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1.
Microsc Microanal ; 25(2): 349-355, 2019 04.
Article in English | MEDLINE | ID: mdl-30871649

ABSTRACT

A procedure to analyze the elemental concentration distribution inside solute clusters after detection of clusters from atom probe tomography data set was proposed. We developed a code which can directly illustrate an average concentration profile inside a cluster even in the case of including various sizes of ellipsoidal clusters. The profile can be with respect to absolute distance and includes errors in each data point. The reliability of the developed code was verified by analyzing an artificial cluster model which has inhomogeneous elemental distribution. It was found that the precise estimation of cluster centroids is important and that the preferable conditions for targeting clusters are a detection efficiency of over 20%, over 30 atoms in a cluster on average, and over 100 atoms for each concentration data point.

2.
Sci Rep ; 8(1): 16629, 2018 Nov 09.
Article in English | MEDLINE | ID: mdl-30413757

ABSTRACT

Atomic scale characterization of fine precipitates in an under-aged Cu added Al-Mg-Si alloy was carried out by combination of atomically-resolved annular dark-field scanning transmission electron microscopy and energy dispersive X-ray spectroscopy. Two types of precipitates were observed in the alloy. In the case of ordered ß" precipitates, ß" was proposed as Mg5-xAl2+xSi4 (x ≈ 1) with solute Cu atoms replacing Al site of ß" precipitate. In the case of disordered precipitates, the precipitates were found to consist of ß" sub-unit cells, three-fold symmetric structure without Cu atoms, Cu containing structures termed as "Cu sub-unit cluster", and Q' sub-unit cells. Among these structures, the morphologies of three-fold symmetric structure without Cu atoms, Cu sub-unit cluster, and Q' sub-unit cell were almost the same, so that these structures should be the clusters of Q' phase. Since the areal density, length and diameter of precipitates were almost equal between Cu free Al-Mg-Si alloy and Cu added Al-Mg-Si alloy, the increase of hardness by Cu addition should be due to the precipitation of Cu related precipitates, such as Cu sub-unit clusters and Q' sub-unit cells.

3.
Microscopy (Oxf) ; 65(2): 169-76, 2016 Apr.
Article in English | MEDLINE | ID: mdl-26520787

ABSTRACT

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.

4.
Ultramicroscopy ; 132: 199-204, 2013 Sep.
Article in English | MEDLINE | ID: mdl-23480959

ABSTRACT

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.

5.
Ultramicroscopy ; 132: 31-5, 2013 Sep.
Article in English | MEDLINE | ID: mdl-23234834

ABSTRACT

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.

6.
Ultramicroscopy ; 111(6): 725-9, 2011 May.
Article in English | MEDLINE | ID: mdl-21295913

ABSTRACT

A temporal evolution of clusters associated with age hardening behavior in a Cu-Ni-P alloy during ageing at 250 °C for up to 100 ks after solution treatment has been carried out. A three-dimensional atom probe (3DAP) analysis has showed that Ni-P clusters are present in the as-quenched condition, and that the cluster density increases as the ageing time increases. The clusters have a wide range of Ni/P ratios when they are relatively small, whereas larger clusters exhibit a narrow distribution of the Ni/P ratio, approaching a ratio of approximately two. These results would indicate that the clusters with various Ni/P ratios form at the early stage of precipitation and the ratio approaches a value identical to that of the equilibrium phase at 250 °C as the clusters enlarge during ageing.

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