The microstructural evolution of intermetallic compound layers formed in Fe/Zn diffusion couples (DCs) was examined by optical and scanning electron microscopies and electron-probe microanalysis. In the solid-Fe/liquid-Zn DCs at 450°C, the δ
p phase nucleates between the δ
k, and ζ phases after dipping for about 100 s and every intermediate phase seems to obey the square root law individually before and after the appearance of the δ
pphase at 100 s. In the concentration-penetration profiles, a composition gap is observed in the δ
p phase of the solid-Fe/liquid-Zn DCs dipped for a long time at temperatures ranging from 450 to 550°C, while only a singular point, but no gap, is obtained in the DCs dipped at elevated temperatures over 575°C. On the other hand, in the case of the solid-Fe/solid-Zn DCs at 400°C, the d phase instead of the δ
pphase appeares later between the δ
pand Γphases and finally covers the whole δ region.
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