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以CaF_2+SiO_2作为硅传感器辅助电极材料,将其均匀涂覆于ZrO_2(MgO)固体电解质表面,在高纯Ar气保护下,1400℃焙烧30min制备得到定硅传感器.利用X射线衍射仪、扫描电子显微镜以及能量色散谱仪系统研究了制备条件对于焙烧后形成的辅助电极膜层组成、物相和微观形貌的影响.膜层中不存在CaF2,而是以SiO2固体颗粒、CaO·MgO·2SiO_2固溶体及ZrSiO_4为主.另外,探讨了辅助电极膜层中物相的变化对于膜层黏结性以及定硅性能的影响.在1450℃下对铁液中硅含量进行测试,传感器响应时间在10s左右,稳定时间在20s以上,而且传感器的重复性也很理想.当铁液中硅质量分数在0.5%~1.5%时,硅传感器测量值与化学分析法分析值相吻合.
A silicon sensor was fabricated by using CaF_2 + SiO_2 as the auxiliary electrode material of silicon sensor and uniformly coating the surface of ZrO_2 (MgO) solid electrolyte under the protection of high purity Ar gas at 1400 ℃ for 30min. Using X-ray diffractometer, Electron microscopy and energy dispersive spectroscopy were used to study the influence of the preparation conditions on the composition, phase and morphology of the auxiliary electrode films formed after calcination.The results show that CaF2 does not exist in the film, but SiO2 solid particles, CaO · MgO · 2SiO_2 solid solution and ZrSiO 4 as the main.In addition, the influence of the phase change in the auxiliary electrode film on the cohesiveness of the film and the silicon-fixing performance was investigated.The silicon content in the molten iron was tested at 1450 ℃, the response time of the sensor was 10s , The stability time is more than 20s, and the repeatability of the sensor is also ideal.When the mass fraction of silicon in the molten iron is between 0.5% and 1.5%, the measured values of the silicon sensor coincide with those of the chemical analysis.