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 aprotic systems, can be measured in situ by both atomic force microscopy and scanning tunneling microscopy (STM). The workstation includes an evacuable glovebox that maintains a pure atmosphere in which the microscopes are located, 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 experiments, while all the piping connections are removed. The concept of an evacuable glovebox, which can be back-filled by a pure atmosphere, enables measurements to be performed under a pure inert atmosphere, eliminating the need for noisy gas purification systems. Pure solutions and highly reactive electrode materials are introduced into this glovebox by the use of a transfer method, based on a hermetically sealed transfer vessel and a special vacuum chamber in the glovebox. Preliminary results demonstrated that high-quality imaging of reactive electrochemical systems can be obtained using this system. A procedure for the preparation of STM tips is also described. (C) 1999 American Institute of Physics. [S0034-6748(99)01312-X].