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The FNCT is widely used to characterize the slow crack growth (SCG) behavior of polyolefinic 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 PE-HD - especially for transport and packaging of dangerous goods but also for most other high-performance applications.
Usually the FNCT 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 PE-HD 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 ESC behavior of PE-HD in media that are sorbed to a significant extent – one example are fuels, such as 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 FNCT-device with 12 individual sub-stations, each equipped with individual electronic stress and temperature control and continuous online monitoring of the specimen elongation.
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 tf*. Usually the FNCT is applied as a standardized testing method (ISO 16770) using a few universal liquid media, such as solutions of Arkopal N 100 (detergent).
Selected relevant PE-HD materials are investigated also in real media and influences of temperature and geometry of specimen and notch are explicitly addressed. The investigations comprise also the ESC behavior of PE-HD in media that are sorbed to a significant extent – such as Diesel and Biodiesel – based on comparison with samples previously saturated with those media.
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.
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 damage mechanisms. 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 inherent resistance of the material against those damage mechanisms, the Full-Notch Creep Test (FNCT) is widely used. Therefore, the FNCT is of paramount importance particularly for the assessment of pipe and blow molding types of PE-HD – especially in the field of polymer development and improvement for high-performance applications.
In this study, the FNCT – usually applied as a standardized testing method (ISO 16770) using a few universal model liquid media – is extended by investigation 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 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.
Additional 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. Correlations of elongation behavior and data derived from imaging analysis were obtained.
Damage of PE-HD induced by liquid media - Full Notch Creep Testing (FNCT) and Imaging analysis
(2017)
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 damage mechanisms. 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 inherent resistance of the material against those damage mechanisms, the Full-Notch Creep Test (FNCT) is widely used. Therefore, the FNCT is of paramount importance particularly for the assessment of pipe and blow molding types of PE-HD – especially for automotive but also for most other high-performance applications.
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 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.
Additional 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. Correlations of elongation behavior and data derived from imaging analysis such as fracture plane roughness were obtained.
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.
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.
As the well-known damage mechanisms slow crack growth (SCG) and environmental stress cracking (ESC) are the major causes for possible failure of polyolefin-based materials, especially for PE-HD, they are highly relevant and need to be considered thoroughly. Furthermore, due to slight but perceptible differences in damaging effect, a differentiation between SCG and ESC is expedient. SCG appears in “inert” or “neutral” media without a decisive influence of the surrounding medium whereas ESC occurs in “active” media, which influence the failure behavior and time to failure crucially.
To characterize the inherent resistance of the material against those damage mechanisms, the well-established Full-Notch Creep Test (FNCT) is used. In this study, the FNCT – usually applied according to ISO 16770 [3] using a few universal model liquid media and mainly for pipe materials – is extended by investigations with appropriate parameters of selected relevant PE-HD container materials also in real media, such as the topical fuels diesel and biodiesel. 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.
Especially, mechanical stress and temperature were varied systematically during FNCT and time to failure values, time-dependent elongation data as well as detailed fracture surface analysis by laser scanning microscopy (LSM) were combined for the first time (Fig. 1). Particularly, the fracture surface analysis provides a sound basis to characterize failure behavior, mainly regarding the balance between brittle crack propagation and ductile deformation. Therefore, fracture surface analysis is an essential tool for a decent assessment of SCG and ESC by FNCT measurements.
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.
The aim of this research is to study the influence of moisture absorption at low moisture contents on the creep behaviour of an epoxy adhesive in steel bonded joints. Single lap joints were manufactured using high strength steel adherends and a two-component epoxy adhesive. The single lap joints were tested at load Levels corresponding to average lap shear stresses of±5%, 15%, 30% and 45% of the dry lap shear strength in both 40 °C air and 40 °C distilled water. Specimens were not pre-aged to be able to analyse the coupled effect of moisture and loading. The test results show that an increase in the load level resulted in an increase in the instantaneous strain and in the creep strain rate. The creep strain of single lap joints loaded in water was generally larger than for the ones loaded in air. For joints loaded in water the creep behaviour was found to be dependent on the moisture concentration in the adhesive. At low moisture percentages creep was suppressed, resulting in a lower instantaneous strain. At higher moisture percentages creep was promoted, resulting in a larger strain rate. The suppression of creep at low moisture percentages is attributed to water molecules bonding to the epoxy macromolecules, resulting in a reduction in molecular mobility and a smaller creep strain. At higher moisture percentages the plasticizing effect of the water dominates, resulting in a larger creep strain. The Maxwell threeelement solid model and Kelvin-Voigt three-element solid model were used to simulate the creep behaviour of the single lap joints loaded in air and water. The models gave good representations of the creep Response across the different load levels in both water and air, they were however unable to give a correct representation of the instantaneous strain of the single lap joints loaded in water. This is attributed to the models being unable to account for the present short-term relaxation process that is dependent on the moisture concentration.