The Influence of Nanocrystalization of the FeSiB Amorphous Alloy by Means of Nd: YAG Pulsed Laser heating on its Magnetic Properties.

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1 Solid State Phenomena Vol. 94 (2003) pp (2003) Trans Tech Publications, Switzerland doi: / The Influence of Nanocrystalization of the FeSiB Amorphous Alloy by Means of Nd: YAG Pulsed Laser heating on its Magnetic Properties. A.Sypie, J.Kusi ski, T.Stobiecki, M.Czapkiewicz University of Mining and Metallurgy, 30 Mickiewicza Ave., Krakow, Poland Keywords: nanocrystallization; amorphous alloy; laser heating; magnetic properties; Abstract. The influence of laser heating on the magnetic properties and microstructure of amorphous FeSiB alloy ribbon was examined. The material was nanocrystallized by means of Nd: YAG pulsed laser heating. The use of laser beam of relatively low energy, with subsequent overlapping of heated areas, resulted in a much more homogeneous nanostructure of the ribbon. Magnetic properties, the coercivity field, the saturation of magnetization M S, and the slope of the hysteresis loop (dm/dh) H Hc were determined by means of (R-VSM) rezones vibrating sample magnetometer.. These measurements give the information that such heat treatment does not influence on the magnetization saturation M S and the differential magnetic susceptibility, as compared to the amorphous state. Introduction Nanocrystalline materials, are understood to be single- or multi-phase materials with a grain size smaller than 100 nm in at least one dimension. Owing to the extremely small dimensions, nanocrystalline materials are structurally characterized by a large volume fraction of grain boundaries or interphase boundaries. This may significantly alter a variety of physical, mechanical, and chemical properties compared to those of conventional coarse-grained polycrystalline materials [1]. Many properties of nanocrystalline materials are found to be fundamentally different from, and often superior to, those of the conventional polycrystalline and the amorphous solids [2,3]. For example, nanocrystalline materials may exhibit increased strength and hardness, improved ductility and toughness, reduced elastic modulus, enhanced diffusivity, higher specific heat, enhanced thermal expansion coefficient, and superior soft magnetic properties in comparison to conventional polycrystalline materials. In particular, the nanocrystalline structure might be significant in the improvement of brittle materials ductility, such as ceramics and some intermateriallics [4, 5]. Our previous researches [6], by using of Lorenz microscopy, showed that laser annealing of the amorphous ribbons refines their magnetic domain structure. The aim of this the research was to study the influence of laser nanocrystallization of amorphous FeSiB ribbons on microstructure and magnetic properties. Experimental For the microstructural investigations (TEM) and magnetic properties characterization 3 mm discs were cut from Fe 80 Si 11 B 9 as-cast amorphous ribbons. The discs were locally heat treated using the Nb: YAG pulsed laser radiation of TEM 00 mode. The characteristic parameters of the laser heat treatment are listed in table 1. All rights reserved. No part of contents of this paper may be reproduced or transmitted in any form or by any means without the written permission of TTP, (ID: , Pennsylvania State University, University Park, United States of America-04/06/14,01:23:29)

2 76 Interfacial Effects and Novel Properties of Nanomaterials Series Parameters Constant parameters: energy density [J/cm 2 ] defocus step [mm] number of laser pulses: I II III IV 1 HZ frequency; 6,6 ms time ; TIP 12 mm Table.1. The characteristic parameters of laser heat treatment. The magnetic measurements were conducted by using of R-VSM vibrating sample magnetometer. Five series of the laser annealed samples were examined. Results and discussion The structural changes of the amorphous material after laser annealing, with the variable treatment parameters, are shown in Fig.1. Microstructural analyses showed that application of the selected laser treatment parameters permits the desired degree of crystallisation of amorphous material, which increased with the laser energy density and the number of laser pulses used to heat the sample. The degree of a crystallization can be shown by the analysis of the diffraction pattern types. The number of rings which represent nanocrystalline phases increases (see Fig.1.IV), when the crystallization degree increases. I II III IV Fig.1. TEM image and selected area diffraction pattern of FeSiB after laser heating. I -1 J/cm 2,11 mm, 2 pulses, II - 1 J/cm 2, 11 mm, 3 pulses. III - 2 J/cm 2,16 mm, 1 pulses, IV - 2 J/cm 2, 16 mm, 2 pulses. The thermal shock that accompanied the pulsed laser heating caused the appearance of the many crystalline nuclei in the amorphous matrix. The average size of the nanocrystals is about 20 nm. Due to the very short laser pulse duration (6.6 ms) subsequent laser pulses did not cause crystal growth but induced the appearance of new nanocrystals. Indeed, annealing of the amorphous material with several subsequent pulse laser heating (using 1 J/cm 2 energy density) produced a fine nanocrystalline microstructure. After annealing with the higher energy density (2 J/cm 2 ) the

3 Solid State Phenomena Vol samples showed a dendritic type of microstructure which however still remains nanocrystalline. The large dendrites (of 300 nm) are composed of the very fine subgrains (of diameter less than 30 nm). The magnetic properties were investigated by means of the resonance vibration sample magnetometer (R-VSM). The sample magnetization µ 0 M (measured at the field of H = 700 ka/m) slightly increased with the number of laser pulses and the laser energy density (1.20 T T). The magnetic hysteresis loops of the laser treated samples (Fig. 2) shows that the slope ((dm/dh) H Hc ) decreased slightly with the increased intensity of laser treatment. This means that the pulsed laser nanocrystallization of FeSiB amorphous ribbon does not significantly influence the magnetization saturation M S and the differential magnetic susceptibility, compared to amorphous state. 1.5 I I I I II I V µ0ms[t] H [ka/ m ] Fig.2. The comparison of coercive field of the samples that were laser treated to the variable parameters (see Table.1.). laser treated Fig.3. The comparison of X - ray diffraction of samples that were laser treated with variable parameters. Intensity annealed 650 C Th e ta

4 78 Interfacial Effects and Novel Properties of Nanomaterials Figure 3 shows X-ray diffraction patterns (a) of the material conventionally annealed at 650 C for 1 h and (b) the pulsed laser annealed material. On the diffraction pattern for conventionally annealed material the α-fe (Si) and the Fe 2 B phases were identified. The diffraction pattern of the laser annealed material is different. Only one strong diffraction line of α-fe (Si)-{110} crystalline phases is present, while the other lines are very weak. This corresponds well, with the TEM diffraction patterns. The broadening of the line (2θ = ) is caused by the presence of both amorphous and nanocrystalline phases. Summary The research proved that the pulsed laser treatment (using of 1 J/cm 2 laser energy density) with several subsequent pulses resulted in a homogeneous nanostructure, with the average nanocrystals grain size being less than 25 nm. It seems that the laser energy supplied during the very short laser pulses to metastable amorphous material involves the appearance of the new nanocrystalline nuclei, rather than causing the growth of existing crystals. During annealing with a higher energy density (2 J/cm 2 ) eutectic type of crystallization occurs. As a consequence, large dendrites (of 300 nm) are present in microstructure. They are composed of the very fine nanocrystalline subgrains (of diameter less than 30 nm). Pulsed laser nanocrystallization of FeSiB amorphous ribbon has no significant influence on the magnetization saturation M S, or differential magnetic susceptibility, compared to amorphous state. Acknowledgement This work was supported by the Polish State Committee for Scientific Research (KBN), grant No. PBZ/KBN - 013/T08/11. References [1] K. Lu: Material Science and Engineering, R 16 (1996), p. 161 [2] H. Gleiter, Prog. Mater.Sci., 33 (1989), p. 223 [3] R. Birringer, Mater. Sci. Eng. A, 117 (1989), p. 33 [4] J. Karch, R. Birringer and H. Gleiter, Nature, 330 (1987), p.536. [5] R. Bohn, T. Haubold, R. Birringer and H. Gleiter, Scr. Metall. Mater., 25 (1991), p [6] J.Kusi ski, A. Sypie, G. Kusi ski, C. Nielson: Tem studies of the FeSiB amorphous alloy nanocrystalized by means of Nd: YAG pulsed laser heating, Proceedings XI International Conference on Electron Microscopy of Solids, (2002), is press.

5 Interfacial Effects and Novel Properties of Nanomaterials / The Influence of Nanocrystallization of the FeSiB Amorphous Alloy by Means of Nd: YAG Pulsed Laser Heating on its Magnetic Properties / DOI References [5] R. Bohn, T. Haubold, R. Birringer and H. Gleiter, Scr. Metall. Mater., 25 (1991), p doi: / x(91)90230-x

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