Atom probe tomography study of the decomposition of a bulk metallic glass

The microstructural evolution of a Pd₄₀Ni₄₀P₂₀ bulk metallic glass that was isothermally annealed at 260 °C for 14 h, and then aged at 340 °C for times up to 1280 min has been studied. Differential scanning calorimetry (DSC) curves of the aged samples show an endothermic peak at approximately 370 °C in addition to the ubiquitous glass transition. The endothermic peak appears after 20 min aging and disappears after 320 min aging. The corresponding X-ray diffraction (XRD) data show no Bragg peaks that could indicate the formation of a crystalline phase. Near-atomic-resolution atom probe tomography (APT) was used to study changes in the atomic spatial distributions as a function of aging time. The chemical environment around each of the atomic species, and the tendencies for solute clustering and chemical short range ordering, were determined from statistical analysis of the APT data. Clustering and possible phase separation are identified by APT after only 20 min aging at 340 °C, which correlates with the appearance of the peak in the DSC signal. Crystallization is apparent in the APT and XRD data after aging for 320 min. The study suggests that the amorphous Pd₄₀Ni₄₀P₂₀ annealed at a temperature 40 °C above T_g phase separates into two or more amorphous phases. The endothermic peak in the DSC trace is produced by the dissolution of the phase separation.