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The evolution of atomistic-level nanostructure during the early stages of both standard, high-temperature T6 heat treatment, and low-temperature secondary ageing after interruption of the former (T6I4), has been investigated in rapid hardening Al-Cu-Mg alloys using a variety of microscopy and microanalytical techniques, including transmission electron microscopy (TEM), positron annihilation spectroscopy (PAS) and atom probe tomography (APT). In order to carry out this objective, quantitative data-analysis methods were developed with respect to new cluster-finding algorithms, specifically designed for use with three-dimensional APT data. Prior to this detailed characterisation work, the actual thermal impact from both heat treatment and quenching of small, lab-scale specimens was determined through correlation of both experimental results and calculations that modelled the heat transfer conditions using the lumped capacitance method. Subsequently, the maximum diffusion distance by random walk of the solute atoms was calculated for these periods, bearing significance on the propensity for these atoms to have the ability to cluster together, rather than segregate to the dislocation loops in the microstructure, which have a relatively larger interspacing distance. Age-hardening curves for the Al-1.1Cu-xMg (x = 0, 0.2, 0.5, 0.75, 1.0, 1.7 at.%) alloys at 150ºC show that the rapid hardening phenomenon (RHP) exists for Mg compositions ≥ 0.5Mg. Given that zone-like precipitate structures were unable to be detected by TEM or APT during the early stages of ageing at 150ºC, and that statistically significant dispersions of clusters were found in the APT data after ageing for 60 s, the RHP is attributed to these clustering reactions. Identification of clusters in the APT data has been achieved using the core-linkage algorithm and they have been found to be quite small, containing only a few atoms up to a couple of tens of atoms. The RHP is governed by some critical number density of both Mg clusters and Cu-Mg co-clusters of a critical size, whereas Cu clusters do not contribute significantly to the hardening mechanism. Significance testing indicates that Mg clusters are more significant at smaller clusters sizes and Cu-Mg co-clusters more important at larger cluster sizes. Hardness results also confirm the existence of rapid early hardening during secondary ageing at 65ºC in Al-1.1Cu-1.7Mg. The mechanism of secondary rapid hardening involves a combination of both secondary clustering from solute (mainly Mg atoms) residual in solution, and pre-existing amorphous primary clusters that have slower growth kinetics at the lower secondary ageing temperature. The latter occurs mainly by vacancy-assisted diffusion of Mg atoms as evidenced by the gradual increase of the Mg:Cu ratio of co-clusters. From an alloy design point of view it is important to fully understand the solute distribution in the microstructure to be able to subsequently optimise the configuration for enhanced material properties. The change in dispersion of solute atoms during ageing was determined by combining calculations of % vacancy-solute associations with detailed measurements of the dislocation loops to estimate the solute distribution within the microstructure. The implication of the balance of solute atoms segregated to the loops compared with that in the matrix is then discussed in the context of hardnening mechanisms.