Synthesis and characterization of Fe–Mn–Si shape memory alloy by mechanical alloying and subsequent sintering

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Abstract

An Fe‐Mn‐Si bulk alloy was produced from elemental powders by mechanical alloying (MA) and subsequent sintering. The shape memory effect, microstructure and mechanical property of the bulk alloy were investigated. The α phase transformed into the γ phase during MA. The MA played an essential role in stabilizing the γ phase, which is associated with the shape memory effect in this alloy system. The γ phase with small amounts of ε and α′ martensitic phases formed after subsequent sintering. After deformation, a γ→ε stress-induced martensitic phase transformation occurred. Shape recovery was observed after subsequent heating, associated with an ε→γ reverse martensitic transformation. The grain size of the bulk alloy was about 2–3 μm, and the yield strength was about 500 MPa. These results show that powder metallurgy, a combination of MA and subsequent sintering, has the potential to produce Fe–Mn–Si shape memory alloy.

Introduction

Fe–Mn–Si alloys are a prominent system with a characteristic shape memory effect (SME). The SME of the Fe–Mn–Si alloy system has been undergone continued development since its discovery by Sato et al. in 1982 [1], [2], [3]. Because the alloying elements (Fe, Mn and Si) are relatively inexpensive, this system has been expected to be a promising alternative to expensive Ti–Ni-based shape memory alloys. While the SME of the Ti–Ni-based alloys occurs due to a thermo-elastic martensitic phase transformation, the effect in the Fe–Mn–Si alloys originates from a stress-induced γ (fcc)→ε (hcp) martensitic transformation, followed by an ε→γ reverse transformation during heating. The stress-induced martensitic transformation occurs due to the motion of Shockley partial dislocations in the fcc structure; the Burgers vector a/6[112¯]FCC glides between two (111) layers of the fcc lattice. The γ phase forms and is stabilized at room temperature by the substitution of Mn and Si atoms in the α (bcc) phase lattice (elemental α-Fe). The stress-induced martensitic transformation dominates, overwhelming slip deformation within 3–4% deformation of the Fe–Mn–Si shape memory alloy [3]. The composition and additional alloying elements have been optimized in order to maximize SME for applications. Basic composition was established as Fe–(28–33)Mn–6Si (wt%) after the discovery of the SME in this alloy system [3], [4]. The addition of Cr (Fe–28Mn–6Si–5Cr) produced a stronger SME [5]. Furthermore, a combination of Cr and Ni (Fe–16Mn–5Si–12Cr–5Ni) led to better corrosion resistance, while still exhibiting the SME [5]. It has also been found that the SME can be further improved by the formation of fine precipitates of NbC [6] or VN [7]. In the meantime, a variety of industrial applications has been considered. Recently, construction components such as pipe joints and rail couplings have been discussed as potential applications of the Fe–Mn–Si-based shape memory alloys [8]. In general the Fe–Mn–Si-based shape memory alloy is produced by melting and subsequent casting under high vacuum (or in air) followed by thermo-mechanical processing [1], [2], [3], [4], [5], [6], [7].

Powder metallurgy offers several advantages for manufacturing industrial products. It enables the production of alloys in near net shape, minimizing the additional machining required to form the final product, compared with casting techniques. Therefore, it is worth exploring the alternative production route for the Fe–Mn–Si shape memory alloys. Mechanical alloying (MA) is a prominent synthetic technique involving solid state reaction among powders due to high energy collisions [9]. This offers many advantages, such as reduced grain size, the formation of intermetallic compounds, the ability to synthesize alloys from elements with different melting points and the capability of producing nano-sized structures [9]. These characteristic advantages can lead to excellent mechanical properties as well as other unique properties. MA of the Fe–Mn–Si alloy system has been discussed from the viewpoint of alloying kinetics [10] and thermal stability [11], resulting in the formation of a stabilized γ phase in the alloyed powder. We reported [12] the synthesis of Fe–Mn–Si alloy by MA and subsequent sintering, and discussed repeatability of the MA. However, further characterization and analysis of the SME and mechanical properties have not yet been reported. A better knowledge of this alternative production route could offer a broader range of applications for the Fe–Mn–Si shape memory alloy. The aim of this study is to attempt to produce Fe–Mn–Si shape memory alloy by MA and sintering from elemental powders, and to investigate the SME, microstructure and mechanical properties of the resulting alloy.

Section snippets

Experimental procedures

Commercially available electrolytic Fe (99.9%), electrolytic Mn (99.9%) and atomized Si (99.9%) elemental powders (100 mesh) with a chemical composition of Fe–30Mn–6Si (wt%) were mechanically alloyed in a stainless steel vial (45 ml) with several stainless steel balls (diameter was 15 mm). The ball-to-powder weight ratio was approximately 8:1. The atmosphere in the vial was argon in order to minimize oxygen contamination during the MA. The MA was performed using a planetary ball mill (a

Phase evolution during the synthesis

Fig. 3 shows XRD patterns for Fe–30Mn–6Si powder after MA for 5, 10, 20, 30 and 50 h, indicating that the α phase (initial phase) existed at the early stages of MA (5 and 10 h). However, the prominent XRD peaks corresponding to the α phase vanished after MA for 20 h. After MA for 20 h, peaks corresponding to the γ phase appeared. This suggests that the α phase transformed to the γ phase during MA. An XRD pattern for the Fe–30Mn–6Si powder after MA for 50 h indicates no difference from that for 20 h.

Conclusions

In this study, we attempted to synthesize Fe–Mn–Si shape memory alloy by MA, sintering and annealing. We then investigated the SME, microstructure and mechanical properties of the resulting alloy. The Fe, Mn and Si elemental powders transformed into the γ and ε phases from the α phase during MA due to diffusion of Mn and Si atoms into the Fe matrix. After subsequent sintering and annealing, the γ phase and small amounts of the ε and α′ martensitic phases formed. Without prior MA, γ phase

Acknowledgments

The authors would like to thank Dr. M. Sikora, Dr. J. Żukrowski and Prof. J. S. Szmyd, AGH University of Science and Technology, Krakow Poland, for their experimental support and further discussion. One of the authors (T. S.) would like to appreciate Prof. K. Aoki, Shibaura Institute of Technology, Tokyo Japan, for his experimental support (deformation) and further discussion.

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    Present affiliation: Norwegian University of Science and Technology (NTNU), Trondheim, Norway.

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