Advanced structure research methods of amorphous Co69Fe4Cr4Si12B11 microwires with giant magnetoimpedance effect: Part 3 – Cluster growth and crystal nucleation

This Part 3 focuses on the detailed study of the nanostructures forming in amorphous microwires which were previously received and described in the Part 2. The clustering process was studied at long-term DC Joule heating's much lower the crystallization temperature. Particular attention is paid to the study of the redistribution of the components of the initial stage of crystallization. The studies were carried out using the Atom Probe Tomography method (APT), which allows for the identification of individually considered atoms. A description and analysis of APT data processing techniques are provided for studying the cluster structure and distribution of elements in the amorphous matrix and crystalline phases. To identify crystalline phases, data obtained using High-Resolution Transmission Electron Microscopy (HR-TEM) and Scanning Transmission Electron Microscopy (STEM), as well as X-Ray Powder Diffraction (XRPD) with synchrotron radiation source were used. The applied techniques made it possible to establish that the formation of nuclei of crystalline phases is preceded by three stages of the amorphous microwire matrix evolution. At the first stage, clusters of the first and second coordination spheres appear. At the second stage, the clusters coagulate and become more than 2 nm in diameter, the stage ends with the predominance of Co-rich and silicide Me-Si clusters. At the third stage, they grow to an average diameter of 4.5 nm, the predominance of clusters of this type remains, and the formation of nuclei of crystalline phases α-Co and Co2Si, with a size of about 8 nm, occurs. This stage is characterized by high stable soft magnetic properties. With a further increase in the heat treatment temperature, a gradual deterioration of the soft magnetic properties and further structural transformation occur – structures of joint crystalline phases from two crystalline phases α-Co and Co2Si are formed in the amorphous matrix, and crystallization occurs with the alternation of these two phases. This leads to a significant redistribution of alloy components. As a result, an amorphous barrier layer is formed in the amorphous matrix near the surface of the growing two-phase substructures, enriched in chromium and silicon; this layer affects the growth of crystalline phases, slowing it down.