铌酸钾钠基透明上转换陶瓷材料制备及性能

doi:10.15541/jim20140131

摘要/Abstract

摘要：

采用热压烧结工艺, 以LiBiO₃作为烧结助剂, 制备了铌酸钾钠基透明上转换陶瓷K_0.5(1-_y₎Na_0.5(1-_y₎Li_yNb_1-_yBi_yO₃- Er_0.005Yb_0.005_x(Er³⁺/Yb³⁺:KNNLB, x=0~3, y=0~0.09)。并对其微观结构、光学透光率和上转换效应等进行了研究。结果表明该透明陶瓷具有正交钙钛矿型结构, 晶粒尺寸约0.5 μm, 致密度较高。该材料在红外区和可见光区有良好的透明性, 但是随着铒镱掺杂量的增加, 可见光区透光率呈明显的下降趋势。当y=0.06、x=0时, 在可见光范围内透过率可达到45%(样品厚度为0.5 mm), 红外光区域透过率达到95%以上。铒镱共掺杂透明陶瓷实现了在波长900 nm氙灯光源激发下的上转换效应。

关键词: 铌酸钾钠, 透明陶瓷, 热压烧结, 上转换发光

Abstract:

Upconversion transparent ceramics K_0.5(1-_y₎Na_0.5(1-_y₎Li_yNb_1-_yBi_yO₃-Er_0.005Yb_0.005_x(Er³⁺/Yb³⁺:KNNLB, x=0-3, y=0-0.09) were fabricated by hot-press sintering process using LiBiO₃as additives. The microstructure, optical transparency and upconversion fluorescence were investigated．The results show that the crystalline phase of the ceramics is orthorhombic-perovskite structure．The ceramics are well densified, and the grain size of the ceramics is about 0.5 μm．These ceramics present good transparency in the infrared and the long-wavelength visible regions, but the optical transparency declines rapidly in the visible region as the amount of Yb³⁺ and Er³⁺ions increases．The transparency of the ceramics with y = 0.06 and x = 0 reaches 45% in the visible region and over 95% in the infrared region(the thickness of the sample is 0.5 mm)．The strong upconversion fluorescence is observed when the ceramics are excited by the 900 nm-wavelength light of an xenon lamp．

Key words: sodium potassium niobate, transparent ceramic, hot-pressing, upconversion emission

中图分类号:

TQ174

耿志明, 李坤, 施东良, 施瑕玉, 黄海涛, 陈王丽华. 铌酸钾钠基透明上转换陶瓷材料制备及性能[J]. 无机材料学报, 2014, 29(12): 1265-1269.

GENG Zhi-Ming, LI Kun, SHI Dong-liang, SHI Xia-Yu, HUANG Hai-Tao, CHAN Helen Lai Wa. Preparation and Performance of KNN-based Upconversion Transparent Ceramics[J]. Journal of Inorganic Materials, 2014, 29(12): 1265-1269.

图/表 7

图 1 Er3+/Yb3+:KNNLB(x=0~3, y=0.06)透明陶瓷的XRD图谱

Fig. 1 XRD patterns of Er3+/Yb3+:KNNLB(x=0-3, y=0.06) transparent ceramics

图 2 Er3+/Yb3+:KNNLB透明陶瓷的SEM照片

Fig. 2 SEM images of Er3+/Yb3+:KNNLB transparent ceramics (a) Without LiBiO3 additives; (b) Added 6mol% LiBiO3 additives

图 3 Er3+/Yb3+:KNNLB(x=0~3, y=0.06)陶瓷实物照片

Fig. 3 Photographs of Er3+/Yb3+:KNNLB transparent ceramics (x=0-3, y=0.06)

图 4 (a) Er3+:KNNLB(y=0.06)陶瓷和(b) Er3+/Yb3+:KNNLB (x=0~3, y=0.06)陶瓷的紫外可见透光率

Fig. 4 Transmittance of Er3+:KNNLB (y=0.06) ceramics (a) and Er3+/Yb3+:KNNLB (x=0-3, y=0.06) ceramics (b) in UV- visible region

图 5 Er3+/Yb3+:KNNLB(x=0~3, y=0.06)陶瓷红外透光率

Fig. 5 Transmittance of Er3+/Yb3+:KNNLB(x=0-3, y=0.06) ceramics in infrared region

图 6 900 nm激发下Er3+/Yb3+:KNNLB(x=0~3, y=0.06)陶瓷的上转换荧光光谱

Fig. 6 Upconversion spectra of Er3+/Yb3+: KNNLB (x=0-3, y=0.06) ceramics at excitation of 900 nm

图 7 900 nm激发下Er3+/Yb3+:KNNLB陶瓷上转换发光的能级跃迁

Fig. 7 Schematic energy level diagram of Er3+and Yb3+ in Er3+/Yb3+:KNNLB ceramics at excitation of 900 nm

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