A metal- coating Chamber for High-Resolution Cryo-SEM

Abstract

Improvements in particulate coatings for printable paper require understanding mechanisms of colloidal interactions in paper coating suspensions. One way to deduce colloidal interactions is to mage particle spacings and orientations at high resolution with cryo-SEM. Recent improvements in cryo-SEM technique have increased resolution enough to image particles in coating paints,vhich are sometimes smaller than 100 nm. In this report, a metal-coating chamber is described for preparation of colloidal suspensions for cryo-SEM at resolution down to 20 nm. It was found that etching is not necessary to achieve this resolution.A 120 K cryo-SEM sample will remain in an SEM for hours without noticeable condensation of imorphous ice. This is due to the high vapor pressure of vapor-condensed amorphous ice, measured by Kouchi. However, clean vacuum is required to coat samples with the thinnest possible continuous metal films which are required for high magnification SEM. Vapor contaminants, especially hrydrocarbons, are known to interfere with thin-film nucleation and growth so that more metal is needed to form continuous films, and resolution is decreased. That is why the metal-coating chamber in fig. 1 is designed for the cleanest possible vacuum. Feedthroughs for the manipulator md the shutter, which are operated during metal coating, are sealed with leak-proof stainless-steel Dellows. The transfer rod slides through a baseplate feedthrough that is double o-ring sealed.