物理化学学报 >> 2010, Vol. 26 >> Issue (12): 3365-3368.doi: 10.3866/PKU.WHXB20101205

材料物理化学 上一篇    下一篇

前驱体法制备Mn2O3空心橄榄形结构及形貌演化

李英品, 郝彦忠   

  1. 河北科技大学理学院, 石家庄050018
  • 收稿日期:2010-06-18 修回日期:2010-09-13 发布日期:2010-12-01
  • 通讯作者: 李英品 E-mail:liyingpin@126.com
  • 基金资助:

    河北科技大学博士科研启动基金(QD200959), 河北省自然科学基金(B2010000856)和国家自然科学基金(20573031)资助项目

Synthesis of Mn2O3 with a Hollow Olive Shape and Its Morphology Evolution

LI Ying-Pin, HAO Yan-Zhong   

  1. College of Science, Hebei University of Science and Technology, Shijiazhuang 050018, P. R. China
  • Received:2010-06-18 Revised:2010-09-13 Published:2010-12-01
  • Contact: LI Ying-Pin E-mail:liyingpin@126.com
  • Supported by:

    The project was supported by the Doctoral Starting up Foundation of Hebei University of Science and Technology, China (QD200959), Provincial Natural Science Foundation of Hebei, China (B2010000856), and National Natural Science Foundation of China (20573031).

摘要:

利用苹果酸还原高锰酸钾以水热合成方法制备了具有橄榄形貌的纳米结构MnCO3 前驱体, 通过600 ℃焙烧MnCO3前驱体得到橄榄形Mn2O3. 以扫描电镜(SEM)、透射电镜(TEM)、X射线衍射(XRD)、热重-差热分析(TG-DTA)等方法对产物的形貌和结构进行了表征. 考察了MnCO3前驱体微观形貌随水热反应时间的演变: 当水热反应时间为2 h 时得到具有橄榄形形貌的MnCO3前驱体, 空心结构的壁比较厚; 当水热反应时间延长到6 h 时得到的MnCO3前驱体仍然具有橄榄形形貌, 壁变薄; 当反应时间延长到24 h 时得到的MnCO3前驱体仍然具有橄榄形形貌, 并且壁非常薄. 我们推测在Ostwald 熟化机理作用下, 空心橄榄形MnCO3前驱体随着反应时间的延长其壁逐渐由160 nm演化为30 nm.

关键词: 水热合成, Mn2O3, 空心, 橄榄形

Abstract:

Permanganic potassium was reduced by malic acid under hydrothermal conditions without a template or additives and olive-shaped MnCO3 particles were obtained. After the MnCO3 precursor was calcined at 600 °C for 3 h, Mn2O3 was obtained and the olive-shape morphology was maintained. The products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and thermogravimetry-differential thermal analysis (TG-DTA). The effect of hydrothermal reaction time on the morphology of the products was studied. A MnCO3 precursor with hollow olive morphology and thick wall was obtained when the reaction time was 2 h. When the reaction time was increased to 6 h, the wall of the hollow olive-shaped particles became thinner. When the reaction time was increased to 24 h the wall thickness of the MnCO3 precursor with the hollow olive morphology was about 30 nm. Because of the Ostwald-Ripening effect, the morphology of the MnCO3 precursor gradually evolved from thick-wall hollow olive to thin-wall hollow olive by increasing the reaction time.

Key words: Hydrothermal synthesis, Mn2O3, Hollow, Olive

MSC2000: 

  • O648