稀土氟化物上转换荧光增强及应用

doi:10.7536/PC190330

• •

稀土氟化物上转换荧光增强及应用

程倩, 于佳酩, 霍薪竹, 沈雨萌, 刘守新^**()

东北林业大学材料科学与工程学院哈尔滨 150040

收稿日期:2019-03-25 出版日期:2019-12-15 发布日期:2019-10-15
通讯作者: 刘守新
基金资助:
中央高校基本科研业务费专项资金项目(2572017EB05); 黑龙江省博士后基金项目(LBH-Z14004); 黑龙江省自然科学基金项目(LH2019E002)

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Enhancement Luminescence and Applications of Rare Earth Fluoride

Qian Cheng, Jiaming Yu, Xinzhu Huo, Yumeng Shen, Shouxin Liu^**()

College of Materails Science and Engineering, Northeast Forest University, Harbin 150040, China

Received:2019-03-25 Online:2019-12-15 Published:2019-10-15
Contact: Shouxin Liu
About author:
** E-mail: liushouxin@126.com
Supported by:
Fundamental Research Funds for the Central Universities(2572017EB05); Heilongjiang Province Postdoctoral Science Foundation(LBH-Z14004); Natural Science Foundation of Heilongjiang Province(LH2019E002)

稀土氟化物上转换纳米材料具有化学稳定性高、反斯托克位移大、无光漂白、荧光寿命长、发光谱带窄和穿透深度深等优点,在荧光成像和光热疗、传感器、太阳能电池及防伪技术等领域具有广泛的应用前景,是一种极具发展潜力的荧光材料。然而该类材料在实际应用时还存在有荧光效率低、吸收截面小等亟待解决的瓶颈问题。针对以上问题,本文系统阐述了离子共掺杂、核壳结构、表面等离子耦合、光子晶体、宽频敏化和热效应等增强稀土氟化物上转换荧光的方法及其近年的研究进展。并在此基础上,总结了近年来荧光增强稀土氟化物上转换纳米材料在生物成像和光热疗、生物传感、太阳能电池及防伪技术等领域的应用研究现状。最后,分析了稀土氟化物UCNPs目前仍存在的不足,并对将来的发展方向进行了展望。

关键词： 稀土氟化物, 上转换发光, 荧光增强, 生物应用

Rare earth fluoride upconversion nanomaterials have immense potential applications for biological imaging and photothermal therapy, biosensing, solar cell and anti-counterfeiting technology, due to its high chemical stability, large anti-stokes shifts, no photobleaching, long fluorescence life, narrow emission band and deep penetration, which is a promising fluorescent material. However,such materials are limited in practical application due to their low upconversion luminescence efficiency and small absorption cross-section of activator. Based on the above problems, upconversion luminescence enhancement of rare earth doped fluoride materials such as ion co-doping, core shell structure, surface plasmon coupling, photonic crystal, broadband sensitization and thermal effect are expounded herein, and the mechanisms of enhancement of upconversion luminescence are analyzed. In addition, the research status in the fields of biological imaging and photothermal therapy, biosensing, solar cell and anti-counterfeiting technology is elaborated. Moreover, the limitations and development directions for future are also prospected.

Key words: rare earth fluoride, upconversion luminescence, luminescence enhancment, biological application

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图1 稀土掺杂上转换纳米材料组成示意图

Fig. 1 Schematic diagram of rare earth doped upconversion nanomaterials

图2 不同半径的离子掺杂到基质晶格内引起晶格的变化:晶格收缩(左) 晶格膨胀(右)[1]

Fig. 2 The changes of the doping of a host atom with a dopant of varied size:crystal lattice contraction(left) and expansion(right)[1]

表1 离子诱导上转换发光提高

Table 1 Ion-induced upconversion enhancement

Upconversion materials	Synthesis method	Enhancement factors	ref
NaYF₄: Yb³⁺/Er³⁺/10%Sc³⁺	Hydrothermal	5	21
NaYF₄: Yb³⁺/Er³⁺/1.57%Ti⁴⁺	Hydrothermal	6(521 nm)	22
NaYF₄: Yb³⁺/Er³⁺/15%Cr³⁺	Hydrothermal	16(G), 7(R)	23
LiYF₄: Yb³⁺/Er³⁺/10%Mn²⁺	Thermal decomposition	15(G), 22(R)	24
NaGdF₄: Yb³⁺/Er³⁺/30%Fe³⁺	Hydrothermal	34(G), 30(R)	25
NaYF₄: Yb³⁺/Er³⁺/15%Co²⁺	Thermal decomposition	114(G), 84(R)	26
LiYF₄: Yb³⁺/Er³⁺/10%Cd²⁺	Thermal decomposition	2.2(G)	27
NaYF₄: Yb³⁺/Er³⁺/20%Ni²⁺	Hydrothermal	32.8(G), 20.99(R)	28
NaGdF₄: Yb³⁺/Er³⁺/13.5%Mg²⁺	Solvothermal	9(R), 6(G)	29
KMnF₃: Yb³⁺/Er³⁺/30%Mg²⁺	Solvothermal	20.8(R)	30
NaYF₄: Yb³⁺/Er³⁺/60%Cu²⁺	Hydrothermal	37(G), 25(R)	31
NaYF₄: Yb³⁺/Er³⁺/5%Zn²⁺	Hydrothermal	<2	32
KLaF₄:Yb³⁺/Er³⁺/10%Al³⁺	Hydrothermal	5.9(G), 7.3(R)	33
NaGdF₄: Yb³⁺/Er³⁺/25%Bi³⁺	Hydrothermal	60(802 nm), 160(B)	34

表1 离子诱导上转换发光提高

Table 1 Ion-induced upconversion enhancement

Upconversion materials	Synthesis method	Enhancement factors	ref
NaYF₄: Yb³⁺/Er³⁺/10%Sc³⁺	Hydrothermal	5	21
NaYF₄: Yb³⁺/Er³⁺/1.57%Ti⁴⁺	Hydrothermal	6(521 nm)	22
NaYF₄: Yb³⁺/Er³⁺/15%Cr³⁺	Hydrothermal	16(G), 7(R)	23
LiYF₄: Yb³⁺/Er³⁺/10%Mn²⁺	Thermal decomposition	15(G), 22(R)	24
NaGdF₄: Yb³⁺/Er³⁺/30%Fe³⁺	Hydrothermal	34(G), 30(R)	25
NaYF₄: Yb³⁺/Er³⁺/15%Co²⁺	Thermal decomposition	114(G), 84(R)	26
LiYF₄: Yb³⁺/Er³⁺/10%Cd²⁺	Thermal decomposition	2.2(G)	27
NaYF₄: Yb³⁺/Er³⁺/20%Ni²⁺	Hydrothermal	32.8(G), 20.99(R)	28
NaGdF₄: Yb³⁺/Er³⁺/13.5%Mg²⁺	Solvothermal	9(R), 6(G)	29
KMnF₃: Yb³⁺/Er³⁺/30%Mg²⁺	Solvothermal	20.8(R)	30
NaYF₄: Yb³⁺/Er³⁺/60%Cu²⁺	Hydrothermal	37(G), 25(R)	31
NaYF₄: Yb³⁺/Er³⁺/5%Zn²⁺	Hydrothermal	<2	32
KLaF₄:Yb³⁺/Er³⁺/10%Al³⁺	Hydrothermal	5.9(G), 7.3(R)	33
NaGdF₄: Yb³⁺/Er³⁺/25%Bi³⁺	Hydrothermal	60(802 nm), 160(B)	34

图3 Mn2+掺杂红色上转换荧光光谱图[35]

Fig. 3 Red emission upnconversion fluorescence spectra of Mn2+ doped NaYF4:Yb3+,Er3+[35]

图4 稀土离子掺杂纳米粒子的壳包覆功能[36]

Fig. 4 Basic functions of a shell around Ln3+ doped nanoparticles[36]

图5 活化壳增强上转换纳米晶发光的机理及光谱图。(a)结构示意图;(b)荧光光谱图(插图为钝化壳和活化壳在相同激发密度下的发光对比);(c)增强发光机制[45];(d)活化壳包覆及未包覆纳米晶的荧光光谱图: BaGdF5:Yb3+, Er3+@BaGdF5:x%Yb3+(左);核、核@活化壳、核@活化壳@活化壳(右)[46]

Fig. 5 The mechanism and spectrogram of the upconversion nanocrystals enhanced by activated shell.(a) Schematic diagram. (b)Upconversion luminescence spectra(The insert illustrated the comparison of the luminescence intensity of nanoparticles coated with inert and activated shells under the same excitation density).(c) Mechanism of enhanced luminescence[45].(d) The upconversion emission spectra and phtographs of nanoparticles coated with active shell and uncoated: BaGdF5:Yb3+, Er3+@BaGdF5:x%Yb3+(left), core、core@active shell、core@active shell@active shell(right)[46]

图6 (a) NaYF4:Yb3+,Er3+异质壳包覆上转换发光光谱及量子产率图[47];(b) NaYF4:Yb3+,Er3+@mNaYF4(m=0、1、2、3、4、5)纳米粒子在980 nm激发下的荧光图[49]

Fig. 6 (a) The upconversion luminscence and quantum yield of NaYF4:Yb3+,Er3+ nanoparticles coated with heterogeneous shell[47].(b)Emission spectra of NaYF4:Yb3+,Er3+@mNaYF4(m=0,1,2,3,4,5)nanoparticles by 980 nm excitation[49]

图7 等离子体共振增强上转换发光机制[1]

Fig. 7 Schematic illustration showing the plausible mechamism of enhancement of upconversion luminescence by plasmon resonance[1]

图8 (a) Ag NP-Al2O3-NaYF4:Yb3+,Er3+ UCNPs的上转换荧光光谱,插图为其结构示意图[58];(b)组装成天线复合结构的上转换荧光增强[59];(c) SiO2隔离层厚度对Ag/SiO2/NaYF4:Yb, Er, Gd复合结构的上转换荧光增强[60];(d) 中心场强度 [E/Eo][2]z=d/2,插图为NaGdF4: Yb3+,Er3+在980 nm激发下的Efupc值[61]

Fig. 8 (a) Upconversion luminescence spectra of Ag NP-Al2O3-NaYF4:Yb3+,Er3+ UCNPs,the inset is its schematic structure[58].(b)Luminscence enhancement through use of a disk-coupled dot-on-pillar antenna array(D2PA)[59].(c) PL enhancement factor as a function of SiO2 spacer layer thickness[60].(d) The center field intensity [E/Eo] [2]z=d/2. The inset table is the numerical Efupc of the NaGdF4: Yb3+,Er3+ under 980 nm excitation[61]

表2 核壳机构体系等离子体增强稀土氟化物上转换发光

Table 2 Core-shell system for plasmonic enhancement luminscence of rare earth fluoride

Upconversion materials	Space	Plasmonic material	Enchancement factors	ref
NaYF₄: Yb³⁺/Er³⁺	——	Ag	green/red↑	64
NaYF₄: Yb³⁺/Tm³⁺	——	Au(≈10 nm)	109.0(345 nm)	65
NaYF₄: Yb³⁺/Er³⁺/Gd³⁺	——	Au(sphere)	3.8(540 nm), 4.0(660 nm)	66
NaYF₄:Yb³⁺/Er³⁺/Tm³⁺	——	Au shell(4~8 nm)	8(646 nm)	67
NaYF₄: Yb³⁺/Tm³⁺	PAA^①/PAH	Au	≈2.5(452 nm,476 nm)	68
NaYF₄:Yb³⁺/Er³⁺/Tm³⁺	PAMAM^②	Ag(20 nm) Au(20 nm)	20(413 nm), 22(452 nm) 20(518 nm), 21(540 nm)	69
NaYF₄: Yb³⁺/Tm³⁺	PAMAM	Au rod	27(805 nm), 6(470,550 nm)	70
NaYF₄: Yb³⁺/Er³⁺	SiO₂(10 nm)	Ag(15 nm) Ag(30 nm)	14.4(542 nm), 12.2(656 nm) 9.5(542 nm), 10.8(656 nm)	71
NaGdF₄: Yb³⁺/Er³⁺	SiO₂(8 nm)	Au rod	9(540 nm)	72
NaYF₄:Nd³⁺/Yb³⁺/Ho³⁺	SiO₂(10 nm)	Ag	15(540 nm), 7.5(655 nm)	73
NaGdF₄: Yb³⁺/Er³⁺	NaGdF₄	Ag	2.0(540 nm), 2.51(650 nm)	74
Ag/graphene	SiO₂(10 nm)	NaLuF₄: Yb³⁺/Gd³⁺/Er³⁺	52(520~550 nm)	75
Au rod	SiO₂(19 nm)	CaF₂: Yb³⁺Er³⁺	2.0(540 nm), 2.0(650 nm)	76
Au	SiO₂(28 nm)	NaGdF₄:Yb³⁺,Nd³⁺@NaGdF₄:Yb³⁺,Er³⁺@NaGdF₄	18.9(545 nm), 4.9(660 nm)	77
Ag-Au nanocage	NaYF₄	NaYF₄: Yb³⁺/Er³⁺	25	78

表2 核壳机构体系等离子体增强稀土氟化物上转换发光

Table 2 Core-shell system for plasmonic enhancement luminscence of rare earth fluoride

Upconversion materials	Space	Plasmonic material	Enchancement factors	ref
NaYF₄: Yb³⁺/Er³⁺	——	Ag	green/red↑	64
NaYF₄: Yb³⁺/Tm³⁺	——	Au(≈10 nm)	109.0(345 nm)	65
NaYF₄: Yb³⁺/Er³⁺/Gd³⁺	——	Au(sphere)	3.8(540 nm), 4.0(660 nm)	66
NaYF₄:Yb³⁺/Er³⁺/Tm³⁺	——	Au shell(4~8 nm)	8(646 nm)	67
NaYF₄: Yb³⁺/Tm³⁺	PAA^①/PAH	Au	≈2.5(452 nm,476 nm)	68
NaYF₄:Yb³⁺/Er³⁺/Tm³⁺	PAMAM^②	Ag(20 nm) Au(20 nm)	20(413 nm), 22(452 nm) 20(518 nm), 21(540 nm)	69
NaYF₄: Yb³⁺/Tm³⁺	PAMAM	Au rod	27(805 nm), 6(470,550 nm)	70
NaYF₄: Yb³⁺/Er³⁺	SiO₂(10 nm)	Ag(15 nm) Ag(30 nm)	14.4(542 nm), 12.2(656 nm) 9.5(542 nm), 10.8(656 nm)	71
NaGdF₄: Yb³⁺/Er³⁺	SiO₂(8 nm)	Au rod	9(540 nm)	72
NaYF₄:Nd³⁺/Yb³⁺/Ho³⁺	SiO₂(10 nm)	Ag	15(540 nm), 7.5(655 nm)	73
NaGdF₄: Yb³⁺/Er³⁺	NaGdF₄	Ag	2.0(540 nm), 2.51(650 nm)	74
Ag/graphene	SiO₂(10 nm)	NaLuF₄: Yb³⁺/Gd³⁺/Er³⁺	52(520~550 nm)	75
Au rod	SiO₂(19 nm)	CaF₂: Yb³⁺Er³⁺	2.0(540 nm), 2.0(650 nm)	76
Au	SiO₂(28 nm)	NaGdF₄:Yb³⁺,Nd³⁺@NaGdF₄:Yb³⁺,Er³⁺@NaGdF₄	18.9(545 nm), 4.9(660 nm)	77
Ag-Au nanocage	NaYF₄	NaYF₄: Yb³⁺/Er³⁺	25	78

图9 (a) PMMA OPCs/NaYF4:Yb3+,Tm3+ UCNP化合物形成示意图;(b) NaYF4:Yb3+,Tm3+ UCNP和PMMA OPCs/NaYF4:Yb3+,Tm3+化合物的荧光光谱比较,插图为NaYF4:Yb3+,Tm3+的能级转换过程图;(c)上转换荧光增强随PMMA OPCs的PSB的关系[81]

Fig. 9 (a)The schematic of the formation of PMMA OPCs/NaYF4:Yb3+,Tm3+ UCNP composites.(b)A comparision of UCL spectra of NaYF4:Yb3+,Tm3+ UCNP and PMMA OPCs/NaYF4:Yb3+,Tm3+ composites. Inset:UC population and emission process of NaYF4:Yb3+,Tm3+.(c) Dependence of the UC enhancement factor as a funciton of PSB of PMMA OPCs[81]

图10 染料敏化上转换发光的结构示意图(a)核(S:敏化剂,A:激活剂);(b)核壳结构(S1∶1类敏化剂,S2∶2类敏化剂,A:激活剂);红色实线、红色虚线,蓝色实线,蓝色虚线及绿色箭头分别代表激发、能量转移、上转换路径和荧光过程[93]

Fig. 10 Schematic illustrations of dye sensitized upconversion in(a) Core(S: sensitizer, A: activator).(b)The core-shell structure(S1: type 1 sensitizer, S2:type 2 sensitizer, A: activator). The red solid line, red dashed line, blue solid line, blue dashed line and green arrows represent the excitation, energy transfer, upconversion pathway and fluorescence process[93]

图11 (a)IR-806敏化β-NaYF4: Yb3+/Er3+纳米晶的结构示意图;(b)样品的荧光光谱图,β-NaYF4: Yb3+/Er3+纳米颗粒(青色线)、IR-806(绿色线)、IR-780/β-NaYF4: Yb3+/Er3+ 纳米颗粒(红色线)、 IR-806/β-NaYF4: Yb3+/Er3+纳米颗粒(蓝色线)[94]

Fig. 11 (a) A schematic illustrations of IR-806 sensitized β-NaYF4: Yb3+/Er3+nanoparticles.(b) Luminescence spectra of β-NaYF4: Yb3+/Er3+nanoparticles(cyan line),IR-806(green line), IR-780/β-NaYF4: Yb3+/Er3+ nanoparticles(red line), IR-806/β-NaYF4: Yb3+/Er3+nanoparticles(blue line)[94]

图12 染料敏化纳米晶实现可调的激发光谱示意图(a)β-NaYF4: Yb3+/Er3+[96];(b)β-NaYF4: Yb3+/Tm3+[97];(c)三种敏化剂结构转移示意图;(d)NaY0.48Gd0.3Yb0.2Er0.02F4 IR806-UCNP 在染料激发下的上转换荧光强度随激发能量的关系图。误差棒代表平均值的标准偏差。插图为染料或者直接激发的发射光谱[98]

Fig. 12 Schematic illustration of dye-sensitized nanoparticles with tunable excitation wavelength(a) β-NaYF4: Yb3+/Er3+[96].(b) β-NaYF4:Yb3+/Tm3+[97].(c)Energy diagram of three sensiticers.(d)Excitation power dependence of upconverted emission from NaY0.48Gd0.3Yb0.2Er0.02F4 IR806-UCNP under excitation of the dye(808 nm excitation) or UCNP(980 nm excitation). Error bars represent one standard deviation from the mean. Inset, emission spectra for dye or direct excitation[98]

图13 表面光子提高上转换发光的过程示意图[102]

Fig. 13 Schematic illustration of the surface-photon-enhanced upconversion process[102]

图14 (a)基于DNA的NR二聚体与上转换纳米材料组装成卫星状纳米结构,并用于多模态成像引导联合光治疗的示意图;(b) PBS、NR-UCNP-Ce6及NR-二聚体-UCNP-Ce6的光热效应;(c) PBS、UCNP-Ce6、NR、NR dimer、NR-UCNP-Ce6及NR-二聚体-UCNP-Ce6在接种海拉肿瘤细胞的裸鼠体内热成像效果对比图[109]

Fig. 14 (a)Schematic illustration of DNA-based NR dimer and UCNP core-satellite assembly for multimodal imaging guided combination phototherapy.(b) Photothermal effect of assemblies of PBS、NR-UCNP-Ce6 and NR-dimer-UCNP-Ce6.(c)Thermal images of HeLa tumor-bearing mice with PBS、UCNP-Ce6、NR、NR dimer、NR-UCNP-Ce6 and NR-dimer-UCNP-Ce6[109]

图15 (a) 三明治结构的纳米晶及FRET检测Cu2+[111];(b)用生物酰化的上转换纳米晶为供体,FITC为受体利用 FRET 探测抗生素蛋白[83];(c)用宽带近红外光和光谱转换为可见范围激活N719染料改进DSSC装置;(d) AM1.5 G模拟阳光辐照(100 mW·cm -2)下DSSC、DSSC-UCNPs、DSSC-DSUCNPs电流密度-电压(J-V)特性[115]

Fig. 15 (a) Schematic illustration of the sandwich structured UCNPs and the principle of FRET based UC probe for Cu2+ detection[111].(b) FRET detection of avidin by employing biotinylated NCs as the donor and FITC as an acceptor[83].(c)Broadband near-infrared sunlight harvesting and then spectral conversion into visible range to activate N719 dye for the improvement of DSSC device.(d) The current density-voltage(J-V) characteristics of DSSC, DSSC-UCNPs and DSSC-DSUCNPs under AM 1.5 G simulated sunlight irradiation(100 mW·cm-2)[115]

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