第33卷第2期 2014年2月
中国材料进展 MATERIALSCHINA
Vol.33No.2 Feb.2014
热处理温度及EDTA对β-NaYF4：Yb3+，Er3+
材料结构与性能的影响袁新生，顾士甲，王连军，江莞（东华大学纤维改性国家重点实验室，上海201620）
摘
要：采用共沉淀法合成了Yb3+、Er+共掺杂的NaYF。粉体，重点研究了热处理温度和整合
剂EDTA对所合成粉体的晶相、表面形貌以及上转换发光性能的影响，并利用X射线衍射、扫描电镜及荧光光谱对其结构组成、晶体表面形貌及发光性能进行了研究。结果表明：随着热处理温度的升高，NaYF。：Yb3+，Er+粉体由立方相向六方相转变，当温度高于600℃时又从六方相遥渐转变为立方相，面且颗粒的尺寸逐渐变大，从近似球形到无规则形状；NaYF4：Yb3·，EF+发光强度与热处理温度密切相关，热处理温度对于β-NaYF。：Yb>+，Er+的发光性能有着重要的影响。经过 600热处理后的粉体具有较高的发光强度；整合剂EDTA的添加对所合成粉体的发光性能有着明显的影响，整合剂的添加降低了其发光强度；在1000℃以内，NaYF：Yb3+，E+具有良好的热
袁新生
稳定性。
关键词：NaYF4：Yb3+，Er+；热处理；整合剂；上转换发光
中图分类号：TB34、TQ124.3
文献标识码：A
文章编号：16743962(2014)02012005
The Effect of Heat Treatment Temperature and EDTA on Structure and Performance of β-NaYF4 : Yb3+ , Er3 +
YUAN Xinsheng,GU Shijia,WANG Lianjun,JIANG Wan( State Key Laboratory for Modification of Chemical Fibers and Polymer Materials,
Donghua University, Shanghai 201620, China)
Abstract: Ytterbium (Yb3*) and erbium (Er*) ions co-doped sodium yttrium fluoride was prepared by precipitation method in the presence of EDTA as a chelating agent. The research is mainiy focused on the effect of EDTA and calcina-tion temperature on the powder crystal phase, surface morphology and the luminous performance. The phase composition, microstructure and property of luminescence are characterized by XRD, SEM and fluorescence spectrophotometer. The ex-perimental results showed that with the increase of heat treatment, phase transition frorm cubic to hexagonal of NaYF, : Yb3-, Er powder occurred. When the temperature reached higher than 600 C , the hexagonal phase gradually trans-formed to cubic phase, and the size of the particles increased gradually, from approximately spherical to random shape; The luminous intensity of NaYF, : Yb3+, Er+ is closely related to heat treatment temperature, which has an important efect on the luminous properties., NaYF。: Yb*, E* heated at 600 C shows the relative strongest upconversion( UC) luminous intensity; The powder synthesized with EDTA shows evident effect on the intensity of UC emission, and makes
UC luminous intensity weaker; NaYF : Yb3+, Er+ has a good thermal stability below 1 000 °C. Key words: NaYF,: Yb3+, Er+: heat treatment; chelating agent; up-conversion luminescence
1前言
上转换发光材料通常包括基质、激活剂和敏化剂。以NaYF，作为基质的氟化物材料，是一种效率最高的上收稿日期：2013-1114
基金项目：国家自然科学基金（11179028）
作者简介：衰新生，男，1987年生，颈士研究生，Email：yxs
dh123@ 126. com
DOI; 10. 7502/j. issn. 1674 3962. 2014. 02. 08
转换基质材料之一，具有较低的声子能量（300~ 400cm""）、较小的晶格振动能、较高的辐射发射率及良好的化学稳定性等优点，故引起了研究者的广泛兴趣。目前，稀土掺杂NaYF，已经在生物成像等方面得到了应用(")。三价稀土离子如Er+，Tm+，Ho+等，具有丰富的能级结构和较难的发射谱线，故常被掺杂在各种基质材料中作为发光中心。其中Er+的*Iuc能级与 980nm激光器非常匹配，所以研究的最多。而单离子