----------CaSi2O2N2:Eu2+中空荧光纤维的制备及其发光性能研究

doi:10.15541/jim20130639

无机材料学报 ›› 2014, Vol. 29 ›› Issue (10): 1029-1033.DOI: 10.15541/jim20130639

----------CaSi₂O₂N₂:Eu²⁺中空荧光纤维的制备及其发光性能研究

崔博, 王宏志, 李耀刚, 张青红

(东华大学纤维材料改性国家重点实验室, 材料科学与工程学院, 上海 201620)

收稿日期:2013-12-05 修回日期:2014-03-20 出版日期:2014-10-20 网络出版日期:2014-09-22
作者简介:崔博(1986–), 男, 博士研究生. E-mail: cui2005bo@126.com
基金资助:
国家自然科学基金(51072034);高等学校博士点基金(20110075130001);上海市科委纳米科技专项(12nm0503-900)

Synthesis and Properties of Hollow CaSi₂O₂N₂:Eu²⁺ Luminescence Fibers

CUI Bo, WANG Hong-Zhi, LI Yao-Gang, ZHANG Qing-Hong

(State Key Laboratory for Modification of Chemical Fibers and Polymer Materials, College of Materials Science and Engineering, Donghua University, Shanghai 201620, China)

Received:2013-12-05 Revised:2014-03-20 Published:2014-10-20 Online:2014-09-22
About author:CUI Bo. E-mail: cui2005bo@126.com
Supported by:
Natural Science Foundation of China (51072034);Specialized Research Fund for the Doctoral Program of Higher Education(20110075130001);Science and Technology Commission of Shanghai Municipality (12nm0503900)

摘要/Abstract

摘要：

采用静电纺丝与气相还原氮化相结合的方式制备了用于白光LED的CaSi₂O₂N₂:Eu²⁺荧光纤维。通过调节纺丝溶液溶剂的配比, 得到了空心结构的Ca-Si-O-Eu纳米纤维和CaSi₂O₂N₂:Eu²⁺荧光纳米纤维。样品在微观上保持中空纤维结构, 宏观上也保持薄膜的状态。利用X射线衍射对样品物相结构进行分析, Ca-Si-O-Eu中空纤维在1300℃保温5 h后得到层状结构的CaSi₂O₂N₂, Eu²⁺离子的掺入没有改变CaSi₂O₂N₂的主晶相。在400 nm激发光照射下CaSi₂O₂N₂:Eu²⁺荧光纤维在550 nm附近具有一个宽发射峰, 对应着Eu²⁺离子4f⁶5d→4f⁷跃迁。与CaSi₂O₂N₂:Eu²⁺荧光粉或普通荧光纤维膜比较, 制备的中空荧光纤维膜有更高的发射光强度。

关键词: 中空纤维, 静电纺丝, 荧光纤维, 氮氧化物

Abstract:

Hollow Eu²⁺ doped CaSi₂O₂N₂ and Ca-Si-O-Eu nanofibers were prepared through electrospinning combined with gas-reduction-nitridation method. The Ca-Si-O-Eu precursor was smooth and uniform, has a length arrange from ten to hundred micrometers. The as-obtained sample not only keeps the hollow structure but also assembles to a film. XRD patterns reveal that the sample nitrided under 1300℃ for 5 h are crystallized well and maintained CaSi₂O₂N₂ phase after Eu²⁺ doping. The emission spectra of Eu²⁺ doped CaSi₂O₂N₂ under the 400 nm ultraviolet light irradiation has a board peak centered at 550 nm, which results from Eu²⁺ 5d-4f transition. In comparison with CaSi₂O₂N₂:Eu phosphor powders and fiber film, the hollow CaSi₂O₂N₂:Eu phosphor fiber film has stronger emission intensity under PL measurement.

Key words: hollow fiber, electrospinning, luminescence fiber, oxynitride

中图分类号:

TB34

崔博, 王宏志, 李耀刚, 张青红. ----------CaSi₂O₂N₂:Eu²⁺中空荧光纤维的制备及其发光性能研究[J]. 无机材料学报, 2014, 29(10): 1029-1033.

CUI Bo, WANG Hong-Zhi, LI Yao-Gang, ZHANG Qing-Hong. Synthesis and Properties of Hollow CaSi₂O₂N₂:Eu²⁺ Luminescence Fibers[J]. Journal of Inorganic Materials, 2014, 29(10): 1029-1033.

图/表 7

图1 初生纤维及其经过不同温度处理后得到样品的XRD图谱

Fig. 1 XRD patterns of the samples treated at different temperatures and different atmospheres

图2 不同氮化温度下荧光纤维的XRD图谱

Fig. 2 XRD patterns of luminescence fibers nitride at different temperatures

图3 纳米纤维的FE-SEM照片

Fig. 3 FE-SEM images for nanofiber Precursor (a), hollow nanofiber at low magnification (b) and high magnification (c)

图4 中空纳米纤维形成机理

Fig. 4 Illustrative scheme for the formation mechanism of hollow nanofiber

图5 1300℃氮化后样品(a), 截面低倍(b)和高倍(c)FESEM照片

Fig. 5 FE-SEM image of samples nitrided at 1300℃ (a), cross section image at low maganification (b) and high magnification (c)

图6 CaSi2O2N2:Eu空心纳米纤维的(a)激发光谱和(b)发射光谱

Fig. 6 Excitation spectrum (a) and emission spectrum (b) of hollow CaSi2O2N2:Eu nanofibers Inset is the photo of the nanofibers under the 365 nm ultraviolet light

图7 CaSi2O2N2:Eu 不同氮化条件下得到产物的荧光光谱

Fig. 7 Photoluminescence spectra of the CaSi2O2N2: Eu powders and fibers

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----------CaSi₂O₂N₂:Eu²⁺中空荧光纤维的制备及其发光性能研究

Synthesis and Properties of Hollow CaSi₂O₂N₂:Eu²⁺ Luminescence Fibers

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