Bi1-xEuxPO4纳米荧光粉的制备、晶相调控及发光性能

doi:10.7503/cjcu20131300

摘要/Abstract

摘要：

采用室温共沉淀法合成了一系列六角相荧光材料Bi_1-_xEu_xPO₄(x=0.02, 0.05, 0.07, 0.10). 通过高温烧结和手工研磨分别实现了晶相结构由六角相到高温单斜相再到低温单斜相的调控. 对比了不同相转变过程样品的发光性能, 发现样品Bi_0.95Eu_0.05PO₄在研磨后内量子产率比烧结后样品高5%, 并分析了晶体结构和粒径对发光性能的影响.

关键词: BiPO4, 纳米荧光材料, 室温共沉淀, 寿命, 量子产率

Abstract:

We synthesized a series of hexagonal phase Bi_1-_xEu_xPO₄ by a room-temperature co-precipitation method. The phase structure transformation from hexagonal phase to high temperature monoclinic phase, then to low temperature monoclinic phase was achieved by calcinations and grinding, respectively. Concerning the luminescent properties, the internal quantum yield of the grinded samples for Bi_0.95Eu_0.05PO₄ is 5% higher than that of the calcined samples. These luminescent changes were further discussed in terms of the phase structure and particle size.

Key words: Bismuth phosphate(BiPO4), Nano-phosphor-material, Room-temperature co-precipitation, Lifetime, Quantum yield

中图分类号:

O614
O646

TrendMD:

郑云龙, 赵明磊, 李莉萍, 李广社, 张喜田. Bi_1-_xEu_xPO₄纳米荧光粉的制备、晶相调控及发光性能. 高等学校化学学报, 2014, 35(5): 921.

ZHENG Yunlong, ZHAO Minglei, LI Liping, LI Guangshe, ZHANG Xitian. Preparation, Phase Structure Control and Luminescent Properties of Bi_1-_xEu_xPO₄ Nanophosphors^†. Chem. J. Chinese Universities, 2014, 35(5): 921.

图/表 9

Fig.1 XRD patterns of the Bi1-xPO4∶Eux(x=0.02, 0.05, 0.07, 0.10) samples(A) and crystal structure of hexagonal phase(B)^ (A) a. JCPDS 45-1370; b. x=0.02; c. x=0.05; d. x=0.07; e. x=0.10. (B) PO4 tetrahedra are shown in pink and BiO8 polyhedra in light blue.

Fig.2 XRD patterns of Bi0.98Eu0.02PO4 sample obtained at different calcination temperatures(A) and the crystal structure of HTMP phase(B)^ (A) Temperature/℃: a. 800; b. 900; c. 1000; d. 1100.

Table 1 Phase structures of all samples obtained by calcining the Bi1-xEuxPO4 samples at different temperatures for 10 min

x	Temperature/℃
x	800	900	1000	1100
0.02	HTMP+LTMP	HTMP	HTMP	HTMP
0.05	HTMP+LTMP	HTMP+LTMP	HTMP	HTMP
0.07	HTMP+LTMP	HTMP+LTMP	HTMP+LTMP	HTMP
0.10	HTMP+LTMP	HTMP+LTMP	HTMP+LTMP	HTMP+LTMP

Fig.3 Typical Rietveld structural refinements over the PXRD data of Bi0.98Eu0.02PO4 obtained at different grinding times(A); grinding time dependence of phase contents of LTMP for Bi0.98Eu0.02PO4 and Bi0.95Eu0.05PO4 samples calcined at 1000 ℃(B) and the crystal structure of LTMP phase(C)^(A) Grinding time/min: a. 0; b. 2; c. 30; d. 120; (B) a. Bi0.98Eu0.02PO4; b. Bi0.95Eu0.05PO4.

Table 2 Structural refinement parameters for samples obtained at different grinding times by Rietveld refinement using GSAS program

Time/min	Bi_0.98Eu_0.02PO₄				Bi_0.95Eu_0.05PO₄
Time/min	R_wp	R_p	R_-blnk	χ²	R_wp	R_p	R_-blnk	χ²
0	0.1176	0.0846	0.1004	1.646	0.1232	0.0883	0.1023	1.448
2	0.0981	0.0677	0.0748	1.326	0.1475	0.1063	0.1273	1.634
5	0.1075	0.0769	0.0843	1.420	0.1161	0.0859	0.0966	1.641
30	0.1327	0.0970	0.1127	1.914	0.0906	0.0635	0.0690	1.784
60	0.1186	0.0840	0.0948	1.472	0.1256	0.0905	0.1045	1.571
120	0.1201	0.0864	0.1013	1.575	0.1245	0.0971	0.1194	2.097

Fig.4 SEM images of Bi0.98Eu0.02PO4 samples initially synthesized at room temperature(A), calcined at 1000 ℃(B) and those obtained after grinding for 2 min(C), 5 min(D), 60 min(E) and 120 min(F)

Fig.5 Excitation(A) and emission(B) spectra of Bi0.98Eu0.02PO4 sample synthesized at room temperature(a) and those after calcination at 800 ℃(b), 900 ℃(c) and 1000 ℃(d)^(A) λem=593 nm; (B) λex=394 nm.

Fig.6 Emission spectra of Bi0.98Eu0.02PO4 samples obtained after calcination at 1000 ℃(a) and those obtained after grinding for different times(b―f)^t/min: b. 2; c. 5; d. 30; e. 60; f. 120.

Fig.7 Decay curves of Bi0.98Eu0.02PO4 sample obtained after calcination at 1000 ℃(a) and grinding for 30 min(b)(A) and variation of lifetime and the corresponding internal quantum yield of samples Bi0.98Eu0.02PO4(a, a') and Bi0.95Eu0.05PO4(b, b') with different grinding time(B)

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Bi_1-_xEu_xPO₄纳米荧光粉的制备、晶相调控及发光性能

Preparation, Phase Structure Control and Luminescent Properties of Bi_1-_xEu_xPO₄ Nanophosphors^†

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