Structure modification and recovery of amorphous Fe73.5Si13.5B9Nb3Cu1 magnetic ribbons after autoclave treatment: SAXS and thermodynamic analysis

doi:10.1016/j.jmst.2018.09.010

Abstract

Abstract:

The structure, crystallization kinetics and magnetic property of as-quenched Fe_73.5Si_13.5B₉Nb₃Cu₁ amorphous ribbon (R0) as well as ribbons after autoclave treatment at 100?°C and 150?°C (R1 and R2) have been systematically studied by various techniques. With increasing autoclave treatment temperature, the measured structural, kinetic and magnetic parameters of samples increase firstly, i.e. R0?r_M) MRO (medium range order), but increase the small r_M MRO. The measured structural, thermal and magnetic parameters of R2 sample have a tendency to recover toward as-quenched R0 sample. The thermal and magnetic parameters of samples after solely annealing treatment at higher temperature have no obvious recover phenomenon. The uneven actions of pressure and temperature in autoclave treatment may be helpful for us to search a new method to improve the magnetic properties of Fe-based glasses.

Key words: SAXS (small-angle X-ray scattering), Fe-based glass, Thermodynamic, Magnetic ribbon, DSC (differential scanning calorimetry)

L.Y. Guo, X. Wang, K.C. Shen, K.B. Kim, S. Lan, X. WangL., W.M. Wang. Structure modification and recovery of amorphous Fe_73.5Si_13.5B₉Nb₃Cu₁ magnetic ribbons after autoclave treatment: SAXS and thermodynamic analysis[J]. J. Mater. Sci. Technol., 2019, 35(1): 118-126.

Figures/Tables 14

Fig. 1. XRD pattern of Fe73.5Si13.5B9Nb3Cu1 amorphous ribbons under different autoclave treatments.

Fig. 2. (a) SAXS data and fitting results for Fe73.5Si13.5B9Nb3Cu1 amorphous ribbons under different autoclave treatments, (b) the pair distance distribution function p(r) curve deduced from the SAXS by indirect Fourier transformation.

Fig. 3. DSC curves for Fe73.5Si13.5B9Nb3Cu1 amorphous ribbons under different autoclave treatments at a heating rates of (a) 20?°C/min and (b) 40?°C/min; inset in (a) gives the Curie temperature of samples.

Table 1 Characteristic temperatures of exothermic peak in the DSC patterns for Fe73.5Si13.5B9Nb3Cu1 amorphous ribbons under different autoclave treatments.

Sample		β (^oC/min)
(^oC)
R0	10	518	663	536.3	682.5	322.6	320.9
	20	526	669	546.1	692.6	320.6
	30	531	676	551.6	699.4	321.3
	40	534	678	554.2	702.0	319.4
R1	10	518	662	537.0	682.8	323.6	321.9
	20	526	668	546.7	693.2	321.3
	30	531	675	551.6	698.8	321.8
	40	535	678	553.9	701.3	320.9
R2	10	517	660	536.0	682.1	322.3	321.3
	20	526	669	544.8	692.6	321.6
	30	533	677	551.3	699.7	321.1
	40	536	679	554.2	701.7	320.2

Fig. 4. Kissinger plot for calculation of activation energies for Fe73.5Si13.5B9Nb3Cu1 amorphous ribbons. The activation energie corresponds to the first exothermic peak: (a) the onset temperature and (b) the peak temperature; the second exothermic peak: (c) the onset temperature and (d) the peak temperature.

Fig. 5. DSC data and crystallized volume fraction (α) curves related to the first exothermic peak for as-quenched Fe73.5Si13.5B9Nb3Cu1 amorphous ribbons at different heating rates.

Fig. 6. Dependence of local activation energy E(α) on the crystalline fraction α for the primary crystallization process of Fe73.5Si13.5B9Nb3Cu1 amorphous ribbons under different autoclave treatments.

Fig. 7. Normalized z(α) function curves obtained by transformation of non-isothermal data at different heating rate for the primary crystallization process of as-quenched Fe73.5Si13.5B9Nb3Cu1 amorphous ribbons.

Fig. 8. (a) Suri?ach representations of non-isothermal DSC curves for the primary crystallization process of Fe73.5Si13.5B9Nb3Cu1 amorphous ribbons under different autoclave treatments at the heating rate of 20?°C/min. Scatter plots is the experimental results. Continuous lines are the plots for the theoretical NGG kinetics with different m value. (b) Local Avrami exponent n(α) vs crystallized volume fraction for the first stage which fits JMA model.

Table 2 Parameters of NGG stages for the primary crystallization reaction of different samples at the heating rate of 20?°C/min.

Sample	Stages	α	lnA₀	m
R0	Stage I-NGG	0.41-0.87	60.0	1.1(m_I)
R0	Stage II-NGG	0.87-0.97	58.8	0.5(m_II)
R1	Stage I-NGG	0.40-0.86	63.5	1.4(m_I)
R1	Stage II-NGG	0.86-0.97	61.5	0.4(m_II)
R2	Stage I-NGG	0.41-0.87	59.1	1.1(m_I)
R2	Stage II-NGG	0.87-0.97	57.8	0.5(m_II)

Table 3 Values of a, b and ω when α?=?0.15, 0.25 and 0.35, and the roots of Eqs. (13) and (14) for as-quenched sample when heating rate is 20?°C/min. The bold case 4 has the lowest standard deviation.

Case No.	α	E(α)	n	ω	a	b	Roots of Eq. (13) (kJ/mol)	Roots of Eq. (14) (kJ/mol)	Standard Deviation (kJ/mol)
1	0.15	420.51	2.00	0.5	1.50	1	E_n?=?442.23 E_g?=?355.12	E_n?=?442.13 E_g?=?355.44	σ_n?=?0.11 σ_g?=?0.32
	0.25	414.74	1.58	0.5	1.08	1
	0.35	408.31	1.28	0.5	0.78	1
2	0.15	420.51	2.00	0.5	1.50	1	E_n?=?442.23 E_g?=?355.12	E_n?=?426.24 E_g?=?403.26	σ_n?=?15.99 σ_g?=?48.14
	0.25	414.74	1.58	0.5	1.08	1
	0.35	408.31	1.28	0.5	0.28	2
3	0.15	420.51	2.00	0.5	1.50	1	E_n?=?424.27 E_g?=?409.17	E_n?=?426.24 E_g?=?403.26	σ_n?=?1.97 σ_g?=?5.91
	0.25	414.74	1.58	0.5	0.58	2
	0.35	408.31	1.28	0.5	0.28	2
4	0.15	420.51	2.00	0.5	1.00	2	E_n?=?442.23 E_g?=?398.68	E_n?=?442.13 E_g?=?398.78	σ_n?=?0.10 σ_g?=?0.10
	0.25	414.74	1.58	0.5	0.58	2
	0.35	408.31	1.28	0.5	0.28	2

Table 4 Nucleation and growth activation energies of Fe73.5Si13.5B9Nb3Cu1 amorphous ribbons under different autoclave treatments.

Sample	ω	α?=?0.15		α?=?0.25		α?=?0.35		E_n (kJ/mol)	E_g (kJ/mol)
Sample	ω	a	b	a	b	a	b	E_n (kJ/mol)	E_g (kJ/mol)
R0	0.5	1.00	2	0.58	2	0.28	2	442.2	398.7
R1	0.5	1.49	1	0.55	2	0.24	2	410.4	403.7
R2	0.5	1.17	2	0.74	2	0.43	2	424.5	375.6

Fig. 9. Magnetic hysteresis loops of Fe73.5Si13.5B9Nb3Cu1 amorphous ribbons under different autoclave treatments.

Fig. 10. Schematic diagram for structural, thermal and magnetic parameters variation with temperature and pressure.

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Structure modification and recovery of amorphous Fe_73.5Si_13.5B₉Nb₃Cu₁ magnetic ribbons after autoclave treatment: SAXS and thermodynamic analysis

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