Damage analysis microscopy

Practical case studies are used to demonstrate how useful differential scanning microscopy analysis can be for material testing and damage analysis on plastics and plastic parts. It measures the physical and chemical properties of the plastic as a function of temperature. Information gained by use of the analytical tool is examined, and case studies relating to fluctuating material quality through the use of recyclate, and the oxidation of PP water pipes are discussed. 

No analytical method is perfect. Spectral interpretation is still difficult, and standard spectra databases are scarce. The issues of quantification, comparison with data collected by other methods, and scale up are important, especially in spectromi-croscopy studies. Radiation damage and sectioning artifacts can make analysis of susceptible samples difficult. The biggest obstacle to widespread use of NEXAFS spectroscopy, microscopy, and spectromicroscopy in environmental studies remains the extremely limited number of such instruments. Typically, each beamline allocation committee receives 2 or 3 times as many requests for time as is available. Studies, when granted, are usually for 2-5 days every 4-6 months. Thus, scientists have to be very selective about the types of questions and samples that they choose to examine using these techniques. Continued pressure and education from the scientific community will be needed to increase the number of beamlines suitable for NOM studies in the future, even as new synchrotron facilities are planned or built. 

There are a number of indicators of fatigue damage that have attracted interest in the literature. During the life of a component subjected to fatigue, the material can exhibit changes in modulus, permanent offset strain, shape of the hysteresis loops, and temperature rise of the specimen surface. Direct evidence of matrix crack density can be obtained by surface replication, while a more detailed analysis of microstructural damage requires scanning electron microscopy (SEM). 

Relevant and complementary information about the damage process of polymers can be obtained among others by the analysis of the force-displacement curves, by the observation of the fracture surfaces (cf. Sects. 3.2.5 and 5.4) and, as will be shown in Sect. 6.2.2, by the determination of the amount of voids in a sample during and/or after deformation. However, a complete elucidation of the deformation mechanisms is only possible by their direct observation at the sub-micron level. Transmission electron microscopy is often used for this purpose. For convenience, the tests (which require experience and touch) are generally carried out at room temperature and at a low strain rate. 

The paper is presented in three parts. First, the tests employed to determine the mixed mode fracture envelope of a glass fibre reinforced epoxy composite adhesively bonded with either a brittle or a ductile adhesive are briefly described. These include mode I (DCB), and mixed mode (MMB) with various mixed mode (I/II) ratios. In the second part of the paper different structural joints will be discussed. These include single and double lap shear and L-specimens. In a recent European thematic network lap shear and double lap shear composite joints were tested, and predictions of failure load were made by different academic and industrial partners [9,10]. It was apparent that considerable differences existed between different analytical predictions and FE analyses, and correlation with tests proved complex. In particular, the progressive damage development in assemblies bonded with a ductile adhesive was not treated adequately. A more detailed study of damage mechanisms was therefore undertaken, using image analysis combined with microscopy to examine the crack tip strain fields and measure adherend displacements. This is described below and correlation is made between predicted displacements and failure loads, based on the mixed mode envelope determined previously, and measured values. 

The effect of clioquinol-metal chelates has been tested on neural crest-derived melanoma cells (6). The effect of clioquinol chelates on cells was further studied by electron microscopy and by a mitochondrial potential-sensitive fluorescent dye. Of the ions tested, only clioquinol-zinc chelate was cytotoxic. This cytotoxicity was extremely rapid, suggesting that its primary effect was on the mitochondria, and electron microscopic analysis showed that the chelate caused mitochondrial damage. This was further confirmed by the observation that the chelate reduced the mitochondrial membrane potential. The phenomenon of cUoquinol-mediated toxicity appeared to be specific to zinc and was not seen with other metals tested. Since clioquinol causes increased systemic absorption of zinc, it is likely that clioquinol-zinc chelate was present in appreciable concentrations in patients with SMON and may have been the causative toxin. 

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