Ni2+掺杂尖晶石相透明微晶玻璃制备及光学性能

doi:10.15541/jim20170347

摘要/Abstract

摘要：

实验制备了Ni²⁺掺杂的ZnO-MgO-Al₂O₃-SiO₂(ZMAS)体系的透明微晶玻璃, 研究了微晶玻璃的超宽带发光现象。热分析结果表明样品的玻璃化转变温度(T_g)和析晶峰温度(T_c)分别为754℃和948℃。采用X射线粉末衍射分析了两种热处理制度对玻璃的晶体形核、晶体生长及物相变化的影响, 结果表明: 采用阶梯温度热处理制度可以得到Ni²⁺掺杂的尖晶石相透明微晶玻璃。紫外-可见吸收光谱和荧光光谱测试表明制备的Ni²⁺掺杂ZMAS微晶玻璃中Ni²⁺以四配位和六配位共同存在于尖晶石相中, 红外荧光中心位于1324 nm的样品荧光半高宽达490 nm。样品的超宽带荧光主要是由于微晶玻璃中六配位Ni²⁺在ZnAl₂O₄和MgAl₂O₄形成的尖晶石相固溶体晶体场中的³T_2g(³F)→³A_2g(³F) 能级跃迁。实验结果表明, 制备的微晶玻璃在超宽带光纤放大器等光子器件中具有潜在的应用前景。

关键词: 超宽带发光, 尖晶石, 微晶玻璃, 近红外发光

Abstract:

Transparent Ni²⁺-doped ZnO-MgO-Al₂O₃-SiO₂ (ZMAS) system glass-ceramics with broadband infrared luminescence were prepared by heat-treatment of parent glass via melt quenching method. According to DTA results, glass transition temperature (T_g) and maximum crystallization temperature (T_c) of the as-prepared samples are 754℃ and 948℃, respectively. Glass-ceramics obtained from two different heat-treatment systems were characterized by X-ray diffraction, and crystallization behaviors and phase transitions were analyzed. The results show that transparent Ni²⁺-doped spinel-phase glass-ceramics can be obtained by using two-step heat-treatment process. Ultraviolet-visible absorption spectra and luminescence spectra of the prepared glass-ceramics were investigated. The results indicate that tetrahedral and octahedral sites Ni²⁺ ions coexist in spinel microcrystals of Ni²⁺-doped ZMAS system glass-ceramics. The broadband infrared luminescence centered at 1324 nm with full width at half maximum (FWHM) of about 490 nm was observed from the samples. Mechanism underlined these phenomena is attributed to the transitions of ³T_2g(³F)→³A_2g(³F) of octahedral six-folded Ni²⁺ in the solid solution of spinel structure of Zn/MgAl₂O₄. These data confirm that the glass-ceramics may have potential applications for photonic devices such as super broadband optical fiber amplifiers.

Key words: broad band infrared luminescence, spinel, glass-ceramics, infrared luminescence

中图分类号:

TQ171

焦志伟, 段翠翠, 周伟, 刘峰斌, 杨越, 赵攀, 项俊帆. Ni²⁺掺杂尖晶石相透明微晶玻璃制备及光学性能[J]. 无机材料学报, 2018, 33(6): 673-677.

JIAO Zhi-Wei, DUAN Cui-Cui, ZHOU Wei, LIU Feng-Bin, YANG Yue, ZHAO Pan, XIANG Jun-Fan. Preparation and Infrared Luminescence of Transparent Ni²⁺-doped ZMAS Glass-ceramics[J]. Journal of Inorganic Materials, 2018, 33(6): 673-677.

图/表 7

表1 Ni掺杂ZMAS玻璃成分/g

Table 1 Composition of Ni2+-doped ZMAS glass/g

Composition	Content/g	Composition	Content/g
MgO	3.420	ZrO₂	2.790
ZnO	8.940	NiO	0.733
Al₂O₃	20.753	Na₂SO₄	0.320
SiO₂	31.710	NaNO₃	0.360
TiO₂	4.890	SnO₂	0.165

图1 Ni掺杂ZMAS玻璃的DTA (黑色)和TG (红色)曲线

Fig. 1 DTA (black line) and TG (red line) curves of Ni2+-doped ZMAS glass

图2 等温热处理不同时间得到的玻璃样品的XRD图谱

Fig. 2 XRD patterns of glass samples isothermal heat-treated at 800℃ for different time

图3 利用阶梯温度热处理制度得到玻璃样品的XRD图谱

Fig. 3 XRD patterns of glass samples treated by two-step heat-treatment process

图4 Ni掺杂ZMAS微晶玻璃样品的吸收光谱和外观形貌

Fig. 4 Absorption spectra of Ni2+-doped ZMAS glass-ceramic samplesInsets represent the images of polished samples. (b)-(e) indicate the crystallization temperature of 900℃, 950℃, 1000℃ and 1050℃, respectively

图5 Ni掺杂ZMAS微晶玻璃的荧光光谱

Fig. 5 Luminescence spectra of Ni2+-doped ZMAS glass- ceramic samples

图6 近红外荧光光谱峰位置与热处理温度关系

Fig. 6 Dependence between the peak position of the infrared luminescence and the heat-treatment temperature

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Ni²⁺掺杂尖晶石相透明微晶玻璃制备及光学性能

Preparation and Infrared Luminescence of Transparent Ni²⁺-doped ZMAS Glass-ceramics

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