Construction and performance test of apparatus for permeation experiments with controlled surfaces

A new apparatus was constructed to examine gas-, atom- and plasma-driven permeation of hydrogen isotopes through group VA metal membranes with precisely controlled surface states. Absorption and desorption experiments are also possible. The new apparatus consists of two vacuum chambers, an upstream chamber and a downstream chamber, separated by a specimen membrane. Both chambers are evacuated by turbo-molecular pumps and sputter-ion pumps. The upstream chamber is equipped with Ta filaments serving as atomizers in atom-driven permeation experiments and cathodes in plasma-driven permeation experiments. The specimen membrane is formed into a tubular shape and electrically isolated from the chamber. Hence, ohmic heating of the membrane is possible, and this feature of the membrane is suitable for surface cleaning by high-temperature heating an impurity doping for the control of surface chemical composition through surface segregation. Both chambers were evacuated to 1 x 10-7 Pa after baking. The main component of residual gas was H2, and the partial pressures of impurity gases other than H2 were ca. 1 x 10-8 Pa. Gas- and atom-driven permeation experiments were successfully carried out with hydrogen gas for Nb membrane activated by heating in vacuum at 1173 K. Superpermeation was observed in the atom-driven permeation experiments. Absorption experiments with a clean surface were also carried out. The surface was, however, cleaned only partially, because the temperature distribution was not uniform during high-temperature heating. Nevertheless, surface cleanliness was retained during absorption experiments under the present vacuum conditions. A new membrane assembly that will enable a uniform temperature distribution is now under construction. (author)