Constant stress creep experiments at 550 °C were performed on a high-purity Fe-3Au-4W (wt.%) ternary alloy with about 1 at.% supersaturation for Au and W in order to study self healing of grain-boundary cavities by both Au-rich and W-rich precipitates. Using synchrotron X-ray nano-tomography, the development of the creep cavities and the healing precipitates at different stages of creep was visualised using two spatial resolutions (30 and 100 nm voxel size) for separate samples taken after different loading times. The healing kinetics was found to strongly depend on the nucleation time of the cavities. Cavities nucleated at an early stage of creep could be fully healed, while the healing of the late-nucleated cavities is much slower due to a decrease in the diffusional flux of the healing supersaturated solutes over time, as a result of (i) a decrease in inter-cavity spacing caused by cavity nucleation and (ii) a gradual depletion of the supersaturated solutes near the grain boundaries. The interaction between the competing healing mechanisms for creep cavities by Au-rich and W-rich precipitates is discussed. It was found that Au-rich precipitates are formed much faster than the W-rich precipitates, and thereby effectively provide creep damage healing on different time scales.

The autonomous filling of creep-loading induced grain-boundary cavities by gold-rich precipitates at a temperature of 550 °C has been studied as a function of the applied load for Fe-Au alloys using synchrotron X-ray nano-tomography. The alloy serves as a model alloy for future self-healing creep resistant steels. The size, shape and spatial distribution of cavities and precipitates are analyzed quantitatively in 3D at a nanometer resolution scale. The filling ratios for individual cavities are determined and thus a map of the filling ratio evolution is obtained. It is found that the gold-rich precipitates only form at cavity surfaces and thereby repair the creep cavity. The shape of the cavities changes from equiaxed to planar crack like morphologies as the cavities grow. The time evolution of the filling ratio is explained by a simple model considering isolated cavities as well as linked cavities. The model predictions are in good agreement with the measurements.