Pr-ZrSiO4颜料(镨锆黄)的两步法合成与表征

doi:10.3724/SP.J.1077.2012.11677

无机材料学报 ›› 2012, Vol. 27 ›› Issue (9): 984-990.DOI: 10.3724/SP.J.1077.2012.11677 CSTR: 32189.14.SP.J.1077.2012.11677

Pr-ZrSiO₄颜料(镨锆黄)的两步法合成与表征

曹坤武^1,2, 郭旭虹², 高彦峰¹, 罗宏杰¹

(1. 中国科学院上海硅酸盐研究所, 上海200050; 2. 华东理工大学化学工程联合国家重点实验室, 上海200237)

收稿日期:2011-10-29 修回日期:2012-02-29 出版日期:2012-09-20 网络出版日期:2012-08-28
作者简介:曹坤武(1987-), 男, 硕士研究生.
基金资助:
国家自然科学基金(51172265); 上海市纳米专项基金(1052nm02100)

Synthesis and Characterization of Pr-ZrSiO₄ Pigment by a Two-step Method

CAO Kun-Wu^1,2, GUO Xu-Hong², GAO Yan-Feng¹, LUO Hong-Jie¹

(1. Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China; 2. State-Key Laboratory of Chemical Engineering, East China University of Science and Technology, Shanghai 200237, China)

Received:2011-10-29 Revised:2012-02-29 Published:2012-09-20 Online:2012-08-28
About author:CAO Kun-Wu.
Supported by:
National Natural Science Foundation of China(51172265); Shanghai Nano Science and Technology Special Project (1052nm02100)

摘要/Abstract

摘要： 以ZrOCl₂•8H₂O、Na₂SiO₃•9H₂O及Pr₆O₁₁为原料, 采用水热合成加高温热处理两步法制备得到纳米级镨锆黄颜料. 用XRD、TEM、SEM、反射光谱、L*a*b*参数等测试方法表征了样品晶体结构、形貌、颜色以及反射光谱参数. 研究结果表明: 水热体系溶液的pH值、水热温度、热处理温度是影响产物晶体结构及颜料性能的主要因素. 综合考虑颜料的晶型、光谱差值、粒径大小、均匀性以及分散性, 当反应条件为水热温度220℃, 水热体系溶液的pH值为3.5, 热处理温度为900℃条件下所得样品的颜料性能较佳.

关键词: 硅酸锆, 镨锆黄, 纳米颜料, 水热, 热处理

Abstract: Nanoscale praseodymium-doped zircon yellowish pigment was prepared by a two-step new method using ZrOCl₂•8H₂O, Na₂SiO₃•9H₂O and Pr₆O₁₁ as raw materials. Intermediate nanopowders were hydrothermally synthesized firstly, then these intermediate powders were calcined at high temperatures to produce nanoscale Pr-zircon yellowish pigment. The products were characterized by XRD, TEM, SEM, reflectance spectra and the CIE L*a*b* parameters. The pH of hydrothermal solution, the hydrothermal temperature and the heat treatment temperature are main factors that influenced the quality of pigment. Low pH is favorable for decreasing the calcination temperatures and producing the pigment with good dispersion and homogeneous sizes. The product with best pigment performance is obtained at the reaction conditions as follows, pH=3.5 of hydrothermal solution, hydrothermal temperature of 220℃ and heat treatment temperature of 900℃.

Key words: zircon, yellow, nano-pigments, hydrothermal, post-heat treatment

中图分类号:

TQ174

曹坤武, 郭旭虹, 高彦峰, 罗宏杰. Pr-ZrSiO₄颜料(镨锆黄)的两步法合成与表征[J]. 无机材料学报, 2012, 27(9): 984-990.

CAO Kun-Wu, GUO Xu-Hong, GAO Yan-Feng, LUO Hong-Jie. Synthesis and Characterization of Pr-ZrSiO₄ Pigment by a Two-step Method[J]. Journal of Inorganic Materials, 2012, 27(9): 984-990.

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Pr-ZrSiO₄颜料(镨锆黄)的两步法合成与表征

Synthesis and Characterization of Pr-ZrSiO₄ Pigment by a Two-step Method

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