Heat-treatment on Crystallization and Dielecty Property of Mg-Al-Si-Ti-B Glass-ceramics

doi:10.15541/jim20180102

Abstract

Abstract:

Effects of different heat-treatment process on the crystallization, phase composition and content, and microstructure of 19MgO-23Al₂O₃-53SiO₂-4TiO₂-2.5B₂O₃ (wt%, M-A-S-T-B) were studied by means of differential scanning calorimeter (DSC), X-ray diffraction (XRD) and scanning electron microscope (SEM) techniques. The influence of different nucleation and crystallization time on the microwave dielectric properties were discussed as well. The results showed that, based on the controlled crystallization mechanism of glass, MgSiO₃ phase was precipitated adequately for M-A-S-T-B samples heat-treated at 850℃/2 h + 950℃/2 h, and also, the α-cordierite, xMgO-yAl₂O₃-zSiO₂ and α-SiO₂ phases could be precipitated from matrix phase. Additionally, with the increase of nucleation time, types of crystalline and phase content were found no discernible changes in the M-A-S-T-B glass-ceramics. While crystallization time increased to 20 h, the crystallized volume fraction of the glass increased, leading to the improvement of the quality factor (Q×f) and the obvious precipitation of granular grains. However, the dielectric loss slightly increased and the relative density of specimens decreased with further increase of crystallization time (30 h). Wherein, the M-A-S-T-B glass-ceramic sample heat-treated at 850℃/2 h + 950℃/20 h exhibited the excellent microwave dielectric properties of ε_r ~ 3.85, Q×f ~ 12740 GHz (at 13.973 GHz) and τ_f ~-5.37×10^-6/℃.

Key words: heat-treatment, glass-ceramics, MgSiO₃, microwave dielectric properties

CLC Number:

TM277

QU Jing-Jing, WEI Xing, LIU Fei, YUAN Chang-Lai, CHEN Guo-Hua, HUANG Xian-Pei. Heat-treatment on Crystallization and Dielecty Property of Mg-Al-Si-Ti-B Glass-ceramics[J]. Journal of Inorganic Materials, 2018, 33(12): 1309-1315.

Figures/Tables 7

Fig. 1 DSC curve of M-A-S-T-B base glass sample Inset shows the heat treatment process of the glass

Table 1 Heat treatment process of M-A-S-T-B glass

Specimens	T_g/sintering time	T_p/sintering time
1	850℃/1 h	950℃/2 h
2	850℃/2 h	950℃/2 h
3	850℃/4 h	950℃/2 h
4	850℃/8 h	950℃/2 h
5	850℃/20 h	950℃/2 h
6	850℃/2 h	950℃/1 h
7	850℃/2 h	950℃/4 h
8	850℃/2 h	950℃/8 h
9	850℃/2 h	950℃/12 h
10	850℃/2 h	950℃/20 h
11	850℃/2 h	950℃/30 h

Fig. 2 XRD patterns of the M-A-S-T-B glass-ceramics heat- treated at the same nucleation and crystallization temperatures for different time(a) 850℃/1-20 h + 950℃/2 h; (b) 850℃/2 h + 950℃/1-30 h; (c) the enlarged pattern at 2θ = 23.5-27º

Fig. 3 SEM images of the M-A-S-T-B glass-ceramics heat-treated at the same nucleation and crystallization temperatures for different time

Fig. 4 (a) SEM images of the M-A-S-T-B glass-ceramics heat-treated at 850℃/20 h + 930℃/2 h, and (b) EDS pattern of region ‘A’ marked in (a)

Fig. 5 Curves of density(r) and porosity of the M-A-S-T-B glass-ceramics heat-treated at the same nucleation and crystallization temperatures for different time

Fig. 6 Curves of εr and Q×f values of the M-A-S-T-B glass-ceramics heat-treated at the same nucleation and crystallization temperatures for different time

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