一锅法制备氧化锆纤维前躯体
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摘要
以氧氯化锆、硝酸钇等为原料,采用一锅法制备氧化锆纤维前躯体,研究了不同反应温度、液相黏度对制备的氧化锆纤维前躯体性能的影响;采用X射线衍射、红外光谱、扫描电子显微镜以及差热-热重分析对氧化锆纤维前躯体及氧化锆纤维进行表征,采用静电纺丝法对制备的氧化锆纤维前躯体的可纺性进行了验证。结果表明:采用一锅法可以快速制备氧化锆纤维前躯体——聚乙酰丙酮锆纺丝液,采用静电纺丝可以获得高纯立方相氧化锆纤维。
The spinning solution of zirconia fiber precursor was prepared by using zirconium oxychloride and acetylacetone as raw materials by one-pot method. The effects of different reaction temperature and solution viscosity on the properties of the zirconia fiber precursors were studied. The prepared precursors and zirconia fibers were characterized by X ray diffraction,infrared spectroscopy(FT-IR),scanning electron microscope and differential thermal-thermogravimetric analysis,the spinability of the prepared precursor was verified by electrospinning method. The results show that the zirconia fiber precursor,spinning solution of polyacetylacetonatozirconium is prepared rapidly by one-pot method,and the zirconia fibers with high purity and cubic crystal are obtained by electrospinning method.
The spinning solution of zirconia fiber precursor was prepared by using zirconium oxychloride and acetylacetone as raw materials by one-pot method. The effects of different reaction temperature and solution viscosity on the properties of the zirconia fiber precursors were studied. The prepared precursors and zirconia fibers were characterized by X ray diffraction,infrared spectroscopy(FT-IR),scanning electron microscope and differential thermal-thermogravimetric analysis,the spinability of the prepared precursor was verified by electrospinning method. The results show that the zirconia fiber precursor,spinning solution of polyacetylacetonatozirconium is prepared rapidly by one-pot method,and the zirconia fibers with high purity and cubic crystal are obtained by electrospinning method.
引文
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[2]胡立明,高芳,齐健梅,等.高压Ni-H2电池用氧化锆纤维布性能研究[J].硅酸盐通报,2009,28(2):395-399.
[3]胡立明.氧化锆纤维布的研究[D].武汉:武汉理工大学,2002.
[4] HARTRIDGEAL A,TAYLORAL M D,BHATTACHARYA A K.Synthesis and characterization of partially and fully stabilized zirconia fibers made from an inorganic precursor[J]. Journal of Materials Research,2001,16(8):2384-2390.
[5] LI L,ZHANG P,LIANG J,et al. Phase transformation and morphological evolution of electrospun zirconia nanofibers during thermal annealing[J]. Ceramics International,2010,36(2):589-594.
[6]刘和义,刘贵双,裴石光,等.聚乙酰丙酮合锆甩丝法制备氧化锆纤维棉[J].硅酸盐通报,2011,30(6):1410-1414,1424.
[7]李泉,李靖华.溶胶-凝胶法微晶氧化锆纤维的研究[J].钢铁研究学报,1993,5(2):68-71.
[8]刘久荣,潘梅,许东,等. Sol-gel法制备Zr O2连续纤维的烧结过程的研究[J].山东工业大学学报,2001,31(2):140-146.
[9]刘贵双.氧化锆纤维及纤维板的制备与性能研究[D].南京:南京理工大学,2012.