5 Werkstofftechnik
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Polyethylen hoher Dichte (PE-HD) wird als Werkstoff für Rohre und Behälter für den Transport und zur Lagerung von Gefahrgütern verwendet. Für die Beurteilung und technische Freigabe dieser Materialien ist insbesondere das Verständnis des Schädigungsmechanismus des langsamen, umgebungsbedingten Spannungsrisses (engl.: „environmental stress cracking“, ESC) essentiell. ESC tritt bei relativ geringen auf einen Werkstoff einwirkenden mechanischen Spannungen auf. An lokalen Fehlstellen (z.B. Defekte, Inhomogenitäten, Kerben) beginnend wächst ein Riss langsam durch das Material und führt nach gewisser Zeit zu einem charakteristischen, pseudo-spröden Bruch. Dabei wird das Risswachstum durch äußere Medieneinwirkung zusätzlich entscheidend beeinflusst. Dieses langsame Risswachstum wird als Hauptursache für das plötzliche und unerwartete Versagen von Polymerwerkstoffen angesehen.
Eine etablierte Prüfmethode zur Bewertung des Materialverhaltens gegenüber dieses Schädigungsmechanismus ist der Full-Notch Creep Test (FNCT), der für PE-HD Behältermaterialien üblicherweise unter Verwendung von wässrigen Netzmittellösungen (Arkopal N 100) durchgeführt wird. Die aus dem FNCT erhaltene Standzeit dient dabei als Bewertungskriterium für verschiedene PE-HD-Werkstoffe. In einer Studie wurden neben einer typischen Arkopal-N-100-Netzmittellösung praktisch relevante, organische Flüssigkeiten wie Biodiesel und Diesel als Testmedien verwendet, um deren Einfluss auf das ESC-Verhalten von PE-HD-Behältermaterialien zu charakterisieren. Neben der klassischen Standzeit-Auswertung erfolgte eine erweiterte Bruchflächenanalyse mittels Licht- (LM), Laserscanning- (LSM) und Rasterelektronenmikroskopie (REM). Insbesondere die LSM erlaubt eine schnelle und einfache Unterscheidung pseudo-spröder und duktiler Bruchbilder, die zur Beurteilung der Repräsentativität des FNCT für das dem Spannungsriss zugrundeliegenden langsamen Risswachstum von Bedeutung ist.
If the particle size decreases, the ratio of surface area to volume increases considerably. This provides benefits for all surface-driven processes that run faster or at lower temperatures than larger particles. However, handling and characterization of the nanopowders are much more difficult. Particularly polydisperse powders with irregular shape, as grinding products, represent a challenge. Granulometry in the submicron and nanoscale often leads to incorrect results without knowledge of particle morphology.
This presentation demonstrates potentials of using the volume-specific surface area (SV or VSSA) in the granulometric characterization of nanopowders, for instance, correlations between the volume-specific surface area and the median particle size are discussed considering the particle morphology and the model of the logarithmic normal distribution.
Moreover, the presentation deals with the optimal dispersion of nanopowders during sample preparation. Indirect ultrasound device with defined cooling was developed to prevent both contamination by sonotrode abrasion and sample changes by heat.
Successful granulometric characterization of nanopowders demands both improved dispersion technology and very often an effective combination of two or more measurement methods.
Im Vortrag werden das Messprinzip des Zentrifugen-Sedimentationsverfahrens erläutert und die Anforderungen der zugrundeliegenden Normen diskutiert. Es schließen sich umfangreiche Ausführungen zur praktischen Durchführung der Messung, insbesondere auch zu den vorbereitenden Arbeiten, sowie zur Auswertung der Rohdaten an. Nach einem Vergleich der Ergebnisse mit anderen Messverfahren, wird das Verfahren in einer Zusammenfassung bewertet.
Efficient studies of scarce or expensive materials require material saving processes. Therefore, a high yield concept for small batch preparation of ready-to-press powder is exemplarily presented for yttria stabilized nano-zirconia (d50 < 50 nm).
The concept involves small batch preparation in an ultrasound resonator, dispersant selection based on zeta potential measurements, evaluation of slurry stability using an analytical centrifuge, and preparation of ready-to-press powder by freeze drying.
Freeze drying offers key advantages. Process efficiency and high yield above 95 % are independent of sample size. The dried product does not require further mechanical treatment like milling or grinding. Side effects like migration of additives are avoided.
An optimized freeze drying process tolerates slurries with moderate stability. Thus, efforts for slurry development can be reduced. Generally, identifying a suitable dispersing agent requires only 3-5 zeta potential measurements. Slurry stability is rechecked using an analytical centrifuge, which also accounts for steric stabilization. An ultrasound resonator is used to disperse the powder without contamination, which becomes critical for small batches.
The described route is exemplarily presented for the development of an additive recipe for nano-sized zirconia powder, targeting for good pressing behavior and high green density. Therefore, a variety of binding and lubricating agents were tested.
Following the presented route, 80 g zirconia powder were sufficient to conduct a study including slurry development and five sample sets with varying composition, each set comprising five discs (d = 20 mm and h = 2 mm).
Glass powders are promising candidates for manufacturing a broad diversity of sintered materials like sintered glass-ceramics, glass matrix composites, glass bonded ceramics or pastes. Powder processing, however, can substantially affect sinterability, e.g. by promoting surface crystallization. On the other hand, densification can be hindered by gas bubble formation for slow crystallizing glass powders. Against this background, we studied sintering and foaming of silicate glass powders with different crystallization tendency for wet milling and dry milling in air, Ar, N2, and CO2 by means of heating microscopy, DTA, Vacuum Hot Extraction (VHE), SEM, IR spectroscopy, XPS, and ToF-SIMS. In any case, foaming activity increased significantly with progressive milling. For moderately milled glass powders, subsequent storage in air could also promote foaming. Contrarily, foaming could be substantially reduced by milling in water and 10 wt% HCl. Although all powder compacts were uniaxially pressed and sintered in air, foaming was significantly affected by different milling atmosphere and was found most pronounced for milling in CO2 atmosphere. Conformingly, VHE studies revealed that foaming is mainly driven by carbonaceous species, even for powders milled in other gases. Current results of this study thus indicate that foaming is caused by carbonaceous species trapped on the glass powder surface.
Up to now, oriented surface crystallization phenomena are discussed controversially, and related studies are restricted to few glasses. The vast majority of previous work does not consider possible effects of surface preparation and surrounding atmosphere. Moreover, very few observations of surface crystal orientation were made on separately grown crystals.
The aim of our project is to advance the basic understanding of oriented surface crystallization, e.g. whether preferred orientation of surface crystals results from oriented nucleation or reorientation mechanisms during early crystal growth. In both cases, crystal orientation may reflect the orientation of the glass surface or that of anisotropic active surface nucleation sites. Therefore, we focus on orientation of surface crystals separately growing under controlled conditions.
First results on diopside (MgCaSi2O6) and walstromite (BaCa2Si3O9) crystals growing from 18BaO·22CaO·60SiO2 and MgO·CaO·2SiO2 glass surfaces, respectively, indicate that different orientation mechanisms may occur.
Neighbored walstromite crystals were found to gradually reorient themselves when they are going to impinge each other during stepwise isothermal treatments (log η = 4,5 Pa*s) of polished glass samples. Nevertheless, no preferred crystal orientation was evident for separate crystals.
For diopside crystals growing from polished glass surfaces (1 μm diamond lapping foil), strong preferred orientation was observed for 3.5 to 85 min annealing at 850 °C. Electron Backscatter Diffraction (EBSD) studies showed that the c-axis of surface crystals is oriented parallel to the glass surface and that separated diopside crystals as small as 600 nm are already oriented. Studies on glass surfaces, polished with diamond lapping foils starting from 16 μm down to 1 μm grain, revealed that crystal orientation may scatter arround this preferential orientation and that this scatter progressively decreases with decreasing polishing grain size.
During their lifetime, polymer components subjected to mechanical loads and environmental influences show a loss of their mechanical properties required for their specific applications. In this respect, the craze-crack damage mechanism slow crack growth (SCG) is relevant for PE-HD components used in high-performance applications such as pipes and containers for the storage and transport of dangerous goods. SCG is considered to be the major failure mechanism in polyolefins and it typically occurs suddenly and unexpectedly. Due to the fields of application, SCG is a safety relevant issue. To test for the resistance of PE-HD pipe and container materials against SCG, the full-notch creep test (FNCT) is widely applied in Europe. In this study, SCG phenomena in PE-HD are investigated in detail based on an improved FNCT, especially including the consideration of the influence of environmental liquids effecting the damage mechanism. Using an enhanced fracture surface and a crack propagation analysis with imaging techniques such as light microscopy (LM), laser scanning microscopy (LSM), X-ray computed tomography (CT-scan) and scanning electron microscopy (SEM), detailed data concerning SCG are obtained.
The combined application of FNCT and such imaging techniques is explicitly advantageous and recommended to gain important information on damage occurring to PE-HD induced by mechanical stress and the influence of environmental liquids, which is essential within the Fourth Industry Revolution.
Charakterisierung von Hochtemperaturwerkstoffen durch Zug- und Ermüdungsversuche an Kleinproben
(2019)
Die Verwendung von miniaturisierten Probengeometrien in der mechanischen Prüfung ermöglicht die Entnahme des Probenmaterials direkt aus kritischen Bereichen wie Fügeverbindungen und ermöglicht die Prüfung von kleinen Bauteilen wie additiv gefertigten Strukturen. In der vorliegenden Arbeit werden exemplarisch die Ergebnisse von vergleichenden Zug- und niederzyklischen Schwingversuchen (LCF) an dem austenitischen Stahl AISI 316L und der Nickelbasislegierung IN718 vorgestellt. Die Prüfergebnisse der Kleinproben aus AISI 316L weisen die charakteristischen Eigenschaften des Werkstoffs auf, und die Analyse der Zug- und Ermüdungsdaten führt zu Werten, die den Literaturdaten weitgehend entsprechen. Der direkte Vergleich mit Standardprobendaten zeigt jedoch systematische Abweichungen bei Zugfestigkeit, Dehngrenze und Gleichmaßdehnung, die in diesem Beitrag diskutiert werden.
Der Fachbereich Mechanik der Polymerwerkstoffe befasst sich mit der Charakterisierung der mechanischen Eigenschaften und der Degradation von Polymeren und Faserverbundwerkstoffen, die in hochbeanspruchten, sicherheitsrelevanten Konstruktionen wie jenen des Flugzeugbaus, des Automobilbaus und der Windenergie-Industrie eingesetzt werden. Auch die Analyse der chemischen und physikalischen Eigenschaften von Polymeren zählt zu unserem Aufgabenbereich.
Das Spektrum reicht von der statischen Festigkeit über die Betriebsfestigkeit, die Messung bruchmechanischer und viskoelastischer Parameter bis hin zur Formulierung molekularer Schädigungsmechanismen.
Even for the basic measurements of material data for design and engineering of composite structures there is a need to upgrade standards. With a new shear frame test rig more precise values can be obtained.
With advanced methods in the research on the fatigue behaviour of FRP it was found a load level of infinite life for GFRP and CFRP. This is in the range of typical strain values of airliners and rotor blades in normal operation.
Statistically the mean time between damage events on rotor blades is 6 years (Deutscher Windenergie Report 2006). Due to imperfection in the production the shell structures get cracks after a few years fare before the designed life time. A shell test rig was built at BAM for efficient research on the effects of defects in production.
Test blades of ~10m are an efficient way for SHM research and evaluation of NDT-methods and blade geometry.