Journal of Inorganic Materials ›› 2011, Vol. 26 ›› Issue (3): 321-326.DOI: 10.3724/SP.J.1077.2011.00321

• Research Paper • Previous Articles     Next Articles

Synthesis of Ramsdellite by Refluxing Processand Its Influencing Factors

YIN Hui, LIU Fan, FENG Xiong-Han, TAN Wen-Feng, QIU Guo-Hong, Chen Xiu-Hua, LIU Ming-Ming   

  1. Collegeof Resources and Environment, Huazhong Agricultural University, Wuhan 430070,China
  • Received:2010-05-20 Revised:2010-07-26 Published:2011-03-20 Online:2011-02-18
  • Supported by:

    National Natural Science Foundation of China (20807019, 40771102); Specialized Research Fund for the Doctoral Program of Higher Education of China (20070504053)

Abstract: Nanosized ramsdellite was synthesized by oxidizing 30mmol Manganese(II) sulfate dissolved in different amounts of hydrochloride (0,10, 20 and 40 mmol) with adding 60 mmol sodium hypochlorite solution atconstant velocity of 1 mL/min minute using a refluxing process at atmosphericpressure at different temperatures (60, 80 and 100℃). The products were characterized by XRD diffraction,scanning electron microscope and automated surface area analyzer. The effectsof reflux temperature, time and amount of hydrochloric acid on the crystalstructures, micromorphologies and yield of products were investigated. It was observed that nano-particles of conglobated ramsdellite was prepared at 60℃, and particle size increased with elevating the refluxing temperature. Both aggregate level and particle size of ramsdellite decrease after adding hydrochloric acid into the reaction solution. When the reflux reaction was carried out at 100℃ with adding different amount of hydrochloric acid,nano-size particles of ramsdellite were formed firstly, and then needle-like fibers of products came into being formed. The concentration of hydrochloricacid in the reaction system plays an important role in the morphologies of ramsdellitecrystal, which acts more remarkably at higher temperatures. It is favorable tothe formation of needle-like ramsdellite in nano size and aggregation with loose structures by addition of no less than 10 mmol hydrochloric acid into thereaction solution at 100℃. Ramsdellite particles with high specific surface area(maximum of 66.32 m2/g) are more prone to be formed byadding hydrochloric acid into the reaction solution at lower refluxing temperature. Product yield increases firstly and then decreases with the increase of the amount of hydrochloric acid and refluxing temperature, and the highest yield can be as high as 97.5%.

Key words: manganeseoxides, ramsdellite, refluxing at atmospheric pressure, nano-materials

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