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不同鋯源對聚丙烯酰胺凝膠法制備氧化鋯納米粉體的影響
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內(nèi)蒙古工業(yè)大學(xué)

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國家自然科學(xué)基金資助(51164023,51364026);內(nèi)蒙古自然科學(xué)基金資助(2016MS0505);內(nèi)蒙古工業(yè)大學(xué)科學(xué)研究項(xiàng)目(X201410)資助


Effect of Zirconium Salts on Preparation of Zirconia Nanopowders via Polyacrylamide Gel Route
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Inner Mongolia University of Technology

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    摘要:

    采用聚丙烯酰胺凝膠法,分別以氧氯化鋯、硫酸鋯和硝酸氧鋯為鋯源制備ZrO2納米粉體,利用熱重-差熱同步分析儀(TG-DSC)、X射線衍射儀(XRD)和掃描電子顯微鏡(SEM) 分別對凝膠的熱分解過程及氧化鋯粉體的物相組成和形貌進(jìn)行分析和表征,研究了不同鋯源對聚丙烯酰胺凝膠法所制備的ZrO2納米粉體相轉(zhuǎn)變、物相組成及粉體形貌的影響。結(jié)果表明,鋯鹽影響聚丙烯酰胺凝膠的熱分解完全溫度,以硝酸氧鋯為前驅(qū)體制得的凝膠熱分解完全溫度最低,約為530 ℃,以硫酸鋯和氧氯化鋯為前驅(qū)體制得的凝膠熱分解完全溫度分別為573 ℃和580 ℃。鋯鹽影響氧化鋯的晶化溫度,但氧化鋯的相轉(zhuǎn)變過程相似,均是由無定型氧化鋯轉(zhuǎn)變?yōu)樗姆较嘌趸?,并?00 ℃時完全轉(zhuǎn)變?yōu)閱涡毕嘌趸?。氧化鋯的晶化溫度越高,平均粒徑越小,團(tuán)聚程度越高,以上述三種鋯源為前驅(qū)體均可制備出近似球形的納米氧化鋯粉體,粉體粒徑分布在52~97.4 nm范圍內(nèi)。

    Abstract:

    Zirconia nanopowders were prepared via polyzcrylamide gel route with different zirconium salt, including ZrOCl2·8H2O, Zr(SO4)2·4H2O and ZrO(NO3)2·2H2O. Thermogravimetric analysis (TG), differential scanning calorimetry analysis (DSC), X-ray diffraction (XRD) and scanning electron microscope (SEM) were used to characterize the thermal decomposition process of xerogel, phase compositions and morphologies of zirconia nanopowders. The influence of different zirconium salts on the phase transformation, phase compositions and morphologies of the as-prepared zirconia nanopowders by polyacrylamide gel route were studied. The results demonstrate that zirconium salt affects thermo-decomposing temperature of polyacrylamide gel. When precursor is zirconium oxynitrate, the thermo-decomposing temperature of xerogel is the lowest which is around 530 ℃. When precursors are zirconium sulfate and zirconium oxychloride, the thermo-decomposing temperatures of xerogels are around 573 ℃ and 580 ℃, respectively. Zirconium salt affects the crystallization temperature of zirconia, but the phase transformation of zirconia is similar, which transforms from amorphous to tetragonal and completely converts to monoclinic at 900 ℃. The higher the crystallization temperature of zirconia, the smaller the mean particle size, the more particle agglomeration. The nearly spherical zirconia nanopowders can be prepared and the particle size distribution is within the range of 52~97.4 nm with the above three zirconium salts as precursors.

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劉婷,陳偉東,鞠紅民,閆淑芳,馬文.不同鋯源對聚丙烯酰胺凝膠法制備氧化鋯納米粉體的影響[J].稀有金屬材料與工程,2019,48(6):2044~2048.[Liu Ting, Chen Weidong, Ju Hongmin, Yan Shufang, Ma Wen. Effect of Zirconium Salts on Preparation of Zirconia Nanopowders via Polyacrylamide Gel Route[J]. Rare Metal Materials and Engineering,2019,48(6):2044~2048.]
DOI:10.12442/j. issn.1002-185X.20171201

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  • 收稿日期:2017-12-26
  • 最后修改日期:2018-02-23
  • 錄用日期:2018-03-12
  • 在線發(fā)布日期: 2019-07-30
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