Yasuhiro Aruga

In situ observations of compressive behaviour of aluminium foams by local tomography using high-resolution X-rays

We have investigated the compressive behaviour of closed-cell aluminium foams using a high-resolution X-ray CT. The microstructures of cell walls or Plateau borders in the foams were visualized in 3D using the local tomography technique which is a high-resolution CT method to reconstruct a region of interest within a large sample. The shapes and the 3D distribution of micropores, particles, and regions of solute segregation in the foams are evaluated, comparing the cell walls with the Plateau borders. Under compressive loads, the damage behaviour of such microstructures has been observed using an in situ test rig. It is found that the microcracks were mainly initiated from the cell walls and the micropores with large diameters were also damaged. The crack initiation sites are classified from the results. In addition, a method for non-destructive characterization of elastic and plastic deformation in the foams, which is called a 3D microstructure gauge (MG) method, is presented. Thousands of micropores as markers on each load were automatically matched by the information of those volumes and surface areas. The local strain mapping by the MG indicates that the edges of the micropores with large diameters have large strain under compression and this is consistent with the crack analyses.

In Situ Observation of Fracture of Aluminium Foam Using Synchrotron X-Ray Microtomography

Synchrotron X-ray microtomography has been utilized for the 3D characterisation of microstructure in the cell materials of aluminium foams. Tomographs, consisting of about 109 isotropic voxels with a maximum of 1.0µm edge, were collected at the SPring-8 in Japan. A combination of high-resolution phase contrast imaging technique and several state-of–the-art application techniques has enabled the quantitative image analyses of micro-pore, intermetallic particles and grain boundary as well as the assessment of their effects on compressive deformation and fracture behaviours in two kinds of aluminium foams.

Effects of Zn Addition and Aging Condition on Serrated Flow in Al-Mg Alloys

The serrated flow phenomena in Al-Mg alloys with and without Zn were investigated after aging on several conditions, focusing on the role of precipitates. Al-6mass%Mg-0~3mass%Zn alloys were solution treated at 753~803K, quenched, and then aged at room temperature. Further artificial aging at 323~573K for 86.4ks was performed for some of them after natural aging for 2.6Ms. The serrated flow behavior was evaluated by tensile test. Microstructure was characterized by differential scanning calorimetry, transmission electron microscopy, atom probe tomography, and positron annihilation lifetime spectroscopy. The increase in the amount of Zn addition and the natural aging time lead to a delayed onset of serrated flow. The artificial aging at higher temperatures after natural aging, on the other hand, decreases the onset strain. A large number of small coherent Zn-Mg clusters are formed during natural aging in the Al-Mg-Zn alloys, which are transformed to the larger incoherent meta-stable precipitates during subsequent artificial aging. These results suggest that the mechanism of interfering with serrated flow is related to the vacancy trapping effect, which is enhanced by the coherent clusters.

Application of Local Tomography Technique to High-Resolution Synchrotron X-Ray Imaging

X-ray CT method is a kind of nondestructive inspection, but has strong limitation in sample size due to a small field of view (FOV). The higher the resolution, the smaller FOV is, mainly due to the element number of available detectors commercially. Therefore, sample machining is more or less necessary so that the sample size is fit within the small FOV in the case of the high-resolution observation. Local tomography technique enables a high resolution reconstruction of small region of interests within a sample without the sample machining. In this study, we have evaluated the size effects of aluminum foam samples in terms of the 3D image quality by the local tomography techniques.

Influence of experimental parameters on the composition of precipitates in metallic alloys.

We report on the change in the shape, size and composition of spherical precipitates, found in an Fe-Cu and an Al-Ag alloy, as the base temperature, pulsing mode and parameters are adjusted. In the case of the Al-Ag alloy, the difference in the evaporation field between precipitates and matrix can be minimised at low temperature, while in the Fe-Cu alloy minimal changes are observed within the range of experimental conditions investigated. Comparison with transmission electron microscopy shows that some experimental conditions yield accurate precipitates size, while others enable reaching accurate composition measurements.

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 Cu or Li Addition and Multi-Step Aging Conditions on the Bake-Hardenability of an Al-Mg-Si Alloy

In recent years, automobiles with lower fuel consumption are required because the exhaust fume is severely regulated. The weight-saving is quite effective to realize such low fuel consumption, and therefore aluminum alloy becomes attractive as an alternative material of steels due to its high specific strength. 6XXX series Al-Mg-Si alloys exhibit good bake-hardenability during paint-bake treatment in the automobile manufacturing process, but to reduce further environmental impact, the paint-baking temperature is supposed to be lowered than the present temperature of about 443K. In this study, it was aimed to investigate the attained hardness after paint-bake treatment at various temperatures of 408-443K for an Al-0.55wt%Mg-0.90wt%Si alloy with/without microalloying elements of Cu and Li. The effects of multi-step aging conditions; e.g. pre-aging, natural aging and paint-bake treatments, were also investigated through Vickers hardness test, TEM observation and DSC analysis. From the obtained experimental results, it was clarified that the addition of Cu or Li to the Al-Mg-Si alloy increases the attained hardness even at a paint-baking temperature of 408K due to the increased volume fraction of precipitates. Furthermore, pre-aging treatment at 373K for 18ks was also effective in suppressing the increase in hardness during natural aging, resulting in the highest attained hardness among the investigated multi-step aging conditions; i.e. HV100 in the Li-added alloy paint-baked at 408K.

Effect of Mg or Ag addition on the evaporation field of Al.

It is known that the distribution of the charge-states as well as the evaporation field shift to higher values as the specimen temperature is decreased at a constant rate of evaporation. This study has explored the effect of Mg or Ag addition on the evaporation field of Al in terms of the charge state distribution of the field evaporated Al ions. The fractional abundance of Al(2+) ions with respect to the total Al ions in Al-Mg alloy is lower than that in pure Al, whereas it shows higher level in the Al-Ag alloy at lower temperatures. The temperature dependence of the fractional abundance of Al(2+) ions has been also confirmed, suggesting that Al atoms in the Al-Mg alloy need lower evaporation field, while higher field is necessary to evaporate Al atoms in the Al-Ag alloy, compared with pure Al. This tendency is in agreement with that of the evaporation fields estimated theoretically by means of measurements of the work function and calculations of the binding energy of the pure Al, Al-Mg and Al-Ag alloys.

Three-Dimensional Zinc Mapping inside Aluminum Foams Using Synchrotron X-Ray Microtomography

Three-dimensional zinc mapping based on X-ray K-edge scanning has been performed. By microtomographies with energies above and below the K-absorption edges of the elements, the concentration distribution of the elements is evaluated during in-situ experiments, respectively. It is found that the Zn concentration distribution during the heat treatment was changed inside the cell wall of the aluminum foams and it has been homogenized. Also several precipitated phase transformation can be three-dimensionally visualized by the CT-method tuning X-ray energies.