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A phenomenological criterion for an optical assessment of PE-HD fracture surfaces obtained from FNCT
(2021)
The full-notch creep test (FNCT) is a common test method to evaluate the environmental stress cracking (ESC) behavior of high-density polyethylene (PE-HD), e.g. for container materials. The test procedure as specified in ISO 16770 provides a comparative measure of the resistance against ESC using the time to failure of PE-HD specimens under constant mechanical load in a well-defined liquid test environment. Since the craze-crack damage mechanism underlying the ESC phenomenon is associated with brittle failure, the occurrence of a predominantly brittle fracture surface is a prerequisite to consider an FNCT measurement as representative for ESC, i.e. a time to failure dominated by craze-crack propagation.
The craze-crack propagation continuously reduces the effective residual cross-sectional area of the specimen during the test, which results in a corresponding increase of the effective mechanical stress. Thus, a transition to ductile shear deformation is inevitable at later stages of the test, leading usually to a pronounced central ligament.
Therefore, an optical evaluation of FNCT fracture surfaces concerning their brittleness is essential. An enhanced imaging analysis of FNCT fracture surfaces enables a detailed assessment of craze-crack Propagation during ESC. In this study, laser scanning microscopy (LSM) was employed to evaluate whether FNCT fracture surfaces are representative with respect to craze-crack propagation and ESC. Based on LSM height data, a phenomenological criterion is proposed to assess the validity of distinct FNCT measurements. This criterion is
supposed to facilitate a quick evaluation of FNCT results in practical routine testing. Its applicability is verified on a sample basis for seven different commercial PE-HD container materials.
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.
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.
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.