In Situ Transmission Elecron Microscope Triboprobe For Tribological Studies Of Materials At Nanoscale
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In most of the tribological experiments studying friction and wear behaviour, the contact interface is hidden. The present work attempts to overcome this hidden-interface problem by carrying out real-time tribological experiments inside Transmission Electron Microscope (TEM). This is achieved by developing an in situ TEM triboprobe which can carry out nanoscale indentation, sliding and reciprocating tests on an electron transparent sample inside TEM. A novel in situ TEM triboprobe is developed by characterising the individual components involved in the development. Coarse positioning of a sharp probe is achieved using inertial sliders. Fine motion of the probe is controlled using a 4-quadrant tube piezoceramic. This triboprobe is capable of carrying out high stiffness tribological experiments inside TEM. The interface is viewed at high resolutions in real time during the experiments using a movie rate CCD camera. In indentation experiments a sharp probe is brought into contact with the sample surface. During indentation of Aluminium alloy tribolayer, it has been observed that the cracks originate from subsurface and propagate to the surface causing delamination-like material removal. Indentation experiments on protruding silicon particle in Aluminium-Silicon (Al-Si) alloy shows that initial deformation is elastic. Once the load is increased, the particle starts indenting the soft aluminum matrix, and results in sinking of the particle into the aluminium matrix. Once the particle starts sinking, the increase in the displacement causes the generation of a crack and the propagation of this crack results in the fracture of the particle. The sliding experiments inside TEM allowed the direct visualization of asperity level interaction during sliding. The preliminary experimental results of nanoscale sliding experiments carried out using an AFM tip as the sample. The adhesive instability is observed as snap-in and snap-out events. The snap-out distance seems to depend on the local geometry of the contact. To simulate reciprocating wear, a sharp diamond probe is brought into contact with Al-Si alloy and reciprocated sinusoidally at 0.5Hz. At lower loads no wear is observed. However, when the normal load is increased, material starts getting removed in thin slivers, and most of the wear debris generated get swept away from the track. Some wear debris get entrapped in between the sliding surfaces; subsequently they join to form larger wear particles. The trapped particles generated during the test act like rollers and a significant increase in the stroke-length is observed accompanying the rolling action of the particle. The phenomena like agglomeration and dissociation of the wear particles has also been observed. Repeated deformation of the trapped particles leads to the formation of tiny liquid drop on some of the wear debris. The liquid consists of gallium which comes from the sample preparation technique. The interaction between the liquid droplets has been studied by carrying out liquid-bridge pulling experiments. Liquid gallium gets cooled with time during tensile pulling of the droplets. A nano-filament is formed between the droplets during pulling. After some time, the droplet gets solidified and coalescence of droplets does not take place. Further frictional heating was necessary to form the bridge again. The in situ TEM triboprobe, which allow the tribological processes to be observed dynamically under high resolutions, is a power full tool in detecting fundamental tribological interactions.