5 Werkstofftechnik
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Organisationseinheit der BAM
- 7.5 Technische Eigenschaften von Polymerwerkstoffen (30) (entfernen)
Eingeladener Vortrag
- nein (10)
This is the stable version of the full-notch creep test ontology (OntoFNCT) that ontologically represents the full-notch creep test. OntoFNCT has been developed in accordance with the corresponding test standard ISO 16770:2019-09 Plastics - Determination of environmental stress cracking (ESC) of polyethylene - Full-notch creep test (FNCT).
The OntoFNCT provides conceptualizations that are supposed to be valid for the description of full-notch creep tests and associated data in accordance with the corresponding test standard. By using OntoFNCT for storing full-notch creep test data, all data will be well structured and based on a common vocabulary agreed on by an expert group (generation of FAIR data) which is meant to lead to enhanced data interoperability. This comprises several data categories such as primary data, secondary data and metadata. Data will be human and machine readable. The usage of OntoFNCT facilitates data retrieval and downstream usage. Due to a close connection to the mid-level PMD core ontology (PMDco), the interoperability of full-notch creep test data is enhanced and querying in combination with other aspects and data within the broad field of materials science and engineering (MSE) is facilitated.
The class structure of OntoFNCT forms a comprehensible and semantic layer for unified storage of data generated in a full-notch creep test including the possibility to record data from analysis and re-evaluation. Furthermore, extensive metadata allows to assess data quality and reliability. Following the open world assumption, object properties are deliberately low restrictive and sparse.
Relation of craze to crack length during slow crack growth phenomena in high‐density polyethylene
(2024)
The craze‐crack mechanism occurring in high‐density polyethylene (HDPE) causing slow crack growth and environmental stress cracking is investigated in detail with respect to the relation of crack length and the related craze zone. This is essential for the understanding of the resulting features of the formed fracture surface and their interpretation in the context of the transition from crack propagation to ductile shear deformation. It turns out that an already formed craze zone does not inevitably result in formation of a propagating crack, but could also undergo ductile failure. For the examination, the full notch creep test (FNCT) was employed with a subsequent advanced fracture surface analysis that was performed using various imaging techniques: light microscopy, laser scanning microscopy, scanning electron microscopy, and X‐ray micro computed tomography scan. FNCT specimens were progressively damaged for increasing durations under standard test conditions applying Arkopal, the standard surfactant solution, and biodiesel as test media were used to analyze the stepwise growth of cracks and crazes. From considerations based on well‐established fracture mechanics approaches, a theoretical correlation between the length of the actual crack and the length of the preceding craze zone was established that could be evidenced and affirmed by FNCT fracture surface analysis. Moreover, the yield strength of a HDPE material exposed to a certain medium as detected by a classic tensile test was found to be the crucial value of true stress to induce the transition from crack propagation due to the craze‐crack mechanism to shear deformation during FNCT measurements.
Highlights
- Progress of crack formation in high‐density polyethylene is analyzed by different imaging techniques
- Determined growth rates depend on distinction between craze zone and crack
- The ratio of the present crack to the anteceding craze zone is validated theoretically
- The transition from crack propagation to ductile shear deformation is identified
- An already formed craze zone may still fail by ductile mechanisms
The dataset provided in this repository comprises data obtained from a series of full-notch creep tests (FNCT) performed on selected high-density polyethylene (PE-HD) materials (for further details, see section 1 Materials in this document) in accordance with the corresponding standard ISO 16770.
The FNCT is one of the mechanical testing procedures used to characterize polymer materials with respect to their environmental stress cracking (ESC) behavior. It is widely applied for PE-HD materials, that are predominantly used for pipe and container applications. It is based on the determination of the time to failure for a test specimen under constant mechanical load in a well-defined and temperature controlled liquid environment. The test device used here also allows for continuous monitoring of applied force, specimen elongation and temperature.
Slow crack growth (SCG) under the influence of external fluid media, usually termed environmental stress cracking (ESC), is still one of the most frequent origins of severe damage and failure of polymeric materials. For polyethylene (PE) this is relevant for mass products, like bottles for consumer products, but also for high-performance materials for pipes or industrial packaging, including containers for chemicals and other dangerous goods. Especially for high-density polyethylene (PE-HD) the susceptibility to SGC and ESC is depending on the complex interplay between molecular weight and architecture and the resulting semicrystalline morphology, especially the formation of tie-molecules.
A reliable assessment of the resistance against this damage phenomenon is essential for demanding as well as safety-critical applications and has to take into account suitable testing methodologies and conditions in combination with environmental media reflecting the properties representative for typical fillings and relevant components causing ESC. In this context a better understanding of different influencing factors, such as sorption, swelling or surface activity is necessary together with a detailed characterization of different stages of crack propagation and underlying mechanisms. Therefor well-established testing methods, such as the Full Notch Creep Test (FNCT), were complemented by detailed fracture surface analysis using e.g. LSM and SEM in combination with a time-dependent optical monitoring of the progressing crack growth.
For the crack growth also the ratio of fibrillated craze zone to crack opening is important for the deeper understanding of crack propagation and related material parameters which can be additionally addressed by X-ray computed tomography.
Packaging containers for dangerous goods that include aggressive liquids require that any packaging material that is based on high-density polyethylene has a high degree of stability and durability. This work is focused on testing the environmental stress cracking of the high-density polyethylenes used for such containers in contact with crop protection formulations, in particular, two model liquids established in Germany as standardized test media representatives for crop protection formulations containing the various admixtures typical for such products. One of the liquids is water-based and contains mostly surface-active ingredients, while the other is solvent-based and includes some emulsifiers. Originally established for pin impression tests, these model liquids and their individual components were here used for the first time as environmental media in the Full Notch Creep Test, which addresses the resistance against environmental stress cracking. The Full Notch Creep Test was carried out on five high-density polyethylene types with both model liquids, and also on one selected material with its components. The evaluation was focused on the fracture surface structures, which were visualized by a scanning electron microscope and by optical in situ imaging of the notch opening. While the water-based model liquid and its surface-active individual components induced environmental stress cracking with the characteristic pattern for a craze-crack mechanism and so-called brittle fracture on the surface, the solvent-based model liquid and its soluble ingredients exhibited rather ductile failure behavior, caused by the plasticizing effect on the polymer that reduced the yield stress of the high-density polyethylene.
For both cases, fracture surface analysis, together with side views of the crack opening, showed a clear relation between surface pattern, notch deformation (e.g., by blunting), or crack opening due to crack growth with time to failure and the solubility of the liquids in high-density polyethylene.
The crack propagation rate of environmental stress cracking was studied on high-density polyethylene compact tension specimens under static loading. Selected environmental liquids are distilled water, 2 wt% aqueous Arkopal N100 solution, and two model liquid mixtures, one based on solvents and one on detergents, representing stress cracking test liquids for commercial crop protection products. The different surface tensions and solubilities, which affect the energetic facilitation of void nucleation and craze development, are studied. Crack growth in surface-active media is strongly accelerated as the solvents induce plasticization, followed by strong blunting significantly retarding both crack initiation and crack propagation. The crack propagation rate for static load as a function of the stress intensity factor within all environments is found to follow the Paris–Erdogan law. Scanning electron micrographs of the fracture surface highlight more pronounced structures with both extensive degrees of plasticization and reduced crack propagation rate, addressing the distinct creep behavior of fibrils. Additionally, the limitations of linear elastic fracture mechanisms for visco-elastic polymers exposed to environmental liquids are discussed.
Das langsame Risswachstum (slow crack growth, SCG) sowie der umgebungsbedingte Spannungsriss (environmental stress cracking, ESC) sind relevante Schädigungsmechanismen für teilkristalline Werkstoffe auf Basis von Polyethylen hoher Dichte (PE-HD).
Der Vortrag gibt einerseits einen Überblick über die grundlegenden Struktur-Eigenschafts-Beziehungen in diesem Kontext, andererseits werden auch verschiedene praxisorientierte Prüfverfahren vorgestellt. Letztere wurden in gemeinsamen Forschungsprojekten von BAM und LBF mit dem Schwerpunkt Gefahrgutbehälter bzw. Pflanzenschutzmittel vergleichend untersucht und durch weitergehende Analytik ergänzt.
The fracture surface of slow and continuous crack propagation during environmental stress cracking of a semicrystalline polyethylene exhibits isotropic roughness exponents at the local scale but resolved across the macroscopic fracture surface a clear position dependence is found. The spatially resolved roughness exponent admits values in the range between 0.1 and 0.4, demonstrating nontrivial exponents in the small length-scale regime. Instead, they vary across the fracture surface according to the stress-state distribution, which suggests that the exponents are intimately linked to the locally dominating dissipation processes during craze cracking.
The phenomenon of environmental stress cracking is still a major issue in materials engineering as well as from a scientific perspective. Especially in the case of packaging materials made of high-density polyethylene, assessing the potential of premature damage due to environmental stress cracking is complex because of the large number of components in possible liquid filling goods. As a first guideline, the well-known effect of detergents and dispersants is usually considered, but the interplay with other components, such as organic solvents is often unknown. Particularly challenging in this respect are crop protection products, consisting of several different admixtures in addition to the biologically active ingredients. This study is based on two model liquids representing these admixtures that were established for testing in this context. The model liquids as well as their constituting components were used as liquid media in the Full Notch Creep Test to characterize the environmental stress cracking behavior of a typical high-density polyethylene. Complementary to the time-to failure of a notched specimen obtained from these tests, the crack opening was monitored optically, and the fracture surface was analyzed post-failure by laser scanning microscopy as well as scanning electron microscopy. Based on the results, the effect of various surfactants as well as the influence of organic solvents on environmental stress cracking are discussed.
Polyethylen hoher Dichte (PE-HD) ist ein weit verbreitetes Material für Transportbehälter, die oft für eine längere Nutzungsdauer vorgesehen sind. Insbesondere in diesem Fall können mikroskopische Schäden im Material auch weit unterhalb der Streckgrenze auftreten, die durch eine Spannungskonzentration verursacht werden, deren Ursprung in intrinsischen Materialfehlern oder äußeren Kratzern liegt. Mit fortschreitender Schädigung bilden sich Rissstrukturen, die von verstreckten Fibrillen aufgespannt werden, bis es zum Versagen dieser Fibrillen kommt und sich der Riss ausbreitet. Dieser Schadensmechanismus des langsamen Risswachstums kann durch eine Vielzahl von Umgebungsmedien beschleunigt werden und wird dann als "environmental stress cracking" (ESC) bezeichnet. Eine international normierte Methode zur Validierung der Spannungsrissbeständigkeit von PE-HD Materialien ist der „Full Notch Creep Test“ (FNCT).
Anhand von Bruchflächenauswertungen mittels Rasterelektronenmikroskopie und Laser-Scanning-Mikroskopie, werden die typischen Schädigungsstrukturen des ESC sichtbar. Die fibrillierten Strukturen des ESC auf der Bruchfläche von PE-HD ergeben sich besonders bei oberflächenaktiven wässrigen Umgebungsmedien. In Lösungsmittel-Umgebungsmedien, im Zusammenspiel mit PE-HD, kommt es aufgrund der plastifizierenden Wirkung zur Herabsetzung der Streckspannung und Bruchflächen aus dem FNCT veranschaulichen keine signifikanten Anzeichen des Schädigungsmechanismus ESC.