Masaya Kozuka

Effects of isoconcentration surface threshold values on the characteristics of needle-shaped precipitates in atom probe tomography data from an aged Al–Mg–Si alloy

Needle-shaped precipitates in an aged Al-0.62Mg-0.93Si (mass%) alloy were identified using a compositional threshold method, an isoconcentration surface, in atom probe tomography (APT). The influence of thresholds on the morphological and compositional characteristics of the precipitates was investigated. Utilizing optimum parameters for the concentration space, a reliable number density of the precipitates is obtained without dependence on the elemental concentration threshold in comparison with evaluation by transmission electron microscopy (TEM). It is suggested that careful selection of the concentration space in APT can lead to a reasonable average Mg/Si ratio for the precipitates. It was found that the maximum length and maximum diameter of the precipitates are affected by the elemental concentration threshold. Adjustment of the concentration threshold gives better agreement with the precipitate dimensions measured by TEM.

Effects of Pre-Aging and Natural Aging on Bake Hardening Behavior in Al-Mg-Si Alloys

The effects of pre-aging and natural aging on the bake hardening behavior of Al-0.62Mg-0.93Si (mass%) alloy with multi-step aging process were investigated by means of Vickers hardness test, tensile test, differential scanning calorimetry analysis (DSC) and transmission electron microscopy (TEM). The characteristics of nanoclusters (nano scale solute atom clusters) formed during pre-aging and natural aging were also investigated using the three dimensional atom probe (3DAP) analysis. The results revealed the occurrence of natural age hardening and that the bake hardening response was decreased after the extended natural aging even though the pre-aging was conducted before natural aging. Since the 3DAP results exhibited the Si-rich clusters were newly formed during extended natural aging, it was assumed that the Si-rich clusters caused the natural age hardening and the reduced bake hardening response corresponding to Cluster(1). The decrease of the bake hardening response was markedly higher in the later stage of bake hardening than in the early stage. The size of the β’’ precipitates were reduced with increasing the natural aging time. Exothermic peaks of Peak 2 and Peak 2’ were observed in the DSC curves for the alloys pre-aged at 363K. Peak 2’ became larger with the natural aging time. This is well understood by the following model. The transition from Cluster(2) to the β’’ phase occurs preferentially at the early stage of the bake hardening. Then the growth of the β’’ phase is inhibited by the presence of Cluster(1) at the later stage of bake hardening. The combined formation of Cluster(1) and Cluster(2) by the multi-step aging essentially affects the bake hardening response and the β’’ precipitates in the Al-Mg-Si alloys.

Effects of Sn Addition on Clustering and Age-Hardening Behavior in a Pre-Aged Al-Mg-Si Alloy

The effects of Sn addition on clustering and age-hardening behavior in an Al-0.6Mg-1.0Si (mass %) alloy were investigated. Addition of Sn delayed the age-hardening in single aging at 170 ̊C. On the other hand, Sn promoted the age-hardening response in 3-step aging process which comprises a pre-aging (PA) at 90 ̊C for 18ks followed by natural aging (NA) for 604.8ks and artificial aging (AA) at 170 ̊C. The characteristics of clusters formed during PA and NA were evaluated by differential scanning calorimetry (DSC) analysis and atom probe tomography (APT). The DSC results show that the endothermic peak at around 160 ̊C to 200 ̊C was observed in the Sn-free alloy. On the other hand, in the Sn-added alloy, endothermic peak was not observed. It is suggested that Sn addition suppresses the formation of the clusters formed during NA. The APT results show that the Sn addition decreases the number density of clusters, especially smaller clusters. No Sn precipitates were found in Mg-Si precipitates formed during AA at 170 ̊C for 3.6ks. It is speculated that suppression of smaller cluster formation by addition of Sn promotes the age-hardening response

A Combined TEM and Atom Probe Approach to Analyse the Early Stages of Age Hardening in AA 6016

In this study we aim at combining the results from transmission electron microscopy (TEM) and atom probe tomography (APT) to study the early stages of phase decomposition in the age hardening alloy AA 6016. Samples are subjected to different periods of natural ageing or artificial pre-ageing at elevated temperature in order to produce different types of clusters and early stages of precipitation before age hardening commences. APT is utilized to detect clusters and identify their compositions, whereas TEM is applied to analyse and quantify number density and sizes of the particles during artificial ageing at 185°C. It is shown that the two techniques, TEM and APT, are complementary and a combined approach yields more detailed insight into the early stages of phase decomposition in age hardening 6xxx series alloys than possible by the sole use of either technique individually.