TY - JOUR A1 - Schilling, Markus A1 - Niebergall, Ute A1 - Böhning, Martin T1 - Full notch creep test (FNCT) of PE-HD – Characterization and differentiation of brittle and ductile fracture behavior during environmental stress cracking (ESC) N2 - The damage mechanisms slow crack growth (SCG) and environmental stress cracking (ESC), relevant for PE-HD materials are characterized based on improved full notch creep testing (FNCT) of two selected typical PE-HD materials for container applications. In this context, a distinction of the failure mechanisms as well as a categorization of involved media is suggested. Employing a novel FNCT device, elongation data were obtained in addition to conventional time-to-failure results of stress-dependent as well as temperature-dependent measurements. Changes in failure behavior, as determined by fracture surface analysis based on light microscopy (LM) and laser scanning microscopy (LSM), are correlated with FNCT results and used to introduce an additional possibility for the identification of brittle/ductile fracture behavior. KW - Environmental stress cracking (ESC) KW - Slow crack growth (SCG) KW - Full notch creep test (FNCT) KW - High-density polyethylene (PE-HD) PY - 2017 U6 - https://doi.org/10.1016/j.polymertesting.2017.09.043 SN - 0142-9418 SN - 1873-2348 VL - 64 SP - 156 EP - 166 PB - Elsevier CY - Amsterdam AN - OPUS4-42484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Böhning, Martin A1 - Oehler, H. A1 - Alig, I. A1 - Niebergall, Ute T1 - Environmental stress cracking of polyethylene high density (PE-HD) induced by liquid media – Validation and verification of the full-notch creep test (FNCT) T1 - Umgebungsinduzierte Spannungsrissbildung von Polyethylen- Werkstoffen hoher Dichte durch flüssige Medien – Validierung und Verifizierung des Kriechversuchs an Probekörpern mit umlaufender Kerbe N2 - The full-notch creep test (FNCT) is widely used to characterize the slow crack growth (SCG) behavior of polyolefin materials in “inert” media as well as effects of environmental stress cracking (ESC) in which the medium has decisive influence on damage mechanism and time to failure. The test is of greatest importance for pipe and blow molding types of polyethylene, high density (PE-HD). Usually the full-notch creep test is applied as a standardized testing method (ISO 16770) using a few universal liquid media, such as solutions of Arkopal N 100. In our study, selected relevant polyethylene, high density materials are investigated also in real media – practical formulations as well as representative pure chemicals – and influences of temperature and geometry of specimen and notch are explicitly addressed. Furthermore, the investigations comprise also the environmental stress cracking behavior of polyethylene, high density in media that are sorbed to a significant extent – examples are diesel and biodiesel – based on comparison with samples previously saturated with those media. Thus, also the underlying diffusion controlled sorption process has to be assessed before. The investigations were performed using a full-notch creep testing device with 12 individual sub-stations, each equipped with individual electronic stress and temperature control and continuous online monitoring of the specimen elongation. N2 - Der Kriechversuch an Probekörpern mit umlaufender Kerbe (FNCT) wird flächendeckend angewendet, um das Verhalten von Polyolefinen sowohl gegenüber langsamen Risswachstums (SCG) bei Kontakt mit „inerten“ Medien als auch gegenüber umgebungsbedingtem Spannungsrisswachstum (ESC), bei welchem das umgebende Medium entscheidenden Einfluss auf den Schädigungsmechanismus und die Standzeit hat, zu charakterisieren. Der Test ist von großer Bedeutung bei der Analyse von hochdichten Polyethylen-Typen, die als Rohr- und Blasformwerkstoffe angewendet werden – dabei besonders für Transport und Verpackung von Gefahrstoffen, aber auch für weitere Hochleistungsanwendungen. Üblicherweise wird der Kriechversuch an Probekörpern mit umlaufender Kerbe als Normmethode (ISO 16770) unter Verwendung einiger weniger universeller Modellflüssigkeiten, wie z. B. Arkopal N 100, durchgeführt. In dieser Studie werden ausgewählte, marktrelevante Polyethylen-Werkstoffe hoher Dichte in realen Medien – praktisch verwendete Gefahrgüter sowie repräsentative reine Chemikalien – untersucht und explizit die Einflüsse von Temperatur und Prüfkörper- sowie Kerbgeometrie adressiert. Weiterhin beinhalten die Untersuchungen die Analyse des umgebungsbedingten Spannungsriss-Verhaltens von Polyethylen hoher Dichte in Medien, die maßgeblich vom Werkstoff sorbiert sind – beispielsweise mit Kraftstoffen wie diesel und biodiesel – basierend auf dem Vergleich mit vorgesättigten Probekörpern. Der dabei vorliegende diffusionsgesteuerte Sorptionsprozess muss dementsprechend zuvor evaluiert werden. Alle Untersuchungen wurden mithilfe einer Kriechversuchsanlage an Probekörpern mit umlaufender Kerbe mit 12 Stationen durchgeführt, welche jeweils mit einer individuell ansteuerbaren elektronischen Spannungs- und Temperatursteuerung sowie fortwährender Online-Überwachung der Prüfkörperdehnung ausgestattet sind. KW - Full-notch creep test (FNCT) KW - Polyethylene (PE-HD) KW - Environmental stress cracking (ESC) KW - Slow crack growth (SCG) KW - Biodiesel PY - 2017 U6 - https://doi.org/10.1002/mawe.201700065 SN - 1521-4052 SN - 0933-5137 VL - 48 IS - 9 SP - 846 EP - 854 PB - Wiley-VCH CY - Weinheim AN - OPUS4-41885 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Schilling, Markus T1 - Environmental Stress Cracking (ESC) and Slow Crack Growth (SCG) of PE-HD induced by external fluids N2 - High-density polyethylene (PE-HD) is widely used as a packaging material. Typical applications are pipes and containers for storage and transport of dangerous goods. For these applications, the understanding of the craze-crack damage mechanisms slow crack growth (SCG) and environmental stress cracking (ESC) is of importance. Since these mechanisms are considered to be the major causes of failure, their understanding is essential for inspection and release of those materials. A well-established test method for the assessment of these damage mechanisms is the full-notch creep test (FNCT). It is used in this study for a detailed investigation of crack propagation phenomena in PE-HD container materials under the influence of different fluids such as air, water and aqueous detergent solutions (Arkopal N 100) as well as biodiesel and diesel. Based on the results of the FNCT, a classification scheme of different fluids is proposed, which allows for an assignment of the respective damage mechanisms. Hereby, it is differentiated between (i) inert, (ii) purely surface-active and (iii) additionally sorptive, bulk-active fluids with respect to SCG. If the test fluid changes the intrinsic properties (at the surface or in the bulk), the damage mechanism is addressed to ESC behavior. In FNCT investigations, stress, temperature and specimen geometry were varied systematically. In addition to the time to failure as common measure for the resistance of a PE-HD type against crack propagation, specimen elongation was considered in detail. Several imaging techniques were applied for fracture surface analysis of specimens tested in FNCT to gain novel information on SCG and ESC behavior. From height profiles obtained by laser scanning microscopy (LSM) and information on surface structures from scanning electron microscopy (SEM), indicators for the differentiation of the crack propagation mechanisms could be derived. Based on the LSM data, an algorithm for the distinction between ductile shear deformation and brittle crack growth as dominating failure mechanism was developed. Imaging techniques were also used for determination of crack propagation rates, which were related to time-resolved FNCT elongation data. From the time-resolved determination of crack lengths of partly damaged FNCT specimens, an increasing length of craze zone with a progressively propagating crack was revealed for the first time. This relation of crack and craze zones was specified by fracture mechanical considerations. N2 - 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 das Verständnis der beiden Schädigungsmechanismen „langsames Risswachstum“ (engl.: „slow crack growth“, SCG) und „umgebungsbedingter Spannungsriss“ (engl.: „environmental stress cracking“, ESC) essentiell. Eine etablierte Prüfmethode zur Bewertung dieser Schädigungsmechanismen ist der Full-Notch Creep Test (FNCT), der in dieser Arbeit zur systematischen Untersuchung des Risswachstums in PE-HD Behältermaterialien unter Einwirkung von Luft, Wasser und wässrigen Netzmittellösungen (Arkopal N 100) sowie Biodiesel und Diesel verwendet wird. Aus den Ergebnissen des FNCT wird ein Klassifikationsschema für Fluide vorgeschlagen, welches ebenfalls eine Zuordnung zu den Schädigungsmechanismen erlaubt. Hierbei wird in (i) inerte, (ii) rein oberflächen-aktive und (iii) zusätzliche sorptive, volumen-aktive Fluide hinsichtlich des langsamen Risswachstums (SCG) unterschieden. Wenn ein Fluid lokal die intrinsischen Materialeigenschaften des Polymers verändert, wird der Schädigungsmechanismus dem umgebungsbedingten Spannungsriss (ESC) zugeordnet. Bei den FNCT-Untersuchungen wurden die mechanische Spannung, die Temperatur und die Prüfkörpergeometrie systematisch variiert. Zusätzlich zur Standzeit wurde die Prüfkörperdehnung zeitabhängig erfasst. Aus einer erweiterten Bruchflächenanalyse konnten neuartige Informationen über SCG und ESC erhalten werden. Hierzu wurden verschiedene Bildgebungsverfahren verwendet. Insbesondere wurden mit Laserscanningmikroskopie (LSM) Höhenprofile und mit Rasterelektronenmikroskopie (REM) Oberflächeninformationen zur Charakterisierung der Rissfortschrittsmechanismen erhalten. Auf Basis der LSM wurde unter Zuhilfenahme von Höhenprofildaten ein Algorithmus zur Unterscheidung zwischen duktiler Scherverformung und sprödem Risswachstum als dominierende Schädigungsmechanismen entwickelt. Die aus den bildgebenden Verfahren ermittelten Rissfortschrittsraten konnten mit den Daten der während des FNCT erfassten Dehnung der Prüfkörper in Beziehung gesetzt werden. Weiterhin wurde mithilfe von zeitaufgelösten Risslängendaten erstmals eine direkte Korrelation der Risslänge zu vorgeschädigten, fibrillierten Bereichen (Crazes) im PE-HD Prüfkörper während des FNCT nachgewiesen. Demnach vergrößert sich die Craze-Länge linear mit zunehmender Risslänge. Dieser Zusammenhang zwischen Riss- und Craze-Längen wurde auf mathematisch, bruchmechanischer Grundlage bestätigt. KW - High-density polyethylene (PE-HD) KW - Full-Notch Creep Test (FNCT) KW - Slow crack growth (SCG) KW - Environmental Stress Cracking (ESC) KW - Biodiesel KW - Diesel KW - Crack propagation analysis KW - Fracture Surface Analysis KW - Test Improvement KW - Imaging PY - 2020 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:tuda-tuprints-115443 SP - 1 EP - 212 CY - Darmstadt AN - OPUS4-50941 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schilling, Markus A1 - Niebergall, Ute A1 - Böhning, Martin T1 - Damage of PE-HD due to environmental stress cracking (ESC) induced by liquid media - Full Notch Creep Testing (FNCT) N2 - Due to the increasing demand for utilization and improvement of energy efficient materials, especially concerning requirements in lightweight construction and design, polyolefin materials are used extensively and in an increasingly broad range of applications. Although loaded with stresses under yield stress, preformed voids, inhomogeneities or notches can possibly lead to damage and unexpected failure induced by liquid media in polyolefin materials. For PE-HD, slow crack growth (SCG) as well as environmental stress cracking (ESC) are relevant mechanisms of damage. SCG appears without influence of a surrounding medium or in “inert” media whereas ESC occurs in “active” media, which have decisive influence on damage mechanism and time to failure. To characterize the intrinsic resistance of the material against those damage mechanisms, the Full-Notch Creep Test (FNCT) is widely used and of paramount importance particularly for the assessment of pipe and blow molding types of PE-HD. In this study, the FNCT – usually applied as a standardized testing method (ISO 16770) using a few universal model liquid media – is extended by investigations of selected relevant PE-HD materials with a variety of properties also in real media. Mainly topical fuels, customary in the market such as diesel and biodiesel are examined. Especially the influence of temperature, and the ESC behavior of PE-HD in media that are sorbed to a significant extent, are addressed. The underlying diffusion-controlled sorption process was assessed before comparing non-saturated specimens with samples previously saturated with sorbing media. The investigations were performed using a novel FNCT-device with 12 individual sub-stations, each equipped with individual electronic stress and temperature control and continuous online monitoring of the specimen elongation. In addition to acquired results concerning time to failure and elongation behavior, imaging techniques, such as light microscopy (LM), laser scanning microscopy (LSM) and X-ray computed tomography (CT scan) were utilized to obtain data concerning crack propagation and media migration. Fracture surface analysis (LM, LSM) and quasi in-situ imaging (CT scan) via measurement in different load stages are considered explicitly. Correlations of elongation behavior and data derived from imaging analysis such as fracture plane roughness and height of areas of ductile deformation were obtained. T2 - EUROCORR2017 CY - Prague, Czech Republic DA - 03.09.2017 KW - Environmental stress cracking (ESC) KW - Slow crack growth (SCG) KW - High-density polyethylene (PE-HD) KW - Full notch creep test (FNCT) KW - Biodiesel KW - Diesel PY - 2017 AN - OPUS4-43518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Niebergall, Ute A1 - Alig, I. A1 - Oehler, H. A1 - Lellinger, D. A1 - Meinel, Dietmar A1 - Böhning, Martin T1 - Crack propagation in PE-HD induced by environmental stress cracking (ESC) analyzed by several imaging techniques N2 - Different imaging techniques were employed to monitor Full Notch Creep Test (FNCT) experiments addressing environmental stress cracking in more detail. The FNCT is a well-established test method to assess slow crack growth and environmental stress cracking of polymer materials, especially polyethylene. The standard test procedure, as specified in ISO 16770, provides a simple comparative measure of the resistance to crack growth of a certain material based on the overall time to failure when loaded with a well-defined mechanical stress and immersed in a liquid medium promoting crack propagation. Destructive techniques which require a direct view on the free fracture surface, such as light microscopy and laser scanning microscopy, are compared to non-destructive techniques, i.e. scanning acoustic microscopy and xray micro computed tomography. All methods allow the determination of an effective crack length. Based on a series of FNCT specimens progressively damaged for varied Durations under standard test conditions, the estimation of crack propagation rates is also enabled. Despite systematic deviations related to the respective Imaging techniques, this nevertheless provides a valuable tool for the detailed evaluation of the FNCT and its further development. KW - Environmental stress cracking (ESC) KW - Slow crack growth (SCG) KW - Full notch creep test (FNCT) KW - X-ray computed tomography (CT) KW - Laser scanning microscopy (LSM) KW - Scanning acoustic microscopy (SAM) PY - 2018 U6 - https://doi.org/10.1016/j.polymertesting.2018.08.014 SN - 0142-9418 SN - 1873-2348 VL - 70 SP - 544 EP - 555 PB - Elsevier AN - OPUS4-45766 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -