Application of in situ Transmission Electron Microscopyfor Tribological Investigations of Magnetron Sputter Assisted Pulsed Laser Deposition of Yttria-stabilized Zirconia-gold Composite Coatings

Yttria-stabilized zirconia (YSZ)-Au composite coatings have great potential as solid film lubricants for aerospace applications over a wide range of environmental conditions. They were grown on steel disks or silicon wafers by pulsed laser ablation of YSZ and simultaneous magnetron sputtering of a Au target. Such a combination of ceramics with soft metals improved the toughness of the composite coating and increased its ability to lubricate at high temperature. Information on the time-dependent response of these microstructures to changes in temperature is essential to tribological investigations of high temperature performance. In situ transmission electron microscopy was used to directly measure the dynamic change of YSZ-Au coating structure at elevated temperatures. High-resolution electron microscopy and electron diffraction showed that amorphous YSZ-5 at.% Au coatings proceeded to crystallize under the irradiation of electron beams. Time varying x-ray energy dispersive spectra measured a loss of oxygen in the sample during about 10 min of irradiation with subsequent slight oxygen recovery. This behavior was related to the activation of oxygen diffusion under electron irradiation. X-ray diffraction patterns from vacuum annealed samples verified crystallization of the coatings at 500 °C. Real-time growth of Au nanograins in the sample was observed as the temperature was increased to 500 °C in a TEM specimen holder that could be heated. The grain growth process was recorded using a charge-coupled device camera installed on the transmission electron microscope. The crystallization and growth of zirconia and Au nanograins resulted in low friction during tribological tests. The nucleation of Au islands on heated ball-on-flat specimens was responsible for lowering friction.