构建NaYF4:Yb3+/Ho3+/Ce3+@NaYF4:Yb3+/Nd3+纳米核壳结构增强Ho3+离子的上转换红光发射

董军; 张晨雪; 程小同; 邢宇; 韩庆艳; 严学文; 祁建霞; 刘继红; 杨祎; 高伟

doi:10.7498/aps.70.20210118

摘要

三阶Ho³⁺离子的红光发射位于生物组织的“光学窗口”中, 在生物医学领域具有巨大应用前景, 增强其红光发射已成为大家关注热点. 为此, 本文借助外延生长技术构建NaYF₄:Yb³⁺/Ho³⁺/Ce³⁺@NaYF₄纳米核壳结构, 并在其外壳中引入不同浓度的敏化离子Yb³⁺和Nd³⁺离子, 以构建新的能量传递通道, 实现Ho³⁺离子的上转换红光发射增强. 实验结果表明: 在近红外光980 nm 及800 nm激发下, NaYF₄:Yb³⁺/Ho³⁺/Ce³⁺@NaYF₄:Yb³⁺ 和NaYF₄:Yb³⁺/Ho³⁺/Ce³⁺@NaYF₄:Yb³⁺/Nd³⁺核壳纳米结构均可实现Ho³⁺离子的红光发射增强, 最高可增强6.1倍, 主要是由于外壳中的敏化离子可传递更多的激发能给Ho³⁺离子. 同时, 研究发现在双波长(980 nm +800 nm)共激发下, NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:15%Yb³⁺/20%Nd³⁺核壳纳米晶体的红光发射强度明显高于两个单一波长激发下的红光发射强度及其之和, 其原因是由双波长共激发的协同效应所致. 由此可见, 通过引入不同敏化离子构建多模式激发的稀土掺杂纳米核壳结构, 不仅可实现上转换红光发射的增强及激发的有效调控, 且可为进一步拓展该类材料在生物医学、防伪编码、多色显示等领域中的应用提供新思路.

关键词:

Abstract

The red upconversion (UC) emission of Ho³⁺ ions is located in an “optical window” range of the biological tissue, which has great prospects in the biology application. In this work, the NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:x%Yb³⁺ and NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:15%Yb³⁺/x%Nd³⁺ core-shell (CS) nanoparticles (NPs) are built based on the epitaxial growth technology by the high-temperature co-precipitation method in order to enhance red UC emission. The crystal structure and morphology of NaYF₄ CS NPs are characterized by X-ray diffraction and transmission electron microscope. It can be found that the morphology of NaYF₄ CS NPs changes from sphere into rod shape when coated with NaYF₄ shell, and has a pure hexagonal-phase crystal structure. Under 980 nm excitation, the red UC emission intensity of NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:5%Yb³⁺ CS NPs is strongest and enhanced about 5.2 times than that of NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺ NPs. Under 800 nm excitation, the red emission intensity of NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:15%Yb³⁺/20%Nd³⁺ CS NPs is increased about 6.1 times compared with that of the NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:15%Yb³⁺/5%Nd³⁺ CS NPs. This is because the constructed CS effectively reduces the non-radiative decay from the surface defects of NPs, and the doped Yb³⁺ and Nd³⁺ ions in the NaYF₄ shells can transfer more excitation energy to Ho³⁺ ions in the core. In addition, the NaYF₄: 20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:15%Yb³⁺/20%Nd³⁺ CS NP is excited by dual-wavelengths co-excitation (800 nm + 980 nm). It is found that the red UC emission intensity under the co-excitation of dual-wavelengths is higher than the sum of the excitation intensities of two single wavelengths (800 nm and 980 nm), which is due to the synergistic effect generated under the co-excitation of 980 nm and 800 nm near infrared laser. Therefore, different CS structures constructed by introducing different energy transfer channels can achieve the enhancement of the red UC emission under different excitation conditions, and the dual-wavelength co-excitation provides a new way to improve the penetration depth and the detection sensitivity for further expanding the applications in the field of biomedicine.

Keywords:

作者及机构信息

西安邮电大学电子工程学院, 西安　710121

通信作者: 高伟, gaowei@xupt.edu.cn

基金项目: 陕西省国际交流项目(批准号: 2019KW-027)、陕西省自然科学基金(批准号: 2019JQ-864)、陕西省重点研发项目(批准号: 2020GY-101, 2020GY-127)、西安市科技创新人才企业项目(批准号: 2020KJRC0107, 2020KJRC0112)和西安邮电大学联合示范工作站项目(批准号: YJGJ201905)资助的课题

Authors and contacts

School of Electronic Engineering, Xi’an University of Post & Telecommunications, Xi’an 710121, China

Corresponding author: Gao Wei, gaowei@xupt.edu.cn

Funds: Project support by the Shaanxi Province International Cooperation and Exchange Program, China (Grant No. 2019KW-027), the Natural Science Basic Research Plan in Shaanxi Province of China (Grant No. 2019JQ-864), the Key R&D program of Shaanxi Province, China (Grant Nos. 2020GY-101, 2020GY-127), the Xi’an Science and Technology Innovation Talent Service Enterprise Project, China (Grant Nos. 2020KJRC0107, 2020KJRC0112), and the Funded by Xi’an University of Posts and Telecommunications Joint Postgraduate Cultivation Workstation, China (Grant No. YJGJ201905)

文章全文 : translate this paragraph

补充材料

154208-20210118补充材料.pdf

参考文献

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施引文献

图 1 NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺纳米晶体及相应核壳纳米晶体的XRD图

Fig. 1. The XRD patterns of NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺ nanoparticles (NPs) and core-shell (CS) structures.

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图 2 (a) NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺纳米晶体、(b) NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@ NaYF₄核壳纳米晶体、(c) NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@ NaYF₄:15%Yb³⁺ 核壳纳米晶体和(d) NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺ @NaYF₄:15% Yb³⁺/10%Nd³⁺核壳纳米晶体的TEM图, 插图分别为相应的粒径尺寸分布图

Fig. 2. The TEM images and size distribution of the (a) NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺ NPs, (b) NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄ CS NPs, (c) NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:15%Yb³⁺ CS NPs, and (d) NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺ @NaYF₄:15%Yb³⁺/10%Nd³⁺ CS NPs.

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图 3 在近红外光980 nm激发下, NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺纳米晶体和NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:x %Yb³⁺ (x = 0, 5, 10, 15)核壳纳米晶体的(a)上转换发射光谱、(b)增强因子和(c)红绿比图

Fig. 3. (a) Upconversion (UC) emission spectra, (b) enhancement factor and (c) R/G ratio of NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺ NPs and NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:x %Yb³⁺ (x = 0, 5, 10, 15) CS NPs under the excitation of a 980 nm NIR laser.

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图 4 在近红外光800 nm激发下, NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:15%Yb³⁺/x %Nd³⁺ (x = 5, 10, 15, 20, 30, 40)核壳纳米晶体的(a)上转换发射光谱、(b)增强因子和(c)红绿比图

Fig. 4. (a) The UC emission spectra, (b) enhancement factor and (c) R/G ratio of NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:15%Yb³⁺/x %Nd³⁺ (x = 5, 10, 15, 20, 30, 40) CS NPs under the excitation of an 800 nm NIR laser.

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图 5 (a) 在980 nm近红外光激发下, NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:5%Yb³⁺核壳纳米晶体和(c)在800 nm近红外光激发下, NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:15%Yb³⁺/20%Nd³⁺核壳纳米晶体的上转换发射光谱, 插图分别为其随激发功率变化的红绿比图; (b)和(d)为对应的发光强度与激发功率间的依赖关系

Fig. 5. (a) and (c) The UC emission spectra and corresponding R/G ratio, (b) and (d) UC emission intensity versus excitation power of NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:5%Yb³⁺ CS NPs with 980 nm excitation power increasing from 40 mW to 100 mW (a), (b) and NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:15%Yb³⁺/20%Nd³⁺ CS NPs with 800 nm excitation power increasing from 70 mW to 130 mW (c), (d).

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图 6 Nd³⁺, Yb³⁺, Ho³⁺ 和 Ce³⁺离子的能级图和可能的上转换跃迁机理

Fig. 6. Energy level diagrams of Nd³⁺, Yb³⁺, Ho³⁺ and Ce³⁺ ions as well as proposed UC mechanisms.

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图 7 在980 nm近红外光激发下, NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺纳米晶体和NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:x %Yb³⁺ (x = 0, 5, 10, 15) 核壳纳米晶体的上转换红光发射的寿命衰减曲线

Fig. 7. Luminescence lifetimes of NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺NPs and NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:x %Yb³⁺ (x = 0, 5, 10, 15) CS NPs under 980 nm excitation at 642 nm.

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图 8 分别在980 nm激发下、800 nm激发下、980 nm和800 nm共同激发下NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:15%Yb³⁺/20%Nd³⁺核壳纳米晶体的(a)上转换发射光谱和(b)红绿比图

Fig. 8. (a) The UC emission spectra and (b) R/G ratio of NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:15%Yb³⁺/20%Nd³⁺CS NPs under 980 nm, 800 nm and simultaneous 980 nm + 800 nm excitation.

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图 9 NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:15%Yb³⁺/20%Nd³⁺核壳纳米晶体在(a) 不同980 nm激光功率下, 固定800 nm激光功率为120 mW时和(d) 不同800 nm激光功率下, 固定980 nm激光功率为120 mW时的上转换发射光谱; (b) 和 (e)为其对应的随不同波长激发功率变化的增强因子图; (c) 和 (f) 为其对应的随不同波长激发功率变化的红绿比图

Fig. 9. (a), (d) The UC emission spectra, (b), (e) enhancement factor and (c), (f) R/G ratio of NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:15%Yb³⁺/20%Nd³⁺CS NPs on the excitation power of 980 nm with the power of 800 nm laser fixed at 120 mW ((a)–(c)) and NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:15%Yb³⁺/20%Nd³⁺CS NPs on the excitation power of 800 nm with the power of 980 nm laser fixed at 120 mW ((d)–(f)).

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表 1 NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺纳米晶体和NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:x %Yb³⁺核壳纳米晶体的上转换红光发射的荧光寿命

Table 1. Luminescence lifetimes of NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺ NPs and NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:x %Yb³⁺ (x = 0, 5, 10, 15) CS NPs under 980 nm excitation at 642 nm.

Samples	Lifetime/μs
a: NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺	208.7 ± 4.7
b: NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄	555.4 ± 4.1
c: NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:5%Yb³⁺	667.6 ± 5.7
d: NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:10%Yb³⁺	499.8 ± 1.7
e: NaYF₄:20%Yb³⁺/2%Ho³⁺/12%Ce³⁺@NaYF₄:15%Yb³⁺	321.8 ± 1.3

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map

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构建NaYF₄:Yb³⁺/Ho³⁺/Ce³⁺@NaYF₄:Yb³⁺/Nd³⁺纳米核壳结构增强Ho³⁺离子的上转换红光发射

Enhancing red upconversion emission of Ho³⁺ ions through constructing NaYF₄:Yb³⁺/Ho³⁺/Ce³⁺@NaYF₄:Yb³⁺/Nd³⁺ core-shell structures

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西安邮电大学电子工程学院, 西安　710121

通信作者: 高伟, gaowei@xupt.edu.cn

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School of Electronic Engineering, Xi’an University of Post & Telecommunications, Xi’an 710121, China

Corresponding author: Gao Wei, gaowei@xupt.edu.cn

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