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通过差热分析(DTA),X射线衍射(XRD)研究、热膨胀系数(CTE)测定及扫描电镜(SEM)观察等实验手段,研究了以 LiO-Al-SiO系统为基础的光纤接头用微晶玻璃材料在低温晶化预处理阶段和高温模拟拉丝条件下的相转变过程.研究结果表明,该微晶玻璃材料在870℃出现的DTA放热峰为β-石英固溶体析晶峰,该亚稳晶相在升高温度后转变为主晶相β-辉石固溶体.在900~1000℃晶化预处理阶段,主晶相的晶粒尺寸在0.2~0.3μm之间,随温度和时间的变化不明显,材料显微结构细密.在1150~1270℃范围内,晶粒尺寸随温度增加迅速长大,玻璃相明显增多.研究还表明,在预处理阶段,由于β-石英固溶体向β-锂辉石固溶体的转变和β-锂辉石固溶体析出量的逐渐饱和,材料的热膨胀系数由小变大并趋于稳定;而在高温模拟拉丝温度下,由于玻璃相的明显增多,材料的热膨胀系数随温度升高迅速增大.

Phase transitions of Li2O-Al2O3-SiO2 based glass-ceramic materials, which can be used for the fabrication of optical fiber ferrule, were studied by
means of DTA, XRD, SEM and CTE. The temperature range of the phase transition studied was 850~1270℃. The results show that the metastable
β-quarts s.s first precipitates at 870℃ and translates into the β-spodumene s.s, the prominent crystal phase, at higher temperature. Increasing the heat-treatment temperatures from 900℃ to 1000℃ and prolonging
the time, the size of the granule changes little. With the transition of β-quarts s.s. to the β-spodumene s.s, the CTE of the material increases greatly and
then it gradually stabilizes when the transition is completed. During the heat-treatment of the material at 1150~1270℃, the granule size grows and the glass
phase increases quickly. At the same time, the CTE of the material increases too.

参考文献

[1] Ueda T, et al. Proceeding of IEICE Japan 1993 Conference, C--315 (in Japanese)
[2] Sakamoto A. New Glass, 1999, 14 (1): 26--31.
[3] Suzuki N, et al. Japanese Unexamined Patent Publication No.56--165109, A
[4] Takeuchi Y, et al. Japanese Unexamined Patent Publication No.08--17130, A
[5] Mitachi S, et al. Glass Technol., 1998. 39 (3): 98--99.
[6] Nagase R, et al. Electronics Letters, 1997, 33 (14): 1243--1244.
[7] Hsu Jen-Yan, et al. J.Am.Ceram. Soc., 1989, 72 (12): 2334--2341.
[8] Chyung C K. J. Am. Ceram. Soc., 1969, 52 (2): 242--245.
[9] Beall G H, et al. Corning Research, 1987, 21--35.
[10] 袁彪, 陈全庆. 特种玻璃, 1988, 5 (3): 42--45.
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