研究论文

氮化铁纳米晶的溶剂热合成

  • 刘淑玲 ,
  • 仝建波
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  • (陕西科技大学 1. 化学与化工学院; 2. 教育部轻化工助剂化学与技术重点实验室, 西安 710021)

收稿日期: 2008-12-08

  修回日期: 2009-02-28

  网络出版日期: 2009-09-20

Solvothermal Synthesis of Iron Nitride Nanocrystal

  • LIU Shu-Ling ,
  • TONG Jian-Bo
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  • (1. College of Chemistry and Chemical Engineering, Shaanxi University of Science & Technology, Xi’an 710021, China; 2. Key Laboratory of Auxiyiary Chemistry & Technology for Chemical Industry, Ministry of Edulation, Xi’an 710021, China)

Received date: 2008-12-08

  Revised date: 2009-02-28

  Online published: 2009-09-20

摘要

以氯化亚铁(FeCl2·4H2O)为铁源, 氯化铵(NH4Cl)和叠氮化钠(NaN3)为混合氮源, 通过溶剂热合成法制备了具有包覆结构的氮化铁纳米晶. 分别采用X射线衍射(XRD)、 透射电镜(TEM)和高分辨透射电镜(HRTEM)对最终产物的形貌特征和物相组成进行了表征, 结合处理前后产物的XRD检测, 探讨了氮化铁纳米晶复合结构形成的机理. 对影响实验的因素,如反应温度、反应时间、加料次序和磁性质等进行了研究. 结果表明:通过严格控制加料次序, 在有机溶剂二甲苯中400℃反应12h可以合成氮化铁复合结构纳米晶. 由于核壳结构的影响, 氮化铁纳米晶最大比饱和磁化强度比文献值低.

本文引用格式

刘淑玲 , 仝建波 . 氮化铁纳米晶的溶剂热合成[J]. 无机材料学报, 2009 , 24(5) : 989 -992 . DOI: 10.3724/SP.J.1077.2009.00989

Abstract

Iron nitride nanocrystallines with core/shell structure were synthesized by solvothermal method using FeCl2·4H2O as Fe source, NH4Cl and NaN3 as mixed nitrogen source. XRD, TEM and HRTEM were adopted to characterize the phase composition morphology, and core/shell structure of the final product, respectively. The mechanism of the formation of Fe4N nanocrystallines with core/shell structure were discussed based on the XRD analysis. The effects of temperature, reaction time and feeding order in the experiment and the magnetic property were studied. The results indicate that Fe4N nanocrystallines with core/shell structure can be prepared in xylene at 400℃ through the precise control of the feeding order. Because of core/shell structure of the product, the maximum value of the specific saturation magnetization of the iron nitride nanocrystal is lower than the value reported by reference.

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