Nanocrystallization of soft magnetic Fe(Co)–Zr–B–Cu alloys
Introduction
Fe-based soft magnetic alloys containing nanocrystalline precipitates embedded in an amorphous matrix are generally prepared by partial devitrification of rapidly solidified amorphous phase. The soft magnetic properties of these materials are mainly attributed to the diminishing value of magnetocrystalline anisotropy and saturation magnetostriction [1]. The strong ferromagnetic coupling of nanocrystalline phase with amorphous matrix leads to the averaging out of magnetocrystalline anisotropy and the exchange interaction forces the magnetization vector to be aligned over several grains along the field direction [2], [3]. Moreover the effective saturation magnetostriction nullifies due to the positive contribution to the magnetostriction from amorphous phase and negative contribution from nanocrystalline phase [3]. It has been found that coercivity increases 6th power of magnitude with grain size below the exchange length [4]. FINEMET, based on Fe–Si–B–Nb–Cu [5], [6]; NANOPERM, based on Fe–Zr–B–Cu [7], [8]; and HITPERM, based on Fe(Co)–Zr–B–Cu [9], [10] alloys are examples of such materials. FINEMET alloys developed by Yoshizawa et al. [5] are derived from the amorphous Fe–Si–B alloys, whereas NANOPERM and HITPERM have been developed from Fe–Zr–B glass-forming alloys [7], [9]. In both cases, Cu is added as a nucleating agent and Nb/Zr restrict the size of the nanocrystalline bcc phase.
A number of investigations have been carried out to optimize the structure and soft magnetic properties of Fe–Zr–B–Cu and Fe–Co–Zr–B–Cu alloy systems. Composition-dependent magnetic properties have been investigated using Mössbauer spectroscopy [11], [12], [13]. Kopcewicz et al [13] carried out a detailed study on structure and properties of Fe–Zr–B–Cu alloys using a special RF-Mössbauer technique which distinguishes magnetically soft nanocrystalline α-Fe particles from the magnetically hard microcrystalline α-Fe particles. Willard et al. [9], [14], [15] investigated the sequence of reaction during annealing treatment of Fe–Co–Zr–B–Cu alloys and reported that α′-FeCo (B2) nanocrystalline phase is precipitated on crystallization. Although these alloys show superior saturation magnetization and Curie temperature as compared to other nanocrystalline alloys, the coercivity and permeability are inferior.
In the present work, detailed crystallization behaviour and kinetics of crystallization of amorphous Fe–Zr–B–Cu and Fe–Co–Zr–B–Cu alloys have been investigated using differential scanning calorimeter (DSC) and X-ray diffraction (XRD). Evolution of microstructure on heat treatment above the crystallization temperature has been observed in transmission electron microscopy (TEM). Variation of magnetic properties with heat treatment temperature has been evaluated and correlated with the microstructure.
Section snippets
Experimental
Alloys of nominal compositions Fe88Zr7B4Cu1 (NP) and Fe44Co44Zr7B4Cu1 (HT) were prepared in a vacuum induction melting furnace. Rapidly solidified ribbons were produced in controlled argon atmosphere by using a vacuum melt-spinning unit. Initially, the chamber was evacuated up to 4.5×10−4 mbar followed by back filling with pure argon up to a pressure slightly below 1 atm pressure. Approximately 5–10 g alloy was melted in a quartz nozzle and the melt was ejected onto a rotating Cu wheel using Ar
Nanocrystallization
Melt spun ribbons of the NP and HT alloys yielded diffused intensity pattern in XRD spectra (Fig. 1), confirming the formation of an amorphous phase. The DSC thermograms of as-spun NP and HT alloys at a heating rate of 10 K/min are shown in Fig. 2. The temperature of onset of crystallization (Tx) for NP is 765 K, whereas HT crystallizes at a lower temperature of 750 K. The apparent activation energy of crystallization (E) was determined from DSC thermograms obtained at different heating rates
Conclusions
- 1.
NP and HT amorphous ribbons have been prepared through vacuum melt spinning.
- 2.
Crystallization of the amorphous alloys yields bcc primary phase. Addition of Co decreases the thermal stability of the amorphous phase.
- 3.
Grain-size analyses obtained from TEM micrographs suggest that the scatter in grain size of the primary phase increases with heat treatment temperature.
- 4.
The coercivity decreases initially with heat treatment temperature, attains a minimum value and then increases at higher temperature.
Acknowledgements
This work was supported by Defence Research and Development Organization (DRDO), Government of India. The authors are grateful to Dr. V Chandrasekaran for fruitful discussions and Dr. A.M. Sriramamurthy, Director, DMRL and Dr. D. Banerjee, CC R&D (AMS), DRDO for their continued support and permission to publish this work.
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