铽离子掺杂锆酸钡粉体制备及其光学性能研究

doi:10.15541/jim20150279

摘要/Abstract

摘要：

采用水热法合成了不同铽离子掺杂量的BaZrO₃粉体, 采用XRD、SEM、FTIR、荧光光谱仪等检测方法对样品的结构、形貌及光学性能进行表征。对部分水热产物进行煅烧处理, 研究温度对其发光性能的影响。结果表明, 水热产物均为立方钙钛矿结构, 铽离子掺杂进入BaZrO₃晶格, 占据B位Zr的位置。样品的微观形貌为粒度分布较为均匀的球体。不同铽掺杂量得到的BaZrO₃球体在244 nm光激发下均观察到了来自基体的宽带发射和Tb³⁺的特征发射峰, 且在Tb³⁺掺杂浓度为5mol%附近峰值最大。温度对发光性能影响显著, 随着煅烧温度的升高, 发光强度逐渐减弱。

关键词: 锆酸钡, 铽掺杂, 光学性能, 猝灭

Abstract:

Tb³⁺doped BaZrO₃ powders at different Tb³⁺ concentrations were synthesized by hydrothermal method. The structure, morphology and luminescence properties of the synthesized materials were examined by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectrum (FTIR) and fluorescence spectrometer, respectively. Parts of hydrothermal products were calcinated to study the effect of temperature on luminescence properties. Analysis results showed that Tb was successfully introduced into the lattice and replaced Zr at B site of perovskite. It was remarkable that all the samples had similar morphology, which was composed of evenly distributed spheres. The broadband emission peaks of the host and the typical emission peaks of Tb³⁺ were observed in the BaZrO₃ doped with Tb³⁺under 244 nm excitation, and these peaks reach the maximum at Tb³⁺ ion content of 5mol%. Temperature had significant influence on their photoluminescence properties. With the calcination temperature increase, the luminescent intensity of Tb³⁺ doped samples was decreased.

Key words: barium zirconate, Tb-doped, optical properties, quenching

中图分类号:

TB321

杨雨佳, 王晶, 何慧芬. 铽离子掺杂锆酸钡粉体制备及其光学性能研究[J]. 无机材料学报, 2016, 31(1): 27-33.

YANG Yu-Jia, WANG Jing, HE Hui-Fen. Synthesis and Luminescence Properties of Tb³⁺ Doped BaZrO₃ Powders[J]. Journal of Inorganic Materials, 2016, 31(1): 27-33.

图/表 11

图1 不同铽离子掺杂量BaTbxZr1-xO3样品的XRD图谱(Ⅰ)和(200)晶面衍射峰的放大图谱(Ⅱ)

Fig. 1 XRD patterns of BaTbxZr1-xO3 samples (Ⅰ) and magnified diffraction peak of (200) crystals face (Ⅱ)

表1 不同铽离子掺杂量BaTbxZr1-xO3样品的晶胞参数

Table 1 Lattice parameters of BaTbxZr1-xO3 samples with different concentrations

Tb³⁺ion content/mol%	0	1	3	5	6
Lattice parameter, a/nm	0.420171	0.420645	0.420840	0.421319	0.421313

图2 不同煅烧温度下BaTb0.05Zr0.95O3样品的XRD衍射图谱(Ⅰ)和(200)晶面衍射峰的放大图谱(Ⅱ)

Fig. 2 XRD patterns of BaTb0.05Zr0.95O3 samples (Ⅰ) and magnified diffraction peak of (200) crystals face (Ⅱ)

表2 不同煅烧温度下BaTb0.05Zr0.95O3样品的晶胞参数

Table 2 Lattice parameters of BaTb0.05Zr0.95O3 samples calcined at different temperatures

Calcination temperature /℃	Room temperature	300	500	700	1000
Lattice parameter, a/nm	0.421319	0.420105	0.418911	0.418974	0.419034

图3 BaTbxZr1-xO3样品 (x=0, 0.01, 0.03, 0.05, 0.06) 的SEM照片

Fig. 3 SEM images of samples of (a)~(e) assigned to BaTbxZr1-xO3 (x=0, 0.01, 0.03, 0.05, 0.06), respectively

图4 不同煅烧温度下BaTb0.05Zr0.95O3样品的SEM照片

Fig. 4 SEM images of BaTb0.05Zr0.95O3 samples calcined at 300 ℃(a), 500 ℃(b), 700 ℃(c) and 1000 ℃(d), respectively

图5 不同铽离子掺杂量BaTbxZr1-xO3样品的红外光谱图

Fig. 5 FT-IR spectra of BaTbxZr1-xO3 samples (a-f assigned to 0, 1mol%, 3mol%, 4mol%, 5mol% and 6mol%, respectively)

图6 不同煅烧温度下BaTb0.05Zr0.95O3样品的红外光谱图

Fig. 6 FT-IR spectra of BaTb0.05Zr0.95O3 samples calcined at different temperatures (a-e) assigned to room temperature, 300 ℃, 500 ℃, 700 ℃ and 1000 ℃, respectively

图7 BaTbxZr1-xO3样品的荧光激发光谱(λem=546 nm)

Fig. 7 Excitation spectra of BaTbxZr1-xO3 samples (λem=546 nm) (a) BaZrO3; (b) BaTb0.03Zr0.97O3

图8 不同铽离子掺杂量BaTbxZr1-xO3样品的荧光发射光谱(λex=244 nm)(Ⅰ)和546 nm处的荧光强度随Tb3+掺杂量变化图(Ⅱ)

Fig. 8 Emission spectra of BaTbxZr1-xO3 samples (λex=244 nm) (Ⅰ) and the relationship point diagram of Tb3+ doping amounts and emission intensity of 546 nm (Ⅱ)

图9 不同煅烧温度下BaTb0.05Zr0.95O3样品的荧光发射光谱图(λex=244 nm)

Fig. 9 Emission spectra of BaTb0.05Zr0.95O3 samples calcined at different temperatures (λex=244 nm)

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