镨掺杂钛酸钙/云母钛荧光效果珠光颜料的制备及其性能研究

doi:10.15541/jim20140149

无机材料学报 ›› 2014, Vol. 29 ›› Issue (12): 1275-1280.DOI: 10.15541/jim20140149

镨掺杂钛酸钙/云母钛荧光效果珠光颜料的制备及其性能研究

周为明^1,3, 陈庆华^{2, 3}, 柯梅珍¹, 吴楠², 罗永晋^{2, 3}, 张华集¹, 钱庆荣^{2, 3}

(1. 福建师范大学材料科学与工程学院, 福州 350007; 2. 福建师范大学环境科学与工程学院, 福州 350007; 3. 福建省污染控制与资源循环利用重点实验室, 福州 350007)

收稿日期:2014-03-26 修回日期:2014-05-22 出版日期:2014-12-20 网络出版日期:2014-11-20
作者简介:周为明(1988–), 男, 硕士研究生. E-mail: zhouweiming721@126.com
基金资助:
福建省科技厅高校产学研重大项目(2011H6005,2013H6007);福建科技厅重点项目(2012H0018, 2013H0017);福建省自然科学基金(2011J01287)

Preparation and Properties of CaTiO₃:Pr³⁺/TiO₂-mica Fluorescent Pearlescent Pigments

ZHOU Wei-Ming^1,3, CHEN Qing-Hua^{2, 3}, KE Mei-Zhen¹, WU Nan², LUO Yong-Jin^{2, 3}, ZHANG Hua-Ji¹, QIAN Qing-Rong^{2, 3}

(1. College of Materials Science and Engineering, Fujian Normal University, Fuzhou 350007, China; 2. College of Environmental Science and Engineering, Fujian Normal University, Fuzhou 350007, China; 3. Fujian Key Laboratory of Pollution Control & Resource Reuse, Fuzhou 350007, China)

Received:2014-03-26 Revised:2014-05-22 Published:2014-12-20 Online:2014-11-20
About author:ZHOU Wei-Ming. E-mail: zhouweiming721@126.com
Supported by:
Fujian Key Project of Industry-University-Research Collaboration (2011H6005, 2013H6007);Key Project of Fujian Science and Technology Agency (2012H0018, 2013H0017);Natural Science Fund of Fujian Province (2011J01287)

摘要/Abstract

摘要：

采用液相沉积法在云母基材表面双层包覆二氧化钛和镨掺杂氢氧化钙, 经高温煅烧在两层之间生成镨掺杂钛酸钙(CaTiO₃:Pr³⁺)荧光层。通过荧光分光光度计、全自动色差计、X射线粉末衍射仪和冷场扫描电子显微镜测试样品的性能。结果表明, 当氧化钙理论包覆率为5.3%、镨浓度相对硝酸钙为0.2mol%、煅烧温度为900℃时, 样品表面均匀、致密, 具有较好的珠光性能和荧光强度, 样品的激发光谱由264、304和380 nm三个激发峰组成, 最大发射波长主峰位于613 nm, 呈红光发射, 对应于Pr³⁺的¹D₂→³H₄跃迁。

关键词: 荧光, 珠光颜料, CaTiO3:Pr3+

Abstract:

Double-layer of titanium dioxide and Pr-doped calcium hydroxide were coated on the surface of mica by liquid phase deposition, and followed by calcination to form the Pr-doped calcium titanates fluorescent layer. The resultant CaTiO₃:Pr³⁺/TiO₂-mica fluorescent pearlescent pigments were characterized by photoluminescence excitation (PLE) and emission (PL), automatic colorimeter (AC), X-ray diffraction (XRD) and field emission scanning electron microscopy (FE-SEM), respectively. The fluorescent pearlescent pigments obtained at the calcium oxide cladding ratios of 5.3%, the praseodymium/calcium nitrate molar concentration of 0.2%, and the calcinations temperature of 900 ℃, show good pearl property with homogeneous, dense and smooth surface, and relatively high fluorescence intensity. The excitation spectrum of these fluorescent pearlescent pigments consists of three bands at 264, 304 and 380 nm. The maximum emission wavelength is found to be a red light of 613 nm, corresponding to the transition for ¹D₂→³H₄.

Key words: fluorescent, pearlescent pigments, CaTiO3:Pr3+

中图分类号:

TQ626

周为明, 陈庆华, 柯梅珍, 吴楠, 罗永晋, 张华集, 钱庆荣. 镨掺杂钛酸钙/云母钛荧光效果珠光颜料的制备及其性能研究[J]. 无机材料学报, 2014, 29(12): 1275-1280.

ZHOU Wei-Ming, CHEN Qing-Hua, KE Mei-Zhen, WU Nan, LUO Yong-Jin, ZHANG Hua-Ji, QIAN Qing-Rong. Preparation and Properties of CaTiO₃:Pr³⁺/TiO₂-mica Fluorescent Pearlescent Pigments[J]. Journal of Inorganic Materials, 2014, 29(12): 1275-1280.

图/表 8

图1 不同理论包覆率样品的发射光谱及其相对荧光强度(插图)

Fig. 1 PL spectra and relative fluorescence intensity of samples with various cladding ratios (inset)

图2 不同理论包覆率样品的明度和饱和度

Fig. 2 The brightness and degree of saturation of samples with various cladding ratio

图3 不同煅烧温度样品的XRD图谱

Fig. 3 XRD patterns of samples calcined at various temperatures

图4 不同煅烧温度所制样品的发射光谱和相对荧光强度 (插图)

Fig. 4 PL spectra and relative fluorescence intensity (inset) of samples calcined at various temperatures

图5 不同镨浓度样品的激发光谱(a)和发射光谱(b)

Fig. 5 PLE (a) and PL (b) spectra of samples with various praseodymium molar concentrations of calcium nitrate

图6 荧光效果珠光颜料SEM照片

Fig. 6 SEM images of fluorescent pearlescent pigments (a) mica, (b) TiO2-mica pearlescent pigments, (c) fluorescent pearlescent pigments, (d) fracture surface of fluorescent pearlescent pigments

图7 云母钛珠光颜料和样品的激光粒径分布图

Fig. 7 Laser particle size distribution of TiO2-mica pearlescent pigments and sample

图8 样品在自然光(a)和254 nm紫外光(b)下的照片

Fig. 8 Images of samples under bright light (a) and 254 nm UV (b)

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镨掺杂钛酸钙/云母钛荧光效果珠光颜料的制备及其性能研究

Preparation and Properties of CaTiO₃:Pr³⁺/TiO₂-mica Fluorescent Pearlescent Pigments

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镨掺杂钛酸钙/云母钛荧光效果珠光颜料的制备及其性能研究

Preparation and Properties of CaTiO3:Pr3+/TiO2-mica Fluorescent Pearlescent Pigments

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Preparation and Properties of CaTiO₃:Pr³⁺/TiO₂-mica Fluorescent Pearlescent Pigments