The sessile-drop method and high-temperature small-angle x-ray diffraction technique were used to characterize the density of liquid Al–Si alloys with Si content C = 0 to 22 wt%. A distinct abnormal volume expansion of the hyper-eutectic melts was identified just above the liquidus (within TL–Tk) during the heating sequence (h.s.), which is irreversible during the cooling sequence (c.s.). This phenomenon is explained by the segregation of Si atoms from the supersaturated “quasi-eutectic” structure and formation of silicon clusters in the superheated melt. In addition, a pre-peak in the x-ray diffraction spectrum of Al–14% Si melt was observed at 850 °C, which is associated with the silicon clusters. The pre-peak remains when the superheated melt is cooled down to the liquidus (670 °C); this result is in accord with the density measurements.
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