LuTaO4:Ln3+(Ln=Eu,Tb)透明薄膜制备改进与其发光性能研究

doi:10.15541/jim20150503

摘要/Abstract

摘要：

LuTaO₄是一种新型的辐射探测材料, 但是制备高质量的透明薄膜面临着巨大挑战。为了在保证薄膜不开裂与高透明度的前提下提高薄膜的厚度, 通过大量摸索选用聚乙烯吡咯烷酮(PVP)为胶黏剂并优化溶胶中固含量及PVP含量成功制备出单层厚度达到100 nm的LuTaO₄:Ln³⁺(Ln=Eu,Tb)薄膜, 保证了薄膜的透明度同时大大提高了发光性能。该方法为高质量LuTaO₄:Ln³⁺(Ln=Eu,Tb)厚膜的制备和应用奠定了基础。

关键词: LuTaO4:Ln3+(Ln=Eu,Tb)薄膜, 溶胶-凝胶法, 固含量, PVP, 发光性能

Abstract:

LuTaO₄ is a kind of novel material for radiation detectors, but using it to prepare high-quality and transparent thin film is of great challenges. In our previous study, high-quality LuTaO₄ thin film was prepared with thickness of single film only about 60 nm, but multilayers film easy to crack. In this study, to ensure no cracking and high transparency of thin film, PVP was chosen as adhesive and single LuTaO₄:Ln³⁺(Ln=Eu,Tb) film of 100 nm was prepared by modulating solid and PVP content through lots of exploration, with improved luminescence properties and high transparency simultaneously. This method lays the foundations for preparation of high-quality applicable LuTaO₄:Ln³⁺(Ln=Eu,Tb) thick film.

Key words: LuTaO4:Ln3+(Ln=Eu,Tb) thin film, Sol-Gel method, solid content, PVP, luminescence properties

中图分类号:

O469

吴霜, 刘波, 邱志澈, 陈士伟, 张娟楠, 刘小林, 顾牡, 黄世明, 倪晨. LuTaO₄:Ln³⁺(Ln=Eu,Tb)透明薄膜制备改进与其发光性能研究[J]. 无机材料学报, 2016, 31(4): 372-376.

WU Shuang, LIU Bo, QIU Zhi-Che, CHEN Shi-Wei, ZHANG Juan-Nan, LIU Xiao-Lin, GU Mu, HUANG Shi-Ming, NI Chen. Improved Preparation Method and Luminescence Properties of LuTaO₄:Ln³⁺(Ln=Eu,Tb) Thin Film[J]. Journal of Inorganic Materials, 2016, 31(4): 372-376.

图/表 8

表1 溶液A中不同固含量的溶胶所制薄膜情况

Table1 Situation of thin film prepared by sol with different solid content in solution A

2-methoxyethanol/mL	HCl/mL	Thin film
25 20 20 16	15 15 8 8	Transparent and crack-free Transparent and crack-free Transparent and crack-free Transparent but crackled
14	8	Opacification and crackled

图1 两种固含量溶胶所制备的双层LuTaO4:Ln3+(Ln=Eu,Tb)薄膜表面形态的SEM及实物照片

Fig. 1 SEM image and real photos of bilayer LuTaO4:Ln3+ (Ln=Eu,Tb) thin films surface morphologies prepared by two sols with different solid contents (a) V2-methoxyethanol = 14 mL, VHCl= 8 mL, LuTaO4:Tb3+; (b) V2-methoxyethanol = 20 mL, VHCl = 8 mL, LuTaO4:Tb3+; (c) V2-methoxyethanol = 14 mL, VHCl= 8 mL, LuTaO4:Eu3+; (d) V2-methoxyethanol = 20 mL, VHCl = 8 mL, LuTaO4:Eu3+

图2 两种固含量溶胶所制备的双层LuTaO4:Ln3+(Ln=Eu (A), Tb(B))薄膜光致发光光谱(激发波长为365 nm)

Fig. 2 Photoluminescence spectra of bilayer LuTaO4:Ln3+ (Ln=Eu(A),Tb(B)) thin films prepared by two sols with different solid contents (λex = 365 nm) (a) V2-methoxyethanol = 14 mL, VHCl= 8 mL; (b) V2-methoxyethanol = 20 mL, VHCl = 8 mL

表2 优化后溶液A的各组份含量

Table 2 Content of each component in solution A after optimization

Lu(NO₃)₃·6H₂O/g	Tb(NO₃)₃·6H₂O/g	Eu₂O₃/g	TaCl₅/g	2-methoxyethanol/mL	HCl/mL
3.2986	0.3541	0.1374	3.0794	20	8

表3 不同PVP含量的溶胶B所制溶胶陈置后情况

Table 3 Situation of sol prepared by solution B with different PVP concentrations

PVP/g	Sol
0.5	Floccule inside
0.4 0.3	Transparent but hyperviscosity Transparent and uniform
0.2	Transparent and uniform

图3 不同PVP含量的两种溶胶所制备的双层LuTaO4:Ln3+ (Ln=Eu,Tb)薄膜剖面SEM照片

Fig. 3 Cross-sectional SEM images of bilayer LuTaO4:Ln3+ (Ln=Eu,Tb) thin films prepared by two sols with different PVP contents (a) mPVP = 0.3 g, LuTaO4:Tb3+; (b) mPVP = 0.2 g, LuTaO4:Tb3+; (c) mPVP = 0.3 g, LuTaO4:Eu3+; (d) mPVP = 0.2 g, LuTaO4:Eu3+

图4 不同PVP含量的两种溶胶所制备的双层LuTaO4: Ln3+(Ln=Eu(A),Tb(B))薄膜光致发光光谱(激发波长为365 nm)

Fig. 4 Photoluminescence spectra of bilayer LuTaO4:Ln3+ (Ln=Eu(A),Tb(B)) thin films prepared by two sols with different PVP contents (λex = 365 nm)

图5 不同PVP含量的两种溶胶所制备的双层LuTaO4:Ln3+ (Ln=Eu,Tb)薄膜透过谱

Fig. 5 Transmission spectra of bilayer LuTaO4:Ln3+(Eu,Tb) thin films prepared by two sols with different PVP contents (a) LuTaO4:Tb3+; (b) LuTaO4:Eu3+

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LuTaO₄:Ln³⁺(Ln=Eu,Tb)透明薄膜制备改进与其发光性能研究

Improved Preparation Method and Luminescence Properties of LuTaO₄:Ln³⁺(Ln=Eu,Tb) Thin Film

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