Elsevier

Powder Technology

Volume 213, Issues 1–3, 10 November 2011, Pages 36-40
Powder Technology

Preparation of amorphous Fe-based magnetic powder by water atomization

https://doi.org/10.1016/j.powtec.2011.06.026Get rights and content

Abstract

Fe–Si–B–C–P amorphous powders were fabricated successfully by water atomization. The morphology, chemical composition, phase structure and soft magnetic properties were then studied in this work. The results indicate that the powders are completely amorphous in nature. DSC analyses show that the powders have a glass transition temperature Tg about 768 K and a crystallization temperature Tx about 816 K, which are almost the same to those of the bulk form. The morphology of the powders can be modified by adjusting the water atomization parameters, and both dendritic particles and spherical particles can be made. Compared with the gas-atomized powders and the bulk form made by casting, the water-atomized powders contain a higher amount of oxygen (about 1800 ppm), and also a higher content of Fe. It suggests that the high content of oxygen impurity may further increase the glass forming ability and a higher content of Fe may increase the saturation magnetization of the material. The water-atomized powders can be easily densified into bulk forms. The soft magnetic properties depend on the densification and heat treatment temperatures. The bulk Fe-based metallic glass, made by using the water-atomized powders, has a saturation magnetization as high as 1.64 T and a value of coercivity as low as 5.9 A/m. Therefore, the water-atomized powders are very cost-effective and suitable for industrial applications.

Graphical abstract

Fe–Si–B–C–P metallic glass powder can be manufactured by high-pressure water atomization. The powders are completely amorphous in nature, and have a Tg about 768 K and Tx about 816 K. The soft magnetic properties depend on the heat treatment temperature. The saturation magnetization increases with the heat treating temperatures, and a value as high as 1.64 T is obtained.

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Highlights

► We successfully prepared Fe-based metallic glass powder by water atomization. ► Oxygen may not be a critical concern for the glass forming ability of this process. ► The magnetic properties are excellent for electronic applications.

Introduction

Fe-based metallic glass has a very low coercivity and a high saturation magnetization, thus is considered as promising soft magnetic materials [1], [2]. In 1982, Inoue et al made the first Fe75Si10B15 metallic glass with a diameter of 0.27 mm [3], and in 1995 developed a Fe73Al5Ga2P11C5B4 metallic glass in a diameter of 1 mm [4]. Since then, many Fe-based bulk metallic glass compositions have been found, for example, Fe70B20Zr8Nb2 and Fe56Co7Ni7Hf8M2 (M = Nb or Ta) [5], [6], Fe30Co30Ni15Si8B17 [7]. In 2003, V. Ponnambalam and S. Joseph Poon developed a nonferromagnetic amorphous steel with a critical diameter of 4 mm [8]. In 2004, Lu and Liu developed a Fe-based metallic glass composition with a critical diameter of 14 mm [9], and in 2005, Shen also added rare earth elements in a Fe-Co-Cr-Mo-C-B alloy and obtained a critical diameter of 16 mm [10].

For magnetic applications, the Fe–Si–B system is usually studied, because of their superior magnetic properties, such as the relatively high saturation magnetization of 1.5–1.7 T, good magnetic softness due to lack of intrinsic magneto-crystalline anisotropy, and also low material cost and excellent productivity [11]. However, the glass forming ability of this system is very low, and usually ribbons as thin as 25 μm, made by melt-spinning, were used. Recently, bulk metallic glasses based on Fe–Si–B–C–P have reportedly a good glass forming ability (a critical size of 3 mm) and high saturation magnetization (1.5 T) [12]. However, this critical size still limits the outer shape and the application of Fe-based metallic glass in a bulk form. Thus, Fe–Si–B metallic glasses are usually used as powder cores. The fabrication process includes the disintegration of the ribbons, mixing with polymers and consolidation.

Bulk metallic glasses can also be made by powder metallurgy, which is a process much more flexible in controlling the size, shape and microstructures of the components. Metallic glass powders can be made by atomization methods and mechanical alloying. In atomization, usually high purity raw materials and Ar are used, in order to decrease the impurity level and increase the glass forming ability. This is especially essential for making Zr-based and Al-based metallic glass powders due to their high affinity to oxygen. Recently, Lu et al reported to develop a Fe–Si–B–C–P bulk metallic glass by using industrially raw materials [13]. This implies that the Fe-based metallic glass may not be as sensitive to impurities as other metallic glass systems. So far, there are some researches on making Fe-based metallic glass powder by the atomization method [14], [15]. In this work, the authors tried to fabricate Fe–Si–B–C–P metallic glass powders by using water-atomization, rather than the costly gas-atomization, and investigate the chemical and physical properties of the powders.

Section snippets

Experimental

Pure Fe(99%), Fe–Si, Fe–B, Fe–P and C (99%) were mixed according to a nominal composition of Fe76Si7.6B9.5P5C1.9 (in atomic percent), and then induction-melted for several times to make sure the compositional homogeneity in vacuum. The Fe76Si7.6B9.5P5C1.9 master alloy was re-melted in an induction furnace at 1473 K, and atomized by water under a pressure of about 20 MPa. The disintegrated melt droplets were cooled down in the chamber, and solidified to powders. The as-atomized slurry was then

Results

Fig. 1 shows the XRD patterns of the as-atomized powders. The powders are fully amorphous without distinct crystalline phases. Thus, water-atomization is a fast enough process to suppress the formation of crystalline phase. The cooling rate can be estimated to be 103–105 °C/s. The similar calculation model was reported in Ref. [16].

Fig. 2 shows the DSC trace of the as-atomized Fe-based metallic glass powder at a heating rate of 10 K/s in an Ar atmosphere. The Tg, Tx and ΔTx of the powder are 768 

Discussions

The glass formability of the Fe–Si–B bulk metallic glasses (BMGs) can be increased by adding glass-forming metal elements, such as Al, Ga, Nb, Mo and Y [1], [17], [18], [19]. These alloys have critical diameters of tens of millimeters. However, the glass-forming metal elements in BMGs result in a remarkable decrease in the saturation magnetization, which is much lower than that of the Fe–Si–B amorphous alloys. P is also an important element for increasing the glass forming ability of Fe-based

Conclusions

Fe–Si–B–C–P metallic glass powder can be successfully manufactured by high-pressure water atomization. The powders are completely amorphous in nature. The powders have a Tg about 768 K and Tx about 816 K, which are almost the same to those of the cast materials. The morphology of the powders can be modified by adjusting the water atomization parameters, and both dendritic and spherical particles can be made. The water-atomized powders can be easily densified into compacts due to their irregular

Acknowledgement

The authors are grateful for the financial supports from National Natural Science Foundation of China under contract Nos. 51021063 and 50823006.

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