Measurement and estimation of temperature rise in TEM sample during ion milling

The actual temperature rise was measured during ion-milling process used in the transmission electron microscopy (TEM) sample preparation. Special probes were fabricated for the measurements, one with shielded, floating thermocouple mounted onto a 3 mm grid to compute the thermal load at the sample, and the other, a bare probe with a polymer coating to measure the maximum temperature attained. The temperature measured in the most commonly used ion-milling system reached up to 295 °C when the typical milling conditions, 6 keV ion-energy and an incident angle of 80°, were used. Based on the temperature profiles that were obtained by the shielded probe, two unknown parameters, the amount of heat deposited by the energetic ions/neutrals to the sample and the thermal conductivities between the materials, were estimated and used to compute the temperature rise in commonly adopted materials. The calculation showed that the temperature of the glass sample reached more than 300 °C under typical ion-milling conditions. The calculated value was confirmed with the experimental result of the crystallization of an amorphous Si on the glass under the typical ion-milling condition, which gave the same extent as annealing at 350 °C.