介孔LaVO4: Eu3+的制备和荧光性能*

doi:10.11901/1005.3093.2013.820

材料研究学报

2014, Vol. 28

Issue (1): 1-7 DOI: 10.11901/1005.3093.2013.820

本期目录 | 过刊浏览

介孔LaVO₄: Eu³⁺的制备和荧光性能^*

刘国聪^1,³(

),董辉¹,韦庆敏²,朱立刚²,梁达文²

1. 惠州学院化学工程系惠州 516007
2. 玉林师范学院新材料研发与化学生物传感技术所玉林 537000
3. 中南大学化学化工学院长沙 410083

Preparation and Luminescence of Mesoporous LaVO₄: Eu³⁺

Guocong LIU^1,^3,^**(

),Hui DONG¹,Qingmin WEI²,Ligang ZHU²,Dawen LIANG²

1. Department of Chemical Engineering, Huizhou University, Huizhou 516007
2. Institute of Advanced Materials & Chembiosensing Technology, Yulin Normal University, Yulin 537000
3. College of Chemistry and Chemical Engineering, Central South University, Changsha 410083

引用本文:

刘国聪,董辉,韦庆敏,朱立刚,梁达文. 介孔LaVO₄: Eu³⁺的制备和荧光性能^*[J]. 材料研究学报, 2014, 28(1): 1-7.
Guocong LIU, Hui DONG, Qingmin WEI, Ligang ZHU, Dawen LIANG. Preparation and Luminescence of Mesoporous LaVO₄: Eu³⁺[J]. Chinese Journal of Materials Research, 2014, 28(1): 1-7.

全文: PDF(4029 KB) HTML

摘要:

以硝酸镧(La(NO₃)₃·6H₂O)、硝酸铕 (Eu(NO₃)₃·6H₂O)、偏钒酸铵(NH₄VO₃)为原料, 以十六烷基三甲基溴化铵(CTAB)为模板剂, 用研磨-溶胶-凝胶法制备了三维蚯蚓状LaVO₄: Eu³⁺介孔材料, 并用XRD、XPS、 TEM、 BET、IR 、FL等手段表征了材料的结构、形貌、比表面积、孔径分布及荧光性能。结果表明, 在673 K焙烧所得的样品是四方锆石型结构的介孔材料, 其比表面积达179.5 m²/g, 平均孔径为2.56 nm , 孔容积为0.115 m³/g, 晶粒尺寸6.38 nm, 表现出很强的红光发射(⁵D₀→⁷F₂)。适当提高焙烧温度能提高样品的红光发射, 但焙烧温度过高(≥1273 K)则破坏材料介孔结构并使其荧光强度急剧降低。

关键词 ：无机非金属材料, LaVO₄: Eu³⁺介孔, 研磨-溶胶法, 量子效率, 荧光性能

Abstract：

Using cetyltrimethyl ammonium bromide (CTAB) as a template agent, a facile grinding sol-gel process was adopted to prepare earthworm-like LaVO₄: Eu³⁺ mesoporous material with La(NO₃)₃·6H₂O, Eu(NO₃)₃6H₂O and NH₄VO₃as raw materials. The as-prepared samples were characterized by X-ray diffraction (XRD), X-ray photoelectron energy spectrum (XPS), transmission electron microscopy (TEM), the BET specific surface area, infrared spectra (IR) and fluorescence spectra (FL). It is found that the as-prepared LaVO₄: Eu³⁺ annealed at 673 K is a typical mesoporous materal with zircon structure of tetragonal phase (t). The specific surface areas and the average pore diameter of the sample is about 179.5 m²/g and 2.56 nm, respectively, and its pore volume and grain size is 0.115 m³/g and 6.40 nm, respectively. The fluorescence results show that the mesoporous LaVO₄: Eu³⁺ exhibits a strong red emission (⁵D₀→⁷F₂), and a suitable range of annealing temperature can improve its fluorescence properties, but more high annealing temperature (≥1273 K) can rapidly decrease its fluorescence intensity due to demolishing the mesoporous structure of LaVO₄: Eu³⁺.

Key words： inorganic non-metallic materials grinding sol-gel synthesis mesoporous LaVO₄: Eu³⁺ quantum efficiency fluorescence

收稿日期: 2013-11-04

基金资助:* 国家自然科学基金项目(51162026), 广西科学技术开发项目(10100003-2), 广西自然科学基金项目(2011GXNSFA018049), 广东自然科学基金项目(S2012010009632), 广东高校人才资助项目[(2012)41-2050205], 惠州市科学技术项目(2012P09)和惠州学院科技项目资助。

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图1 样品LaVO4:Eu3+的广角和小角(插图)XRD谱

图2 样品的TG-DSC曲线

图3 介孔LaVO4:Eu3+的XPS谱

表1 介孔LaVO4:Eu3+中各元素的光电子结合能位置和原子分数

图4 介孔LaVO4:Eu3+的TEM、HRTEM、FFT和EDS像

图5 LaVO4:Eu3+的N2吸附-脱附曲线

图6 不同煅烧温度所得样品的TEM像

图7 介孔LaVO4:Eu3+ 样品的红外光谱图

图8 介孔LaVO4:Eu3+的室温激发和发射光谱

图9 焙烧温度对荧光强度的影响

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