In situ TEM Study of Ni-Silicides Formation Up to 973K

Dodony, Erzsébet and Rečnik, Aleksander and Dódony, István and Sáfrán, György (2022) In situ TEM Study of Ni-Silicides Formation Up to 973K. JOURNAL OF ALLOYS AND COMPOUNDS : AN INTERDISCIPLINARY JOURNAL OF MATERIALS SCIENCE AND SOLID-STATE CHEMISTRY AND PHYSICS, 918. pp. 1-8. ISSN 0925-8388 (print); 1873-4669 (online)

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Abstract

Low-temperature solid-state reactions between Ni and Si were studied using in situ transmission electron microscopy (TEM). In the experiments thin amorphous silicon (a-Si) films were laid on Ni micro-grids and heated up to 973 K. In our approach the supporting Ni-grid serves as an unlimited source of nickel to successively form the whole range of Ni-silicide phases while diffusing into amorphous silicon. Unlike other thin film experiments where Ni and Si are layered on top of each other, our arrangement enables lateral diffusion of Ni along the Si layer and therefore enables the formation and study of successive Ni-Si phases side by side. That allowed us to observe in situ α-NiSi2 as the first reaction product, in contrast to most studies that had reported either δ-Ni2Si or θ-Ni2Si as the first phase to form. α-NiSi2 was continuously present at the reaction front propagating into the a-Si film. The phase sequence followed the increasing Ni concentration from a-Si towards the Ni-grid: α-NiSi2, NiSi, Ni3Si2, δ-Ni2Si, γ-Ni31Si12 and Ni3Si. Almost all known Ni-silicide phases were found to form at relatively low temperatures except the θ-Ni2Si, β-NiSi2 and β3-Ni3Si. The dominant phase was γ-Ni31Si12 which appeared in three structural modifications, differing in lattice periodicity along the c-axis. The periodicity of the basic γ-Ni31Si12 structure along the c-axis is ~12 Å (c0 = 12.288 Å) and that of the other two modifications were ~18 Å and ~36 Å, denoted by S12, S18 and S36 respectively. Of the three, only S12 has a structural model, S18 had been previously observed by Chen, but S36 had not been documented in previous works. During our in situ heating experiments, in addition to the Ni-silicide layer formation a new phenomenon was observed, namely the appearance, growth and transformation of Ni-silicide whiskers which was attributed to the accumulation of compressive stress in the thin layer.

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