Analytical TEM study of annealed nanocrystalline cobalt–phosphorous electrodeposits

Investigation of thermal stability of two nanocrystalline Co–P alloys shows that P atoms segregate to the grain boundaries upon annealing until precipitation of Co2P and CoP precipitates takes place. The P-rich precipitates formed have been investigated by analytical transmission electron microscopy to obtain statistical results of precipitate size, volume fraction and spatial distribution. Electron spectroscopic imaging maps show that the P-rich precipitates are 33 ± 9 nm in Co–1.1at.%P and 33 ± 12 nm in Co–3.2at.%P. The main differences between the alloys are the precipitate size distribution (Co–3.2at.%P having broader distribution) and precipitate volume number density (Co–3.2at.%P has 1.8 times more precipitates than Co–1.1at.%P). The volume fraction of precipitates is 3.0% in Co–1.1at.%P and 4.4% in Co–1.1at.%P. Most of the precipitates are of nearly spherical or slightly elongated shape, and only a few have a plateletlike shape as expected from previous tomographic atom probe measurements. Due to the truncation and projection effects, the composition of the precipitates could not be determined