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无机材料学报

无机材料学报

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乙二醇甲醚体系中α-Fe2O3纳米晶制备与结构分析

牛新书1,2; 徐荭2   

  1. 1. 河南师范大学化学与环境科学学院, 新乡 453002; 2. 河南省高等学校环境科学与工程重点学科开放实验室, 新乡 453002
  • 收稿日期:2000-03-30 修回日期:2000-04-21 出版日期:2001-03-20 网络出版日期:2001-03-20

Preparation and Structure Analysis of α-Fe2O3 Nanocrystalline in 2-Methoxyethanol System

NIU Xin-Shu1,2; XU Hong1   

  1. 1. College of Chemistry & Environmental Science; Henan Normal University; Xinxiang Henan 453002; China; 2. Key Laboratory of Environmental Science and Engineering; Euducation Commission of Henan; Xinxiang Henan 453002, China
  • Received:2000-03-30 Revised:2000-04-21 Published:2001-03-20 Online:2001-03-20

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摘要： 研究了在硝酸铁乙二醇甲醚溶液体系中，用溶胶－乳化－凝胶法制备氧化铁纳米晶，首次将表面活性剂（ＳＤＳ）引入溶胶－凝胶化过程，并采用一种高效缩合催化剂来加速此过程．结合ＴＥＭ、ＸＲＤ和ＴＧ－ＤＴＡ分析手段对产物进行了表征，结果表明，加入的表面活性剂（ＳＤＳ）有助于纯相α－Ｆｅ２Ｏ３纳米晶的生成，而缩合催化剂钛酸了酯的加入则大大缩短凝胶时间，所得粉体的原始晶粒尺寸为３０ｎｍ左右．若以常用的硅酸乙酯代替钛酸丁酯，则胶凝时间明显延长，最终产物为β和α氧化铁的混晶相（γ－Ｆｅ２Ｏ３为主晶相），晶粒尺寸约为１０ｎｍ，并从中提出了一条改进γ－Ｆｅ２Ｏ３基气敏材料性能的新思路．

关键词: 溶胶-乳化-凝胶, 钛酸丁酯, 硅酸乙酯, 十二烷基磺酸钠（SDS）, α-Fe2O3纳米晶

Abstract: The nanocrystal α-Fe2O3 with an average size of about 30nm was prepared by a sol-emulsify-gel method in
the iron nitrate and 2-methoxyethanol system. The powders were characterized by TEM, XRD and the xerogel primary powders thermal stability was studied by
TG-DTA. The gelation time was reduced greatly by adding tetrabutyl titanate. When tetraethyl orthosilicate instead of tetrabutyl titanate, the gelation
time can be much longer. γ-Fe2O3 with spinel structure appeared as the main phase in the calcinated powder and the average particle size
was about 10nm. A new idea to improve the gas sensitivity and stability of γ-Fe2O3 gas-sensitive materials was provided. The results show
that the introduction of surfactant(SDS) is helpful to form pure crystal phase α-Fe2O3.

Key words: sol-emulsify-gel, tetrabutyl titanate, ethyl orthosilicate, sodium dodecyl sulfonate (SDS), α-Fe_2O_3 nanocrystal

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