High temperature impedance measurements on Au microelectrodes deposited on polished yttria stabilized zirconia (YSZ) pellets were demonstrated using a newly designed controlled atmosphere high temperature scanning probe microscope (CAHT-SPM). Probes based on Pt0.8Ir0.2 were fabricated and employed in all the investigations. The electrical properties of the Au microelectrodes were investigated using CAHT-SPM at various temperatures in air. The influences of the tip-sample force and of the size of the microelectrode on the electrical properties of the Au microelectrodes were also studied. The impedance spectra of circular Au microelectrodes down to 8 urn in diameter at different temperatures were successfully obtained. The CAHT-SPM presented in this paper is capable of obtaining topography images, conductivity images and impedance spectra in-situ in a temperature range from room temperature to at least 650 degrees C. (C) 2011 Elsevier B.V. All rights reserved.