Optimisation des paramètres expérimentaux pour l’analyse des fibres d’amiante par microscopie électronique en transmission

Asbestos is a material known and used by man for nearly 5000 years, its commercial definition includes six different types of fibrous mineral. Because of their numerous thermal and mechanical properties, asbestos has been mined intensively for commercial use in the last century. It is now well recognized that asbestos exposure can cause severe damage to health and thus its use and exploitation is therefore banned in many countries and its exposure is strictly regulated. The application of those regulations requires rigorous analytical methods to support it. Transmission electron microscopy (TEM) is the most powerful and efficient tool for the analysis of asbestos fibers. However, identification errors caused by damage to asbestos fibers can occur and this problem has been investigated in depth. Asbestos amosite fibers were initially investigated to evaluate the damage caused by a transmission electron microscope electron beam. Since elemental x-ray intensity ratios obtained by energy dispersive x-ray spectroscopy (EDS) are commonly used for asbestos identification, the impact of beam damage on these ratios was measured. It was determined that the magnesium/silicon ratio was the most sensitive to damage caused by the electron beam. Various tests showed that most fibers have a current density threshold above which the chemical composition of the fiber is modified. The value of this threshold current density varied depending on the fiber. The existence of a threshold electron dose was also demonstrated. This value was dependent on the current density used and can be increased by providing a recovery period between exposures to the electron beam. This study also established that the electron beam current is directly related to the damage rate above a current density of 165 A/cm2. Guidelines were established in order to ensure that the amosite fibers are not damaged. It was determined that analysis should be conducted below a current density of 100 A/cm2. In the second part of this study, the main objective was to assess whether temperature is a factor influencing damage to asbestos fibers and, if so, how it can be used to minimize damage. It was found that lowering the temperature to 123 K can inhibit, for a given time, the manifestation of the damage. The significant decrease of atom diffusion at low temperature momentarily prevents mass loss, greatly reducing the possibility of misidentification of vi anthophyllite asbestos fibers. The results obtained in this study strongly suggest that the predominant mechanism damage is probably related to the induced-electric-field model. In a third part, the effect of the acceleration voltage on the damage of four different types of asbestos fibers; chrysotile, amosite, crocidolite and anthophyllite, was investigated. The results support the conclusion that contrary to what is usually recommended, it is best to use an acceleration voltage of 200 kV than 100 kV in order to avoid damage. The findings shed light on possible damage mechanisms; the most predominant seems to be caused by an induced electric field, radiolysis is not excluded but seems less important and knock-on is thought to be negligible for the conditions used.

Keyphrases: Transmission Electron Microscopy, Asbestos, Electron dose, Current density, Damage mechanism, Accelerating voltage