水热法制备(NH4)xWO3-y和WO3·1/3H2O: 反应温度对产物物相、微结构和光学性能的影响

doi:10.3724/SP.J.1077.2014.14026

无机材料学报 ›› 2014, Vol. 29 ›› Issue (5): 550-556.DOI: 10.3724/SP.J.1077.2014.14026

水热法制备(NH₄)_xWO_3-y和WO₃·1/3H₂O: 反应温度对产物物相、微结构和光学性能的影响

王琨¹, 康利涛¹, 陈石², 董丽¹, 梁伟¹, 高峰^1,3

(1. 太原理工大学材料科学与工程学院, 无机纳米能源实验室, 太原030024; 2. 中国科学院上海硅酸盐研究所, 上海200050; 3. 中国科学院煤炭化学研究所, 煤转化国家重点实验室, 太原030024)

收稿日期:2014-01-10 修回日期:2014-02-26 出版日期:2014-05-20 网络出版日期:2014-04-24
作者简介:王琨. E-mail: 815569005@qq.com
基金资助:
Postdoctoral Science Foundation of China (2012M520605); Research Foundation of Taiyuan University of Technology (tyut-rc201369a, 2013Z040); Open Foundation of State Key Laboratory of Coal Conversion (09-102); Natural Science Foundation of Shanxi Province (2013011042-1)

Effects of Reaction Temperature on Structure and Optical Properties of Hydrothermally Prepared (NH₄)_xWO_3-y and WO₃·1/3H₂O

WANG Kun¹, KANG Li-Tao¹, CHEN Shi², DONG Li¹, LIANG Wei¹, GAO Feng^1,3

(1. Nano-Energy Inorganic Materials Laboratory, College of Materials Science and Engineering, Taiyuan University of Technology, Taiyuan 030024, China; 2. Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China; 3. State Key Laboratory of Coal Conversion, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030024, China)

Received:2014-01-10 Revised:2014-02-26 Published:2014-05-20 Online:2014-04-24
About author:WANG Kun(1989-), female, candidate of master degree. E-mail: 815569005@qq.com
Supported by:
Postdoctoral Science Foundation of China (2012M520605); Research Foundation of Taiyuan University of Technology (tyut-rc201369a, 2013Z040); Open Foundation of State Key Laboratory of Coal Conversion (09-102); Natural Science Foundation of Shanxi Province (2013011042-1)

摘要/Abstract

摘要： 本工作研究了水热法制备钨系氧化物过程中反应温度对产物物相、微结构和光学性能的影响。XRD结果表明100 ℃条件下制备的样品为纳米六方相铵钨青铜 (NH₄)_xWO_3-y。随着水热温度升高(140和180 ℃), 部分六方相(NH₄)_xWO_3-y逐步转变为正交相三氧化钨WO₃·1/3H₂O, 形成两相共存产物。SEM和TEM分析证实(NH₄)_xWO_3-y和WO₃·1/3H₂O粒子均为沿[001]方向(c轴)生长的短棒状单晶, 随水热反应进行它们会通过取向融并(oriented attachment)方式进一步长大。结构分析同时证实, 棒状晶的物相与其尺寸存在明显联系, 纳米尺寸的棒状晶为六方(NH₄)_xWO_3-y相, 而微米尺寸的棒状晶为正交WO₃·1/3H₂O相。依据实验结果, 提出了一种表面能控制的六方相(NH₄)_xWO_3-y向正交相WO₃·1/3H₂O相转变机理。光学性能测量表明, 100℃制备的六方相(NH₄)_xWO_3-y样品可以很好的遮蔽近红外光(遮蔽率: 74.5%), 同时保持高可见光透过率(67.6 %)。

关键词: (NH₄)_xWO_3-y, WO_3-x·1/3H₂O, 反应温度, 近红外光遮蔽性能

Abstract: Effects of reaction temperature on phase, microstructure and optical property of hydrothermally prepared (NH₄)_xWO_3-y and WO₃·1/3H₂O were studied in this work. XRD results show that the sample prepared at 100℃ is hexagonal (NH₄)_xWO_3-_y (h-(NH₄)_xWO_3-y). At higher reaction temperatures of 140℃ and 180℃, the hexagonal (NH₄)_xWO_3-y gradually and partially transforms into orthorhombic WO₃·1/3H₂O (o-WO3·1/3H2O). SEM and TEM images illustrate that both (NH₄)_xWO_3-y and WO₃·1/3H₂O crystallites show a short-rod shape with a [001] growth direction (c axis). The phases of crystallites seem to be strongly related to crystallite sizes; nano- and micro-sized crystallites adopt h-(NH₄)_xWO_3-y and o-WO₃·1/3H₂O, respectively. Based on XRD, SEM and TEM results, a mechanism is extracted to explain the transformation from h-(NH₄)_xWO_3-y to o-WO₃·1/3H₂O. Optical measurements indicate that the h-(NH₄)_xWO_3-y nano-rods prepared at 100℃ exhibit a low infrared light transmittance of 25.5%, and maintaining a high luminous transmittance (67.6%), mainly due to the fice crystallite sizes.

Key words: (NH₄)_xWO_3-y, WO₃·1/3H₂O, reaction temperature, NIR shielding ability

中图分类号:

TB321

王琨, 康利涛, 陈石, 董丽, 梁伟, 高峰. 水热法制备(NH₄)_xWO_3-y和WO₃·1/3H₂O: 反应温度对产物物相、微结构和光学性能的影响[J]. 无机材料学报, 2014, 29(5): 550-556.

WANG Kun, KANG Li-Tao, CHEN Shi, DONG Li, LIANG Wei, GAO Feng. Effects of Reaction Temperature on Structure and Optical Properties of Hydrothermally Prepared (NH₄)_xWO_3-y and WO₃·1/3H₂O[J]. Journal of Inorganic Materials, 2014, 29(5): 550-556.

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水热法制备(NH₄)_xWO_3-y和WO₃·1/3H₂O: 反应温度对产物物相、微结构和光学性能的影响

Effects of Reaction Temperature on Structure and Optical Properties of Hydrothermally Prepared (NH₄)_xWO_3-y and WO₃·1/3H₂O

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