钆锆烧绿石的高温固相法制备及工艺影响研究

The Process Impact on the Preparation of Gd_2Zr_2O_7 Pyrochlore by High Temperature Solid Phase Method

为获得高温固相法制备钆锆烧绿石的最佳工艺条件,弄清制备工艺对钆锆烧绿石物相纯度等的影响,研究以Gd2O3和ZrO2粉体为原料,综合考虑成型压力(0~15 MPa)、烧结温度(1 350~1 500℃)及保温时间(12~72h)对烧结效果的影响,设计L16(45)正交实验开展钆锆烧绿石的制备工作。借助粉末X射线衍射仪(XRD)及拉曼散射光谱仪(Raman)对所制备样品的物相及分子结构进行分析,利用扫描电子显微镜(SEM)对样品的显微形貌进行观察。结果表明:所考虑工艺参数中对钆锆烧绿石烧结效果的影响大小依次为烧结温度、成型压力和保温时间;钆锆烧绿石的最佳制备条件为成型压力15 MPa,1 500℃保温72h。同时,探讨了制备工艺对烧结效果的影响机理。

In order to study the influence of preparation process on the phase purity and to optimize the process,Gd2Zr2O7 pyrochlore was fabricated by the high temperature solid-phase method,using Gd2O3 and ZrO2 as raw materials.Sintering parameters,such as temperature（1 3501 500℃）,holding time（1272 h）and molding pressure（015 MPa）were comprehensively considered.The optimal process for the fabrication of Gd2Zr2O7 pyrochlore was selected by L16（45）orthogonal experiment.XRD,Raman,SEM were exploited to characterize the phase and microstructure of the synthetic samples.The results shows that sintering temperature,shaping pressure and holding time influence the final effect in turn,and the best process conditions were obtained as sintering at 1 500℃for 72 hwith the molding pressure of15 MPa.In addition,the influence mechanism of preparation process on sintering was analyzed.