tuning speeds, negligible power consumption and low manufacturing costs. In particular, ferroelectric thick films based on barium strontium titanate (BaxSr1-xTiO3, BST) are promising systems for use in the frequency range up to approx. 12 GHz. However, due to the high sintering temperatures above 1100°C for pure BST thick films, the fabrication of tunable components based on silver or gold electrodes is limited to planar structures, which are applied after the sintering process.
In this presentation, it will be shown the development of BST-ZnO-B2O3 composite materials for reducing the sintering temperature to 850-900°C. Furthermore, the material and component properties of these composites or rather corresponding MIM (metal-insulator-metal) varactors are presented and compared to planar-structured varactors. The LTCC integration potential of such fully screen-printed MIM varactors based on the developed low sintering BST composites are investigated by the fabrication of phase shifters embedded in LTCC modules.
The wetting behavior of material surfaces can be controlled by surface structures. We functionalized case-hardened alloyed carbon steel to modify the wetting behavior using ultrashort laser pulses (fs- to ps-range). The laser processing was performed by scanning the laser beam across the surface of initially polished flat sample material. An experimental study of the laser processing parameters (peak fluence, scan velocity, line overlap) rendered an assignment of different regimes associated with characteristic surface morphologies (laser-induced periodic surface structures, grooves, micro cones, etc.) possible. Analyzing the surface using optical as well as scanning electron microscopy allowed the identification of morphologies providing the optimum similarity to the natural skin of non-moisture havesting lizards. For mimicking skin structures of moisture-harvesting lizards, additionally a two-step laser processing strategy was established for realizing hierarchical microstructures. In this approach, micrometer-scaled capillaries (step 1) were superimposed by a laser-generated regular array of small dimples (step 2). Optical focus variation imaging measurements finally revealed the three dimensional topography of the laser processed surfaces derived from lizard skin structures. The functionality of these surfaces was analyzed in view of wetting and directional fluid transport properties. The results suggest possible applications of the laser-structured surfaces.
Der Vortrag gibt einen Überblick zu aktuellen Projekt- und Publikationsaktivitäten im BAM-Fachbereich 6.4 Technologien mit Nanowerkstoffen zum Thema “Laser-induzierte periodische Oberflächenstrukturen”. Die Herstellung solcher Mikro- und Nanostrukturen mittels ultrakurzer Laserpulse wird beschrieben, wodurch optische, chemische, mechanische oder biologische Oberflächenfunktionalsierungen vorgenommen werden können. Beispiele aus den Bereichen der Farbwirkung, der Benetzbarkeit mit Flüssigkeiten und der Reibungs- und Verschleissminderung werden erläutert.
Laser-induced periodic surface structures (LIPSS, ripples) are a universal phenomenon that can be observed on almost any material after the irradiation by linearly polarized laser beams, particularly when using ultrashort laser pulses with durations in the picosecond to femtosecond range. During the past few years significantly increasing research activities have been reported in the field of LIPSS, since their generation in a single-step process provides a simple way of nanostructuring and surface functionalization towards the control of optical, mechanical or chemical properties. In this contribution current applications of LIPSS are reviewed, including the colorization of technical surfaces, the control of surface wetting, the mimicry of the natural texture of animal integuments, the tailoring of surface colonization by bacterial biofilms, and the improvement of the tribological performance of nanostructured metal surfaces.
Within a current research project which is funded by the German Research Foundation (DFG) the influence of the size and the geometry of specimens on the spalling result in fire tests is going to be investigated at Bundesanstalt für Materialforschung und -prüfung (BAM). This paper describes some preliminary results and a newly developed test setup. The novel setup enables the efficient and precise quantification of spalling by using a special photogrammetric measurement system.
Die Präsentation gibt einen Überblick über die verschiedenen Aktivitäten der BAM im Bereich der Nanotechnologie mit den Schwerpunkten Nanopartikel und Nanosicherheit. Es wird sowohl die Transportsicherheit, als auch die Sicherheit von Batterien mit Nanopartikeln angesprochen. Verschiedene BAM-Projekte zum Thema Nano werden vorgestellt, beginnend mit relevanten REFOPlanprojekten über die Erstellung der OECD nanoTG110 bis hin zu EU-Projekten zur Standardisierung von Messungen an Nanomaterialien, hier insbesondere AEROMET, NanoDefine, NanoValid und EC4SafeNano.
Influence of solid-state-synthesis conditions on properties of oxide thermoelectric materials
(2017)
Calcium cobaltite and calcium manganate are promising oxide thermoelectric materials for applications between 600 °C and 900 °C in air to convert waste heat directly into electrical power. The solid state reaction, well known for large scale powder synthesis of functional materials, is used for the production of thermoelectric oxides. As a high temperature process, the powder synthesis consumes a lot of energy. In different studies, different synthesis conditions were used for the preparation of calcium cobaltite and calcium manganate powder. To the author’s knowledge, a systematic study of the synthesis conditions of calcium cobaltite and calcium manganate has not yet been published.
Therefore, the synthesis conditions for calcium cobaltite (temperature, dwell time, and particle size of raw materials) were studied with a statistical design of experiments (2³) and investigated regarding phase composition (XRD), densification and thermoelectric properties. The gained knowledge was used to optimize the solid state reaction of calcium manganate.
This study showed that a higher energy input (elevated temperatures, longer dwell times, or repeated calcinations) during powder synthesis does not improve but deteriorate the thermoelectric properties of calcium cobaltite. The same correlation was determined for the densification. As a higher energy input during powder synthesis leads to a larger grain size and therefore to a reduced sinter activity the densification at a given sinter profile is minimize as well as the thermoelectric properties. These results can be used to minimize the energy demand for the powder synthesis of oxide thermoelectric materials.
Calciumcobaltit ist eines der vielversprechendsten thermoelektrischen Oxide, welche zur direkten Wärmerückgewinnung genutzt werden können. Calciumcobaltit weist sowohl eine anisotrope Partikelform als auch anisotrope thermoelektrische Eigenschaften auf. Durch gezielte Ausrichtung der Partikel mittels Foliengießens und druckunterstützter Sinterung kann diese Anisotropie gezielt auf ein Bauteil übertragen werden. Die Partikelmorphologie kann durch Dotierung und Kalzinierung beeinflusst werden. Verschiedene Calciumcobaltitpulver wurden druckgesintert und das Gefüge sowie die thermoelektrischen Eigenschaften untersucht. Die Dotierung mit Bismut führte zu einer Verschlechterung der elektrischen Leitfähigkeit bei druckgesinterten Proben im Gegensatz zu undotierten Pulvern.
Pressure-assisted sintering of tape cast calcium cobaltite Ca3Co4O9 with varied powder compositions
(2017)
Calcium cobaltite Ca3Co4O9 is a promising p-type oxide thermoelectric material for applications between 600 °C and 900 °C in air. The properties and the morphology of Ca3Co4O9 are strongly anisotropic because of its layered crystal structure. By aligning the plate-like grains, the anisotropic properties can be assigned to the component. Hot-pressing of tablets is a well-known technology for grain alignment of Ca3Co4O9 and increases the thermoelectric properties in a/b-direction remarkably. However, hot-pressing of tablets is limited by the tablet size. An interesting alternative for larger components is the pressure assisted sintering of panels from tape casted layers. Tape casting already leads to grain orientation during green body forming. By combining tape casting and pressure assisted sintering (50 kN maximum force) of Ca3Co4O9, high densities and high thermoelectric properties can be reached for large components up to 200 mm edge length.
The morphology of Ca3Co4O9-grains can be designed by doping as well as by varying the powder synthesis conditions. For example Bi-doping increases the anisotropy of the grains, and reaction sintering of uncalcined powder leads to a fine grained microstructure and increases the electrical conductivity for pressure-less sintered specimens.
Doped and undoped Ca3Co4O9 powders were successfully tape cast with the doctor blade technique. Several layers of tape were stacked and laminated to 7 cm x 7 cm panels. These panels were sintered in a LTCC sintering press with combined in-situ shrinkage measurement. Pressure-less sintered panels from undoped powder have a 2.5 times higher electrical conductivity at room temperature than dry-pressed test bars with randomly orientated particles. By applying a uniaxial pressure of 10 MPa during sintering, the electrical conductivity (σ25°C = 15000 S/m) increases by the factor of 6 compared to the pressure-less sintered panels, which is in good accordance to the values reported in literature for conventional hot pressing [1, 3]. It is not possible to assign the increased anisotropy of Ca2.7Bi0.3Co4O9 to the pressure-assisted sintered panels, as Bi leads to an abnormal grain growth (up to 500 µm) with randomly oriented grains. This decreases the electrical conductivity (σ25°C = 5000 S/m). Such an abnormal grain-growth is reported for Bi over-doped Ca3Co4O9 but not because of hot-pressing.
Thermoelectric materials can convert waste heat directly into electrical power by utilizing the Seebeck effect. Calcium cobaltite Ca3Co4O9 is a promising p-type oxide thermoelectric material for applications between 600 °C and 900 °C in air. The properties and morphology of Ca3Co4O9 are strongly anisotropic because of its crystal structure of alternating layers of CoO2 and Ca2CoO3. The electrical conductivity is for example 13.5 times higher in a/b-direction than in c-direction. By aligning the plate-like grains, the anisotropic properties can be assigned to the component. Hot-pressing of tablets is a well-known technology for grain alignment of Ca3Co4O9 and increases the thermoelectric properties in a/b-direction remarkably. It also increases the relative density. However, hot-pressing of tablets is limited by the tablet size. An interesting alternative for larger components is the pressure assisted sintering of panels from tape casted layers. Tape casting already leads to a grain alignment during green body forming. By combining tape casting and pressure assisted sintering (50 kN maximum force) of Ca3Co4O9, high densities and high thermoelectric properties can be reached for large components up to 200 mm edge length.
Ca3Co4O9 was successfully tape casted with the doctor blade technique (binder: polyvinyl butyral, organic solvent). Several layers of tape were stacked and laminated to 5 cm x 5 cm panels. These panels were sintered with different applied pressures in a LTCC sintering press with combined in-situ shrinkage measurement. Pressure-less sintered panels have a 2.5 times higher electrical conductivity at room temperature than test bars with randomly orientated particles. By applying a uniaxial pressure of 10 MPa during sintering, the electrical conductivity increases by the factor of 6 compared to the pressure-less sintered panels. About 40 % linear shrinkage are reached in pressing direction. The Seebeck coefficient (S25 °C=146 μV/K) and the electrical conductivity (σ25 °C=15100 S/m) are in good agreement with the values published in literature for hot-pressed tablets.
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. 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, with particular focus on additively manufactured materials. I will also show how X-ray refraction computed tomography (CT) and Neutron diffraction can be highly complementary to classic absorption CT, being sensitive to internal interfaces and residual stress analysis, respectively.
Applications of X-ray refraction to non-destructive characterization of ceramics and composites
(2017)
X-ray refraction is analogous to visible light deflection by matter, with two main differences: 1- convex objects cause divergence (i.e., the refraction index n is smaller than 1), and 2- deflection angles are very small, from a few seconds to a few minutes of arc (i.e., n is near to 1). Trivially but importantly, deflection of X-rays is also sensitive to the orientation of the object boundaries. These features make X-ray refraction techniques extremely suitable to a) detect defects such as pores and microcracks, and quantify their densities in bulk (light) materials, and b) evaluate porosity and particle properties such as orientation, size, and spatial distribution (by mapping). While X-ray refraction techniques cannot in general image single defects, their detectability is simply limited by the wavelength of the radiation.
We will thereby show the application of X-ray refraction 2D mapping (topography) and tomography to different sorts of problems in ceramic science and technology: 1) Sintering of SiC green bodies; 2) Porosity analysis in diesel particulate filter silicates; 3) fiber de-bonding in metal and polymer matrix composites; 4) micro-cracking of glass-precursor -eucryptite. We will see that the use of X-ray refraction analysis yields quantitative results, also directly usable in available models.
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 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.
Aus Schmierstoffen gebildete Tribofilme bestimmen das Reibungs- und Verschleißverhalten von Tribosystemen neben der Fresslasttragefähgikeit. Die Kaltverfestigung stellt einen weiteren Mechanismus insbesondere zum Verschleißschutz dar. Unter Wälzreibung wird das funktionale Profil organischer und metallorganischer Tribofilme sowie von Kaltverfestigung verglichen, die auf verschiedenen Stahlmetallurgien innerhalb von 10.000 Überrollungen in einem 2Disk-Prüfstand erzeugt wurden. Dabei wurden Hertzsche Kontaktspannungen ober von P0max=2,14 GPa (FZG14) eingesetzt.
Unter Passivität versteht man den Korrosionsschutz durch dünne, festhaftende Schichten aus Korrosionsprodukten. Für den schadensfreien Einsatz nichtrostender Stähle ergeben sich daraus zwei grundsätzliche Anforderungen, die stets erfüllt sein müssen.
Erstens muss sich die Passivschicht vollständig ausbilden können. Dabei sind die Oberflächenausführung,die mechanische Bearbeitung,die Elementverteilung, Ausscheidungen, die Wärmeeinbringung z.B. bei der schweißtechnischen Verarbeitung, Anlauffarben, sowie die chemische Nachbehandlung bzw. Konditionierung der Oberflächen von großer Bedeutung. Zweitens muss die Repassivierung von möglichen Defektstellen unter den Einsatzbedingungen möglich sein. Für das Repassi-vierungsvermögen sind die Legierungszusammensetzung, mögliche kritische Betriebszustände, prozessbedingte Besonderheiten wie etwa Stagnationsbedingungen und Reinigungsprozesse von Bedeutung.
Im Vortrag werden die wesentlichen Grundlagen zum Verständnis der Korrosion metallener Werkstoffe in komprimierter Form vorgestellt. Die Herleitung und Bedeutung von Stromdichte-Potential-Kurven wird ausführlich erläutert und deren praktische Bedeutung für das Verständnis elektrochemischer Zusammenhänge bei der Korrosion herausgestellt.
Corrosion Resistance of the Super-Austenitic Stainless Steel UNS S31266 for Geothermal Applications
(2017)
Super-austenitic stainless steels cover grades with high chromium (20 to 27 %), high nickel (18 to 31 %) and high molybdenum (4 to 6 %) contents. Within this family, the 6%Mo high nitrogen grade S31266 was developed to combine the beneficial influence of chromium, tungsten, molybdenum and nitrogen on its mechanical and corrosion properties. Due to 22 % nickel, 24 % chromium and 0.4 % nitrogen additions, this alloy exhibits a very stable microstructure, being less prone to intermetallic phase precipitation than the other highly alloyed super-austenitic stainless steels.
This paper deals with the corrosion resistance of S31266 in artificial geothermal water with moderate salinity and low pH. Long-term static exposures and electrochemical tests were conducted at various temperatures to evaluate the pitting, crevice and stress corrosion cracking resistance of this material.
The results show that S31266 is resistant up to 220 °C. As a consequence, it can be a good candidate material for geothermal applications involving a highly corrosive environment, especially salinity and low pH.
Im ISO/TC 265 werden Normen zur Entwicklung, Konstruktion, Betrieb, Umweltplanung und -Management, Risikomanagement, Quantifizierung, Monitoring und Verifizierung sowie weitere Aktivitäten für die einzelnen Stufen der CCS-Prozesskette erstellt.
Als neuer Aspekt wurde die Zusammensetzung des CO2-Stroms angesprochen. In Form eines "State-of-the-Art-Reports" soll der derzeitige Kenntnisstand zusammengestellt werden. Dieses soll für einen späteren Normenentwurf als Grundlage dienen.
The evolution of the microstructure of multiphase metal matrix composite AlSi12CuNiMg with 7% vol. Al2O3 + 15% vol. SiC (short fibers and whiskers, respectively) was studied by synchrotron computed tomography. It comprehended as cast and after heat treatment conditions, as well as damage evaluation after ex-situ compression tests at room temperature. The volume fraction of different phases, their distribution, their orientation, and damage events are studied.
The influence on mechanical properties of the orientation of the planar random short fibres Al2O3 towards loading was investigated. Phase-specific load partition analysis for samples with fiber plane parallel and orthogonal to load, respectively, was performed by means of neutron diffraction (ND) during in-situ compression tests at room temperature. ND results proved that damage occurrence in the fillers strongly depends on the preferential orientation of those, playing a crucial role in the failure of the sample. The computed tomography observations confirm the damage observations from curves of load partition analysis of each phase.
The residual stress distribution of IN718 parts produced by Selective Laser Melting (SLM) technique was studied by means of neutron diffraction.
Two deposition hatching lengths were considered in the fabrication. Both lateral (building direction) and top (finishing) near-surface regions were characterized. Measurements on samples in as-built condition and after release from the plate proved the presence of stress gradients both in-plane and along the building direction.
As-built samples presented in top region a longitudinal stress relief for large hatching, whereas small one showed tensile stresses around (200MPa) in the middle, evolving towards compression at the tip of the sample (down to -300MPa). Towards the lateral edge, longitudinal stresses shifted also to compression. The transverse stresses for large hatching were relief in the middle, whereas for small hatching shifted to compression at the edge. As for the normal component, this was more homogenous: stress-relief was proved for large hatching and, in contrast, was in compression (-200MPa) for small hatching. In the building direction (lateral region from base plate to top) of the sample with large hatching all stress components showed tensile values near the base plate (particularly high for normal component around 300MPa), decreasing towards compression to the top, where they were almost released.
After release, in the top region, the longitudinal stress component for small hatching showed high compressive stresses in the central part (down to -250MPa). In contrast, for large hatching a stress relief was found. In the transversal direction, this behavior was inverted: a small hatching released stresses more effectively, while a large hatching presented high tensile stresses (around 200MPa). As for the normal component (i.e., building direction), the sample with small hatching was found in compression, while that with large hatching was stress-released or slightly in tension (around 100MPa). In the lateral surface region, all components showed similar behavior: a small hatching promoted high compressive stresses along the building direction, whereas a large hatching showed small tensile values at the bottom, which balance towards the top region. There is an overall shift of stresses in 3 directions towards tension when compared with as-built condition for top region. In contrast, the lateral region is stress-relief or shifted towards compression after cutting from baseplate.
In conclusion, hatching length parameter strongly influenced the 3D distribution of residual stress in SLM produced parts.
Composite-Druckgefäße für den Gefahrguttransport sowie für Wasserstoff- und Erdgasfahrzeuge bestehen aus einem lasttragenden Composite und einer gasdichten, metallischen oder polymeren Barriereschicht (Liner). Zur Untersuchung des Alterungsverhaltens solcher Composite-Druckgefäße wird in der BAM das interdisziplinäre Themenfeldprojekt COD-AGE durchgeführt. Ziel des Projektes ist die Entwicklung von Methoden und Modellen zur Beschreibung und Bestimmung des Alterungsverhaltens von Carbonfaser-Compositen (CFK) am Beispiel von Druckgefäßen, um eine bessere Vorhersage der Alterung und der sicheren Gebrauchsdauer zu ermöglichen.
Ein Schwerpunkt in diesem Projekt ist die Bereitstellung geeigneter ZfP-Methoden. Dabei geht es sowohl um versuchsbegleitende Prüfungen, als auch um die mögliche Entwicklung von Prüfeinrichtungen für den späteren praktischen Gebrauch. In diesem Vortrag werden Prüfsysteme und Prüfergebnisse der „konventionellen“ Wirbelstromprüfung vorgestellt. In einem ersten Schritt wurden Versuche an bereits geschädigten Druckgefäßen durchgeführt. Dabei wurden Druckgefäße mit den Materialpaarungen Stahl-CFK, Aluminium-CFK und Kunststoff-CFK untersucht. Die Dicken der CFK-Schichten reichten hierbei von ca. 4 mm bis ca. 8 mm. Anfangs wurden die Gefäße mit verschiedenen Sensoren von außen geprüft. Es konnten sowohl Beschädigungen des metallischen Liners, als auch Strukturen des CFK-Geflechts nachgewiesen werden. In einem zweiten Schritt wurden die Gefäße von innen geprüft. Hierbei bestand die besondere Herausforderung in der Prüfung eines Zylinders von 150 mm Durchmesser durch einen Zugang von nur 15 mm Durchmesser.
Mit den bei diesen Vorversuchen optimierten Prüfsystemen wurden dann begleitende Prüfungen bei Alterungsversuchen durchgeführt. In den Alterungsversuchen wurden Druckbehälter mit einem ca. 4 mm dicken Aluminiumliner und ca. 3,5 mm dicker CFK-Ummantelung untersucht. Typisches Einsatzgebiet solcher Flaschen sind Atemschutzgeräte bei der Feuerwehr. Die verschiedenen Prüfsysteme und die mit ihnen erzielten Ergebnisse werden vorgestellt.
A probabilistic finite elements analysis (FEA) of a tunnel lining subject to fire is presented. The probability distributions of the parameters related to the thermal analysis was considered in order to study the variability of the results and to carry out a reliability analysis. This assessment considered as random variables the thermo-mechanical properties of the concrete, the maximum heat release rate (HRR), the duration of the period of maximum HRR, the convective coefficient, the emissivity at the surface exposed to the fire, the air velocity within the tunnel, and the initial fire radius. The temperature-time curve was described by a correlation. An experimental design based on a Latin Hypercube Sampling algorithm was performed to define the input parameters to each analysis case. The definition of a limit state function based on the punctual strain status has permitted to carry out a reliability analysis.
Current interest in hydrogen gas as an energy source is growing due to its attractive properties such as high chemical energy density and the fact that its combustion produces water as by-product, qualifying this gas as an appealing clean energy source. In particular, the use of molecular hydrogen in automotive applications such as the hydrogen internal combustion engine (HICE) or hydrogen fuel cells is an excellent clean alternative.
Despite these promising opportunities, hydrogen gas has a distinct disadvantage as an everyday energy medium, that is, it is highly flammable. Hydrogen processing apparatuses should therefore be constantly monitored so that leaks are immediately detected. The implementation of direct sensing systems for H2(g) is thus a decisive factor for its application and acceptance as a clean energy source. Because the automotive market alone is already a mass market, these sensors do not only have to be reliable, robust and dimensionally small, but operation has to be simple and the device itself cost-effective. In addition, very low detection limits are a must as already escape of small quantities of H2(g) is directly related to public health and safety. Besides electrochemical or semiconductor sensors, optical sensors are especially appealing because the equipment is usually simple and accessible, easily miniaturized and measurements can be performed in situ and in real time.
If one cannot rely for instance on metallic palladium as interacting matrix, a major challenge for optochemical hydrogen sensors is to find a suitable material that fulfils all the requirements mentioned above and undergoes a dedicated indication reaction with H2(g). One such alternative can be Metal-Organic Frameworks (MOFs) which constitute a predefined, organized, mesoporous structure built up from metal ions and organic bridging ligands. With a myriad of building blocks being available, MOFs can be equipped with internal H2 reception sites that shall allow for selective and sensitive indication. For instance, if Pd ions are implemented in such a way that they express open metal sites (OMS), these OMS shall possess a strong affinity for hydrogen. If light absorbing and emitting organic ligands are additionally chosen, luminescent MOFs (LMOFs) can result that are perfect candidates for optical sensors, as changes at the analyte reception site can be effectively transduced into a measurable signal.
In this contribution, we intended to discuss the development of a new luminescent sensor material for the detection of the highly flammable H2(g). This sensor material is based on an LMOF assembled from Pd(II) and aromatic bridging ligands, the advent of hydrogen at the OMS in the LMOF producing distinct variations in the material’s optical properties.
S2XAFS: Time-resolved X-ray absorption spectroscopy in a ‘single-shot’ – First in situ applications
(2017)
The newly developed EXAFS set-up comprises both time- and spatially-resolved EXAFS information simultaneously in a single-shot. This facile, stable and scanningless set-up was tested at the BAMline @ BESSY-II (Berlin, Germany). The pri-mary broadband beam is generated by a filter/X-ray-mirror combination (bandpass). The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by an area sensitive detector, in a theta - 2 theta geometry. The first in situ measurements were successfully carried out and hereby presented. The case-study deals with research on Zn-based Metal-Organic-Frameworks (MOFs) that have potential for medi-cal/pharmaceutical applications. This hot topic of MOF research targets encapsulation of therapeutically relevant bio-macromolecules (e.g. Enzymes) for drug delivery applications. Questions regarding the influence of proteins on the coor-dination of Zn during MOF crystal growth and within the final MOF can be answered with this new setup. We were able to track structural changes within a 1s time resolution.
This presentation gives an overview on the activities and actions of the members of the forum of notified bodies for pyrotechnics under the European Directive 2013/29/EU. It comprises information on the recent members of the forum, details on conformity assessment procedures (e.g. module G), labelling of pyrotechnics, round robin tests and specific category depending Q&A.
Hydrous silicate and borate glasses of up to 8 wt% water were prepared using wet condition of melting under external pressure. Rheological experiments were conducted to determine the effect of the total water content on viscous flow and kinetic fragility. The findings indicate that dissolved water acts as a strong fluxing agent in both glass types. Water decreases particularly viscosity at the glass transition range, makes the viscosity-temperature curve "longer" and thus decreases kinetic fragility. Recent IR and NMR data are presented to link the dynamics of hydrous silicate and borate glasses with their structure particularly with regard to changes in the water-, silicon- and boron-speciation.
The novel heat treatment concept, “quenching and partitioning” (Q&P) has been devel-oped for high strength steels with enhanced formability. This heat treatment involves quenching of austenite to a temperature between martensite start and finish, to receive a several amount of retained austenite. During the subsequent annealing treatment, the so called partitioning, the retained austenite is stabilized due to carbon diffusion, which results in enhanced formability and strength regarding strain induced austenite to mar-tensite transformation. In this study a Q&P heat treatment was applied to a Fe-0.45C-0.65Mn-0.34Si-13.95Cr stainless martensite. Thereby the initial quench end temperature and the partitioning time were varied to characterize their influence on microstructural evolution. The microstructural changes were analysed by dilatometer measurements, X-ray diffraction and scanning electron microscopy, including electron back-scatter diffrac-tion. Compression testing was made to examine the mechanical behaviour. It was found that an increasing partitioning time up to 30 min leads to an enhanced formability with-out loss in strength due to a higher amount of stabilized retained and reversed austenite as well as precipitation hardening.
The quenching and partitioning (Q+P) heat treatment enables a higher deformability of high strength martensitic steels. Therefore, it is necessary to have some metastable austenite in the microstructure, which transforms in martensite during plastic deformation (TRIP-effect). This condition is guaranteed by the quenching and the additional partitioning treatment. Due to local carbon diffusion retained austenite is stabilized and a partial reversion of austenite from martensite occurs. The Q+P heat treatment was investigated for the martensitic stainless steel 1.4034 (X46Cr13) concerning the influence of partitioning time. In line with these efforts metallographic, XRD- and EBSD-measurements were performed to characterize the microstructural evolution. The mechanical experiments included mechanical testing with different strain rates. The reversion of austenite by the partitioning treatment could be detected with EBSD- and XRD-measurements. Further-more the results of the mechanical testing showed improved values of strength and de-formability because of the Q+P heat treatment.
The novel heat treatment concept of “Quenching and Partitioning” (Q&P) enables producing low alloyed martensitic steels with high strength and formability. Therefore austenite, retaining from a quenching temperature between Mf and Ms, is stabilised by carbon diffusion. This stabilised austenite transforms in martensite (TRIP effect) under mechanical loading. Current investigations on the Q&P heat treatment of martensitic stainless steels reveal a further enhancement of mechanical properties due to higher amounts of austenite. Thus a tensile strength of 1.800 MPa and a maximum elongation of 20 % are possible, while mechanical properties under compression are much higher due to a distinct SD effect.
The presentation aims to gain a further understanding of the Q&P heat treatment and the resulting mechanical properties for the steel X46Cr13, especially the mechanical behaviour under dynamic mechanical loading condition. Results of drop work and Split Hopkinson Pressure Bar test confirms the findings of quasi static compression test. Furthermore, Charpy impact tests show higher impact toughness compared to the common heat treatment of quenching and tempering (Q&T). Complementary investigations indicate a higher corrosion resistance of Q&P compared to Q&T.
In the future new types of lift charges for display Shells will enter the market. These types may not be based on black powder and therefore will show different Performance behaviors. The European standard series EN 16261 deals with the testing and assessment of display fireworks in order to satisfy the essential safety requirements which have to be met before placing these items on the EU market.
The aim of the study is to investigate how certain types of lift charges (NC based) influence the lift, tumbling and drift of cylindrical shells. In consequence, if the performance characteristics deviate strongly from those of typical black powder, safety related regulations in the EU and Germany might be affected, as well.
Atomic force microscopy based Infrared spectroscopy (AFM-IR) is a quickly evolving technique that provides chemical analysis and compositional mapping with spatial resolution far below conventional optical diffraction limits. This is possible since the detection method is based on a very sharp AFM tip which starts to oscillate when the sample starts to thermally expand (the changed is caused by the absorption of IR wavelength) where the thermal expansion is related to the IR absorption. This presentation briefly described the application of that new technique from polymer characterization and utilization of AFM-IR in material research, up to life science applications.
Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals. The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms. We recently introduced a setup enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. In this contribution, I will discuss our recent results investigating the formation of (polymorphic) cocrystals and metal phosphonates. First investigations of a mechanochemical synthesis under controlled temperature which allow determining the activation barrier are presented. Furthermore, in situ Raman spectroscopy coupled with thermography revealed a low temperature increase during milling reactions due to the mechanical impact and clear temperature increases as a result of the reaction heat.5 Our results indicate that in situ investigation of milling reactions offer a new approach to tune and optimize mechanochemically synthesized compounds.
Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals.1 The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms.2,3 We recently introduced a setup enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. In this contribution, I will discuss our recent results investigating the formation of (polymorphic) cocrystals and metal phosphonates.4 First investigations of a mechanochemical synthesis under controlled temperature which allow determining the activation barrier are presented. Furthermore, in situ Raman spectroscopy coupled with thermography revealed a low temperature increase during milling reactions due to the mechanical impact and clear temperature increases as a result of the reaction heat.5 Our results indicate that in situ investigation of milling reactions offer a new approach to tune and optimize mechanochemically synthesized compounds.
Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals.1,2 The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms.3,4 We recently introduced a setup enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy (Fig.1a) The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. In this talk I will discuss our recent results investigating the formation of (polymorphic) cocrystals.6-7 First investigations of a mechanochemical synthesis under controlled temperature (Fig 2a) which allow determining the activation barrier are presented.8 Furthermore, in situ Raman spectroscopy coupled with thermography revealed a low temperature increase during milling reactions due to the mechanical impact and clear temperature increases as a result of the reaction heat.
Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals.1,2 The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms.3,4 We recently introduced a setup enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy (Fig.1a) The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. In this talk I will discuss our recent results investigating the formation of (polymorphic) cocrystals.
Data about the creep of metals and their alloys at temperatures close to the melting point are very limited. The reason is that most engineering alloys are used at temperatures below 0.6-0.8 of their melting point, so, investigation of creep at higher temperatures has usually no practical relevance. For some special applications however it is important, in our case hot isostatic pressing (HIP) of single-crystal turbine blades cast from nickel-base superalloys. In order to remove porosity the blades are HIPed at temperatures above GammaP-solvus where superalloy has no strengthening GammaP-phase and therefore is very soft. E.g., the company Howmet Castings hips the superalloy CMSX-4 at 1288°C, which corresponds to a homologous temperature of about 0.97=1561 K/1612 K (solidus temperature). Knowledge about the creep of CMSX-4 at this temperature and understanding of the creep mechanisms are necessary to model the kinetics of pore closure during HIP.
CMSX-4 single-crystals of [001] orientation and few single-crystals of different orientations, [011], [123] and [111], were tested under creep conditions at 1288°C in the stress range between 4 and 16 MPa. At this temperature which is above the GammaP-solvus (for CMSX-4 1280°C) the superalloy has single phase structure representing the Gamma-solid solution of nickel strengthened by solute atoms. On creep curves of CMSX-4 single-crystals of different orientations measured at 1288°C/10 MPa it is seen that despite such a high homological temperature, 0.97, CMSX-4 shows very high anisotropy of creep rate. The average creep rate of [001] single-crystal in the range 0-30% strain is about 11.5 time faster than that for [111], a ratio, which is even higher than at the practically relevant temperatures 750-1100°, see e.g.. Approximation the strain rate – stress dependence by the Norton power law gave a stress exponent n of about 6 which is an indication of dislocation creep. The specimen shape after testing, analysis of traces of plastic deformation by electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) investigations indicate on dislocation slip on the octahedral system <011>{11-1}.This result however does not support the current doctrine that at high temperatures creep of metals and alloys are climb controlled. It is concluded from the obtained results that even at such a high homologous temperature, 0.97, dislocation movement by slip is more preferable than by climb if only relatively week obstacles are present like solute atoms and low angle boundaries (LABs).
It is remarkable that under used testing conditions the necking and recrystallization behavior of differently oriented single-crystals is very different. E.g., the [001] single-crystal showed very large local strain during necking, Phi=99.8%, and no recrystallization (see Fig. 3a), while the [111] single-crystal small necking, Phi=62%, accompanied by recrystallization. Such a specific deformation and recrystallization has to be undestood.
The obtained creep data of CMSX-4 was introduced in a finite element model in order to simulate pore closure during commercial HIP at a temperature of 1288°C.
- Impact tests of concrete blocks
- High energy facility for laminographic testing
- Laminographic arrangement
- Cross-Laminography
- Measurement range extension by detector tiling
- Reconstruction methods
- Fast “shift averaging” method “next to base plane”
- reconstruction --> Removal of reinforcement indications
- 3D-Data analysis
- Crack-Segmentation by „Template Matching“
An approach to develop an arc sensor for gap-width estimation during automated NG-GMAW with a weaving electrode motion is introduced by combining arc sensor readings with optical measurement of the groove shape to allow precise analyses of the process. The two test specimen welded for this study were designed to feature a variable groove geometry in order to maximize efficiency of the conducted experimental efforts, resulting in 1696 individual weaving cycle records with associated arc sensor measurements, process parameters and groove shape information. Gap width was varied from 18 to 25 mm and wire feed rates in the range of 9 to 13 m/min were used in the course of this study. Artificial neural networks were used as a modelling tool to derive an arc sensor for estimation of gap width suitable for online process control that can adapt to changes in process parameters as well as changes in the weaving motion of the electrode. Wire feed rate, weaving current, sidewall dwell currents and angles were used as inputs to calculate the gap width. Evaluation the proposed arc sensor model show very good estimation capabilities for parameters sufficiently covered during experiments.
Copolymer structure elucidation by multidimensional techniques with focus on UPLC x ESI-TOF-MS
(2017)
Structure elucidation of complex synthetic copolymers still represents a challenge. An one-dimensional separation technique cannot give the answer to the question: What are the molar mass distribution (MMD), the functionality distribution (FTD), the chemical composition distribution (CCD), the monomer sequence distribution (MSD), the topology differences within a single broad distributed polymer sample?
Since the first LC/ ESI-MS experiment of the Nobel prize winner John B. Fenn in 1984, the coupling of liquid chromatographic to mass spectrometric techniques gained a continuous rapid development.
Often the deficiencies of stand-alone methods can be bridged. LC, blind to structural information needs mass spectrometry as one of the most powerful detectors able to give detailed information on e.g. the repeat units, functionalization or copolymer composition of the chromatographic separated constituents. A separation prior to MS reduces radical the dispersity which is one of the reasons for failing of MS. Also problems with different ionization probabilities in complex mixtures can partly be overcame.
Different LC separation techniques as size exclusion chromatography (SEC), liquid adsorption chromatography (LAC), liquid chromatography at critical conditions (LCCC) and gradient elution liquid chromatography (GELC) combined with Matrix assisted Laser Desorption Ionization (MALDI) respectively Electrospray Ionization (ESI) Time of Flight (TOF) mass spectrometry are able to give information which otherwise are completely inaccessible. In some cases CID tandem mass spectrometry is applied. Fragmentation of suitable precursor ions resulted in typical fragment ion patterns. This technique enables an additional information on e.g. sequences, structural defects and topology of complex polymer mixtures.
Herein a new approach is demonstrated to provide evidence of different functionalities and short block sequences in statistical EO-PO copolymers. Furthermore silsesquioxane mixtures and Polyglycerols are investigated concerning occurring topology effects.
Structure elucidation of complex synthetic copolymers still represents a challenge. A one-dimensional separation technique cannot give the answer to the question: What are the molar mass distribution (MMD), the functionality distribution (FTD), the chemical composition distribution (CCD), the monomer sequence distribution (MSD), the topology differences within a single broad distributed polymer sample?
Is the coupling of liquid chromatographic separation techniques to mass spectrometry able to fill the gaps to a certain degree?
Different LC separation techniques as size exclusion chromatography (SEC), liquid adsorption chromatography (LAC), liquid chromatography at critical conditions (LCCC) and gradient elution liquid chromatography (GELC) combined with Matrix assisted Laser Desorption Ionization (MALDI) respectively Electrospray Ionization (ESI) Time of Flight (TOF) mass spectrometry are able to give information which otherwise are completely inaccessible. In some cases, CID tandem mass spectrometry is applied. Fragmentation of suitable precursor ions resulted in typical fragment ion patterns. This technique enables an additional information on e.g. sequences, structural defects and topology of complex polymer mixtures.
Often the deficiencies of stand-alone methods can be bridged. LC, blind to structural information needs mass spectrometry as one of the most powerful detectors able to give detailed information on e.g. the repeat units, functionalization or copolymer composition of the chromatographic separated constituents. A separation prior to MS reduces radical the dispersity which is one of the reasons for failing of MS. Also problems with different ionization probabilities in complex mixtures can partly be overcame.
The lecture will provide a series of examples where LC-MS has been applied to evaluate complex macromolecules and mixtures of these.
On- and offline coupling principles will be compared and the pros and cons of both mass spectrometric techniques will be discussed.
The phase transformation under various cooling rates and in different HAZ regions for high strength armour steel was analysed by dilatometry. To develop a Continuous Colling Transformation (CCT) diagram, the samples were heated up to a peak temperature of 1250 °C to achieve a coarse grained microstructure and then cooled down with a cooling time t8/5 varying from 3 s to 240 s. Analysis of dilatation curves revealed the austenite decomposition process, during which transformation temperatures were determined. The results showed martensitic transformations for all welding relevant cooling times.
Furthermore, to analyse different heat affected subzones of the weld, the peak temperature was varied between 550 °C and 1250 °C at a constant cooling time t8/5 of 6 s. The simulated coarse grained heat affected zone (CGHAZ) and fine grained heat affected zone (FGHAZ) showed only martensitic transformations with transformation temperatures below 400 °C. The steel exhibited an inhomogeneous hardness with hardening in the CGHAZ and FGHAZ and softening in the intercritical and subcritical HAZ. The physically simulated microstructure was validated by a real hybrid laser-arc weld microstructure.
Additive Manufacturing (AM) allows for the unique combination of building highly complex parts with integrated functional design. One particular design feature is known as lattice structures, which provide opportunities for innovative applications in the high-temperature regime of gas turbines. These structures require the development of reliable manufacturing methods to produce dependable structural integrity and geometrical accuracy. Consequently, the subsequent validation of these thin structures must also be examined in depth and differently than with current approaches.
In this study, a holistic assessment of Ni based high temperature lattice structures is pursued, utilizing a systematic design-follows-complexity approach. Single struts of different geometries and orientations are investigated first, then combined to a variety of unit cell types and finally multiplied to complex lattice structures.
Initial test trials with these thin structures proved a dependency of geometrical accuracy, microstructure and structural properties to the AM process setup. The trials underlined the need for design guidelines and a distinction between bulk and thin structures, as they showed differences in microstructural and mechanical behaviour. By application of high resolution, non destructive characterization methods such as computer tomography (CT and µCT), evaluation of defects and the thin structures’ metrology has been performed. First results revealed a number of defects compromising the structural integrity and therefore limiting the lifing behaviour. This was confirmed in destructive testing (e.g. tensile and compression). Furthermore, it was proven that the distribution, the number, the size and the type of defects are also dependent on the AM process setup.
While there are large potentials for use of lattice structures in gas turbine applications, the experiments indicate the strong need for an increased understanding of manufacturing and design for these complex structures and that this gap needs to be bridged.
Die thermomechanische Ermüdung (TMF) von Bauteilen kann heutzutage mit der Finite-Elemente (FE) Methode simuliert werden. Dafür werden komplexe viskoplastische Stoffgesetze benötigt, welche in der Regel in kommerziellen FE Programme nicht zur Verfügung stehen. Im Vortrag wird gezeigt wie solche Stoffgesetze mit Hilfe von benutzerdefinierten Subroutinen in kommerzielle Finite-Elemente Programme implementiert werden können. Es wird auf die Vor- und Nachteile einer expliziten oder impliziten Integration der Entwicklungsgleichungen für die inneren Variablen hingewiesen. Schließlich wird ein Postprozessingstool beschrieben, mit dem die Überlagerung einer niederfrequenten (TMF) und einer hochfrequenten (HCF) Belastung im Bauteil analysiert werden können.
The technological importance, the regularity of the microstructure and the complexity of the mechanical behavior of single crystal superalloys have motivated the development of a large number of mathematical models of the mechanical behavior of these alloys in the last two decades. While crystal viscoplasticity has proven to be an efficient framework to account for their anisotropy, several issues are still challenging. Indeed, most models consider that octahedral and cubic slip systems contribute to the largest part of the plastic deformation. However, the exact nature of cubic slip is still controversial and the precipitates can be sheared by <112> slip systems at intermediate temperatures, which largely influence the dependence of the flow rate on the orientation under creep conditions. Due to the different strengths of the matrix and the precipitates and the large volume fraction of the precipitate phase, a complex distribution of internal stresses exists, which can difficultly be captured by the conventional back stress models of plasticity. In addition, at high temperature, the microstructure degrades and the residual mechanical strength is reduced. The driving force for this microstructure degradation is intimately connected to the distribution of the internal stresses. As a result of this complexity, a large number of tests are usually required to fully characterize the mechanical behavior of single crystal superalloys. This in turn largely impedes the implementation of inelastic modeling in the industrial praxis.
The lecture summarizes the principal types of constitutive models for single crystal superalloys and reviews some recent advances in this area. In particular, it is shown how simulations at the microstructure scale level combined with conventional testing and microscopic analysis helped to improve our understanding of the mechanical behavior of single crystal superalloys. Directional coarsening, the importance of internal stresses, orientation dependency and the corresponding modeling issues are discussed. Also open questions are highlighted.
Gas turbines are widely used for a variety of purposes including power generation, compression or as jet engines in aircrafts. The critical components of a gas turbine are the high-pressure turbine blades which operate under severe conditions. These include thermo-mechanical loadings over temperatures ranging from room temperature up to 1100°C.
While a large number of constitutive models for single crystals have been proposed, most applications are restricted to special loading scenarios, temperature range and deformation mechanisms. In particular, a number of models are focused on pure creep. Only a few papers consider application of both creep and fatigue. Applications of the constitutive models to long-term stress relaxation are even scarcer. The new model assumes deformation-induced softening and can properly reproduce the viscous behavior at different time scales.
The model has been calibrated with the uniaxial tests at 800°C and 950°C in [001], [011] and [111] specimens of a nickel-basis superalloy. The predicted creep, short- and long-term relaxation and cyclic tests are in reasonable agreement with the experimental observations.
The investigation of creep behavior of the single crystal superalloy CMSX-4 at 1288°C is important for the understanding of deformations mechanisms under hot isostatic pressing (HIP). This treatment is used to increase the lifetime of single crystal superalloys by reducing the number of cavities. The understanding of the internal processes during this treatment is still limited due to the material being not single-phase at room temperature, the extreme conditions of HIP and the complexity of the material.
The result of predicting the pore shrinkage rate using classical crystal plasticity was not satisfying. A more complex model has been implemented, now taking the heterogeneity of dislocation sources into account. By introducing a dislocation density, one can describe the transport, nucleation and interaction of dislocations.
Ziel war die Entwicklung neuer Konzepte für die Herstellung sicherer, energieeffizienter und erschwinglicher Materialien für Gebäudehüllen und Innenwände für ein gesünderes Wohnklima.
Es werden Komposit-Fertigteile aus UHPC mit Wärmedämmung aus Porenbeton und aus Textilfaserbeton mit Wärmedämmung aus Schaumbeton vorgestellt.
Diskutiert werden die Strategien zum Erreichen einer erhöhten Dauerhaftigkeit und Ressourceneffizienz sowie zur Erzeugung multifunktionaler Oberflächen.
Ziel war die Entwicklung neuer Konzepte für die Herstellung sicherer, energieeffizienter und erschwinglicher Materialien für Gebäudehüllen und Innenwände für ein gesünderes Wohnklima.
Es werden Komposit-Fertigteile aus UHPC mit Wärmedämmung aus Porenbeton und aus Textilfaserbeton mit Wärmedämmung aus Schaumbeton vorgestellt.
Diskutiert werden die Strategien zum Erreichen einer erhöhten Dauerhaftigkeit und Ressourceneffizienz sowie zur Erzeugung multifunktionaler Oberflächen.
The presentation focuses on the current state of the optical spectroscopic studies on plasmon enhanced upconversion luminescent processes of silica-metal core-shell nanocomposites. A general introduction of the upconversion process, the theoretical basis of plasmonic enhancement, the theoretical requirements in regard to NP architecture for plasmon enhanced UC will be outlined. The first proof-of-concept measurements show the difficulty in realization the theoretical measurement parameters in laboratory conditions and underline the need for shifting the experiments to single particle level.“
The present paper investigates the electromagnetic porosity reduction in partial penetration laser beam welding of 6 mm aluminum die casting AlSi9MnMg. Applying an electromagnetic field, a significant reduction of the porosity as well as smoothing of the surface of aluminum die casting can be observed. Starting from the reference case without an electromagnetic support, the porosity was reduced by 76 %. Especially big pores can be removed from the weld pool effectively due to their beneficial volume-to-area ratio whereas very small metallurgical pores tend to remain within the weld pool even when higher magnetic flux densities are applied.