The use of a special work station for in situ measurements of highly reactive electrochemical systems by atomic force and scanning tunneling microscopes

In this article, we describe a special homemade workstation in which highly reactive electrochemical systems, such as lithium electrodes in polar apro tic systems, can be measured in situ by both atomic force microscopy and sc anning tunneling microscopy (STM). The workstation includes an evacuable gl ovebox that maintains a pure atmosphere in which the microscopes are locate d, thus enabling measurements in a highly pure argon atmosphere. The system is based on a compact and functional evacuable glovebox which is placed in a special construction which provides full protection against vibrations. This is obtained by suspending the box by flexible cords during the experim ents, while all the piping connections are removed. The concept of an evacu able glovebox, which can be back-filled by a pure atmosphere, enables measu rements to be performed under a pure inert atmosphere, eliminating the need for noisy gas purification systems. Pure solutions and highly reactive ele ctrode materials are introduced into this glovebox by the use of a transfer method, based on a hermetically sealed transfer vessel and a special vacuu m chamber in the glovebox. Preliminary results demonstrated that high-quali ty imaging of reactive electrochemical systems can be obtained using this s ystem. A procedure for the preparation of STM tips is also described. (C) 1 999 American Institute of Physics. [S0034-6748(99)01312-X].