Er2Ti2O7烧绿石基玻璃陶瓷固化体的制备工艺研究

Study on Preparation Technology of Er2Ti2O7 Pyrochlore-based Glass-ceramic Form

  • 摘要: 为获得含单一钛酸盐烧绿石的玻璃陶瓷固化体,本文以Er2Ti2O7作为钛酸盐烧绿石代表,在传统的烧结法制备工艺基础上,通过热雾喷解和晶核掺入的技术改进,分别研究了烧结温度、烧结时间、玻璃与陶瓷晶核质量配比等参数对Er2Ti2O7基玻璃陶瓷固化体物相及结构的影响规律。XRD结果表明:在不同的烧结温度、烧结时间和质量配比下,均能获得含单一Er2Ti2O7烧绿石的玻璃陶瓷固化体,Er2Ti2O7前驱体在玻璃中的相稳定性好,未发生相分解,玻璃组分亦未受陶瓷相的影响而析出第二相;玻璃组分对陶瓷颗粒存在张应力作用,玻璃含量越高,Er2Ti2O7的晶胞常数越大;提高烧结温度和烧结时间均有利于增强固化体中Er2Ti2O7的结构有序性,但烧结温度效果强于烧结时间。SEM结果表明:Er2Ti2O7在玻璃基体上呈四方形生长,与玻璃界面清晰,相容性好。固化体的物性测试结果表明,玻璃组分占比将直接影响固化体的表观孔隙率和致密度。根据以上结果可知,新工艺制备的样品具有相纯度高、烧绿石相与玻璃相容性好、两相比例可调等优点,较好地解决了钛酸盐烧绿石在玻璃基体中易发生相分解的问题。

     

    Abstract: In order to obtain a glass-ceramic form containing a single titanate pyrochlore, the technologies of spray pyrolysis method and nucleation incorporation were proposed based on the traditional sintering process using Er2Ti2O7 as titanate pyrochlore simulant, and the effects of sintering temperature, sintering time, mass ratio of glass and ceramic crystal nuclei on the phase and structure of Er2Ti2O7 based glass-ceramic were studied. The XRD patterns show that the glass-ceramic containing single Er2Ti2O7 pyrochlore can be obtained under different sintering temperatures, sintering time and mass ratios. The phase stability of the Er2Ti2O7 precursor in the glass is good, no phase decomposition occurs, and the glass component is not affected by the ceramic phase to precipitate the second phase. The glass component has tensile stress on the ceramic phase. The higher the glass content is, the larger the cell constant of Er2Ti2O7 is. Increasing the sintering temperature and sintering time is beneficial to enhance the structural order of Er2Ti2O7 in the solidified body, but the sintering temperature effect is stronger than that of the sintering time. The SEM images show that Er2Ti2O7 grows in a square shape on the glass substrate, and has a clear interface with glass and good compatibility. The physical property test results of the glass-ceramic show that the proportion of the glass component directly affects the apparent porosity and density of the glass-ceramic. The glass-ceramic form prepared by the new process has the advantages of high phase purity, good compatibility between glass and pyrochlore, and adjustable ratio of two comparisons. The problem of phase decomposition of titanate pyrochlore in glass matrix is well solved.

     

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