硅酸盐学报

不同惰性调控离子对钕掺杂氟磷酸锶透明陶瓷微观结构和光谱性能的影响

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张永强 , 梅炳初

硅酸盐学报 | 研究论文 2024,52(3): 899-905

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硅酸盐学报 |研究论文 2024 , 52 (3) : 899 -905

不同惰性调控离子对钕掺杂氟磷酸锶透明陶瓷微观结构和光谱性能的影响

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张永强, 梅炳初

作者信息

武汉理工大学材料，复合新技术国家重点实验室，武汉 430070

通讯作者:

梅炳初（1962—），男，教授。

作者简介:

张永强（1994—），男，博士研究生。

Effect of Buffer Ions on Microstructure and Spectral Properties of Neodymium-Doped Strontium Fluorophosphate Transparent Ceramics

Yongqiang ZHANG, Bingchu MEI

Affiliations

State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070, China

Corresponding Author:

MEI Bingchu (1962-), male, Ph.D., Professor. E-mail: bcmeilab@163.com

ZHANG Yongqiang (1994-), male, Doctoral candidate. E-mail: 1152989914@qq.com

出版时间: 2024-03-20 doi: 10.14062/j.issn.0454-5648.20230524

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采用传统热压烧结法制备了不同惰性调控离子掺杂的Nd：Sr₅（PO₄）₃F（Nd：S-FAP）透明陶瓷，研究了陶瓷相组成对微观结构、光谱性能的影响规律。结果表明：所制备的S-FAP透明陶瓷为纯相，无杂相生成，晶格常数随着掺杂离子与Sr离子半径差异的增大而减小；所制备的样品在1 μm处透过率为70%，在500 nm处为40%；掺入惰性调控离子后，Nd：S-FAP透明陶瓷的发射强度及荧光寿命存在增大的趋势，其中掺入Y离子后调控作用更为有效。通过共掺惰性离子，打破了钕离子在S-FAP基质材料中的团簇现象，提升了钕离子的发光性能。

关键词

钕掺杂氟磷酸锶 / 透明陶瓷 / 微观结构 / 光谱性能

Abstract

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Introduction

The development of laser technology is related to laser materials. In particular, high-power solid-state lasers require the laser material to have the superior performance (i.e., lower pumping thresholds, large absorption and emission cross sections). Compared with glass and single crystal, transparent ceramics have many potential advantages that glass and single crystal are incomparable. In recent years, the breakthrough of ceramic preparation technology has gradually brought ceramics into the field of vision of the majority of scientific researchers. From the perspective of luminescence of doped rare-earth element ions, materials with a low symmetry system have more potential advantages. Strontium fluorophosphate has a hexagonal structure as a typical asymmetric system material. It can provide superior doping sites for rare-earth element ions, having broad potential application prospects in luminescence. Also, neodymium ion (Nd³⁺) is a commonly used active ion, its intense emission wavelength is mainly approximately 1 μm, which is widely used in atmospheric detection and infrared imaging and other fields. However, neodymium ion has a problem of concentration quenching, which will cause the reduction of luminous efficiency. To solve this problem, the commonly used solution is to co-dope inert regulatory ions to break the cluster phenomenon of neodymium ions in the matrix material. Therefore, Nd-doped strontium fluorophosphates transparent ceramics were prepared with S-FAP as a matrix material and Nd³⁺ as an activator ion. In addition, the effect of inert regulatory ions as a sensitizer on the microstructure and spectral properties of Nd:S-FAP was also investigated.

Materials and method

According to the stoichiometric ratio of (Nd_0.015Re_0.02Sr_0.965)₅(PO₄)₃F_1.175, raw materials were weighed and cation was dropped into the anionic solution at a fixed titration rate, and then the suspension was separated in a centrifuge at 11 000 r/min for 4 times. Finally, the separated products were dried in an oven for 24 h. The dried powder was ground in a mortar. The dried powder of 3 g was put into a graphite mold, placed in a vacuum hot press furnace, and sintered at 900 ℃ for 2 h to obtain (Nd, Re):S-FAP transparent ceramics.

The phase composition of the ceramic was analyzed by a model D8-Advance X-ray diffractometer. The Nd³⁺ and Re³⁺ concentrations of (Nd, Re): S-FAP were determined in argon at 0.3 MPa by a model Prodigy 7 inductively coupled plasma emission spectrometer. The transmittance of ceramics was measured by a model Lambda 750S spectrophotometer. The microstructure and pore distribution of ceramics were characterized by a model S4800 scanning electron microscope, and the emission spectrum and fluorescence lifetime of ceramic samples were measured by a model FLS920 spectrometer.

Results and discussion

After doping different kinds of inert regulated ions, each sample has no impurity and a high crystallinity. After high-temperature sintering, the ceramic still maintains a hexagonal structure with a pure phase S-FAP. Moreover, the position of the ceramic emission peak shifts to the right, indicating that the lattice constant gradually decreases The ceramic samples have a good optical transmittance, showing the absorption peaks of the ⁴I_9/2 ground state level transition to the excited state level. For the samples doped with different kinds of inert regulated ions, there are differences in their microstructures. This is because the distortion caused by the doped S-FAP lattice is also different due to the different radii of inert ions. Y ion has the smallest radius and the greater lattice distortion degree. In sintering, the lattice distortion will provide part of the sintering energy, increase the diffusion rate of the grain boundary, eventually resulting in the larger grain size. The main reason affecting the overall transmittance of the sample is a difference in density, and the higher the density of the sample is, the higher the transmittance will be. The emission intensity of transparent ceramics is enhanced after co-doping inert regulated ions. The addition of inert regulated ions breaks the clusters of neodymium ions and increases the distance between different neodymium ions, thereby avoiding the phenomenon of cross relaxation between neodymium ions to a certain extent and thus improving the emission intensity. In addition, the emission peaks of the samples shift to the right to a certain extent after the addition of inert ions, indicating that the crystal field environment of neodymium ions can be changed by co-doped inert ions. The fluorescence lifetimes of ceramic samples doped with different kinds of inert rare-earth ions are 328.44, 331.82 and 355.68 μs, respectively. Compared with 1.5% Nd:S-FAP transparent ceramics, the fluorescence lifetime of ceramic samples doped with inert rare-earth ions increases. The neodymium ion clusters are broken, resulting in an increase in fluorescence intensity/lifetime. In addition, from doping of different kinds of inert rare-earth ions, the fluorescence life of Y ions is the longest after incorporation, reflecting that Y ions are more efficient in breaking clusters in S-FAP matrix materials, and are the most suitable inert regulatory ions for doping.

Conclusions

Inert rare-earth ions doped (Nd, Re):S-FAP transparent ceramics were prepared by a hot pressing sintering method. The lattice constant of rare-earth ion doping decreased, and the main factor affecting the change of lattice constant was rare-earth ion radius. The emission intensity and fluorescence lifetime of ceramic doped inert ions were increased, compared with that of ceramic undoped ions, and the regulation effect of Y ions was dominant. This indicated that the clusters between neodymium ions were broken and the luminous efficiency was improved.

Key words

neodymium doped strontium fluorophosphate / transparent ceramic / microstructures / luminescence property

引用本文

张永强, 梅炳初. 不同惰性调控离子对钕掺杂氟磷酸锶透明陶瓷微观结构和光谱性能的影响. 硅酸盐学报, 2024 , 52 (3) : 899 -905 . DOI: 10.14062/j.issn.0454-5648.20230524

Yongqiang ZHANG, Bingchu MEI. Effect of Buffer Ions on Microstructure and Spectral Properties of Neodymium-Doped Strontium Fluorophosphate Transparent Ceramics[J]. Journal of the Chinese Ceramic Society, 2024 , 52 (3) : 899 -905 . DOI: 10.14062/j.issn.0454-5648.20230524

基金

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国家自然科学基金(51972245)

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2024年第52卷第3期

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doi: 10.14062/j.issn.0454-5648.20230524

接收时间：2023-07-24
首发时间：2026-10-22
出版时间：2024-03-20

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收稿日期：2023-07-24
修回日期：2023-09-16

基金

国家自然科学基金(51972245)

作者信息

武汉理工大学材料，复合新技术国家重点实验室，武汉 430070

通讯作者:

梅炳初（1962—），男，教授。

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https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20230524

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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