Crystallization Kinetics of Amorphous Alloys Fe73.5Si13.5-xGexB9Cu1Nb3(x=3, 6)

doi:10.11901/1005.3093.2013.603

Chinese Journal of Materials Research

2014, Vol. 28

Issue (3): 204-210 DOI: 10.11901/1005.3093.2013.603

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Crystallization Kinetics of Amorphous Alloys Fe_73.5Si_13.5-_xGe_xB₉Cu₁Nb₃(x=3, 6)

Ruwu WANG^1,^3,^**(

),Jing LIU^1,²,Zhanghua GAN¹,Chun ZENG³,Fengquan ZHANG³

1. College of Materials Science and Metallurgical Engineering, Wuhan University of Science and Technology, Wuhan 430081
2. State Key Laboratory for Advanced Metals and Materials, Beijing University of Science and Technology,
Beijing 100083
3. National Engineering Research Center for Silicon Steel, Wuhan 430080

Cite this article:

Ruwu WANG,Jing LIU,Zhanghua GAN,Chun ZENG,Fengquan ZHANG. Crystallization Kinetics of Amorphous Alloys Fe_73.5Si_13.5-_xGe_xB₉Cu₁Nb₃(x=3, 6). Chinese Journal of Materials Research, 2014, 28(3): 204-210.

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Abstract

Amorphous ribbons Fe_73.5Si_13.5-_xGe_xB₉Cu₁Nb₃(x=3, 6) were prepared by a normal single copper wheel melt spinning technique in atmosphere, which then were isothermally annealed at 470℃、510℃、550℃ and 590℃ respectively for 1 h in a vacuum furnace. The microstructure and crystallization kinetics of the ribbons were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM) and differential scanning calorimeter (DSC) measurements. While the crystallization activation energies of amorphous ribbons were calculated by using Kissinger, Ozawa and Augis-Bennett models based on differential thermal analysis data. The local Avrami exponent n for primary crystallization was calculated by using Johnson-Mehl-Avrami (JMA) equation. The significant variation of local Avrami exponent n with crystallization volume fraction α demonstrated that the primary crystallization kinetics of amorphous ribbons varied at different stages. In the initial stage, the crystallization mechanism was diffusion controlled bulk crystallization with three dimensional nucleation and grain growth, while the nucleation rate deceased with time. In the following stage, it was surface crystallization with one dimensional nucleation and grain growth, while the nucleation rate was near zero. The average sizes D of α-Fe (Si, Ge) grains for the samples annealed at 510℃、550℃ and 590℃for 1 h in a vacuum furnace were less than 15 nm as confirmed both by XRD and TEM measurements.

Key words: foundational discipline in materials science Fe_73.5Si_13.5-_xGe_xB₉Cu₁Nb₃ microstructure crystallization kinetics

Received: 16 August 2013

Fund: *Supported by the State Key Lab of Advanced Metals and Materials No.2011-ZD03 and the Hubei Provincial Department of Education No.D20111103.

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https://www.cjmr.org/EN/10.11901/1005.3093.2013.603 OR https://www.cjmr.org/EN/Y2014/V28/I3/204

Fig.1 XRD patterns of as-spun samples Fe_73.5Si_13.5-_xGe_x-B₉Cu₁Nb₃ (x=3, 6)

Fig.2 DSC curves of as-spun samples Fe_73.5Si_10.5Ge₃B₉-Cu₁Nb₃ performed at various heating rates from 5–20℃/min

Fig.3 DSC curves of as-spun samples Fe_73.5Si_7.5Ge₆B₉_-Cu₁Nb₃ performed at various heating rates from 5–20℃/min

Table 1 Crystallization onset temperatures and peak temperatures (T_x1, T_p1 and T_x2, T_p2) and ΔT= T_p2-T_p1 of Fe_73.5Si_13.5-_xGe_xB₉Cu₁Nb₃ (x=3, 6) amorphous alloys obtained from DSC curves

Fig.4 Kissinger plots of as-spun samples Fe_73.5Si_13.5-_xGe_x-B₉Cu₁Nb₃ (x=3, 6), R1-the first crystallization, R2-the second crystallization

Fig.5 Ozawa plots of as-spun samples Fe_73.5Si_13.5-_xGe_x-B₉Cu₁Nb₃ (x=3, 6), R1-the first crystallization, R2-the second crystallization

Fig.6 Augis-Bennett plots of as-spun samples Fe_73.5Si_13.5-_x-Ge_xB₉Cu₁Nb₃ (x=3, 6), R1-the first crystallization, R2-the second crystallization

Table 2 The crystallization activation energies of Fe_73.5Si_13.5-x-Ge_xB₉Cu₁Nb₃ (x=3, 6) amorphous alloys, R1-the first crystallization, R2-the second crystallization

Fig.7 Local Avrami exponent n as a function of crystallized fraction α for as-spun samples Fe_73.5Si_13.5-_xGe_x-B₉Cu₁Nb₃ (x=3, 6) performed at a heating rate of 10℃/min

Fig.8 XRD patterns of as-spun sample Fe_73.5Si_10.5Ge₃-B₉Cu₁Nb₃ annealed at various temperatures for 1 h in a vacuum

Fig.9 XRD patterns of as-spun sample Fe_73.5Si_7.5Ge₆B₉-Cu₁Nb₃ annealed at various temperatures for 1 h in a vacuum

Fig.10 TEM micrographs of Fe_73.5Si_7.5Ge₆B₉Cu₁Nb₃ the as-spun sample (a) and the samples annealed at 470℃ (b), 510℃ (c), 550℃ (d), 590℃ (e) (in 1 h keeping time). The inset shows selected area electron diff raction pattern

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