新型全固态pH传感器的研究

发布时间：2018-04-08 07:16

  本文选题：砂磨　切入点：全固态pH传感器　出处：《华东师范大学》2017年硕士论文

【摘要】：pH值与许多领域都息息相关,pH的测定也一直是这些领域不可缺少的过程。玻璃电极作为目前使用最广泛的pH传感器,其易破碎、测量环境局限性大的缺点日益突出。因此新型的非玻璃型的pH传感器近年来得到广泛研究,其中固体电解质pH传感器机械强度高、抗腐蚀性能强、且可用于高温高压环境;金属/金属氧化物pH传感器机械强度好,可微型化、耐高温高压。基于以上优点,本论文制备了两种全固态pH传感器,即掺Y锆酸钡陶瓷pH传感器以及Zr/ZrO_2PH传感器,对制备方法及性能进行了研究,主要内容如下:(1)分别采用高温固相反应及溶液化学法制备了 Y锆酸钡粉体,并对粉体烧结特性进行了对比,发现溶液化学法制备的空心球纳米粉体烧结性能较差。而高温固相反应制备的粉体颗粒细但团聚严重,需要进行研磨处理。行星球磨和砂磨两种方式对比结果表明,砂磨处理的粉体可以得到粒径小且分散均匀的颗粒。在1640℃烧结15h就能得到相对致密度为99%且超细晶粒的陶瓷,该烧结条件比文献中报道的低,且陶瓷电导率得到了显著提高。并初步探讨烧结致密的Y锆酸钡陶瓷对水蒸气及氨气的传感性能。(2)以掺Y锆酸钡陶瓷为固体电解质制备pH传感器,研究不同固体质子酸作为内参比及工作温度对传感器性能的影响。结果表明,以磷酸为内参比制备的掺Y锆酸钡陶瓷pH传感器,在20℃下响应较慢,但拟合度高,符合线性关系,斜率为-36.5 mV/pH。而在80℃下响应较快,拟合度也较高,但斜率有所下降;以硅钨酸为内参比制备的掺Y锆酸钡陶瓷pH传感器,20℃下响应比磷酸快,拟合度高,达到了 99.18%,符合线性关系,斜率为-29.44mV/pH。(3)通过高温氧化法和电化学氧化法制备了 Zr/ZrO_2PH传感器,并调节制备条件,研究不同方法和不同条件下制备的传感器性能之间的差异。采用高温氧化法制备时,用Na2CO3熔盐氧化制备的传感器性能最佳。在pH为4～12.47范围内,响应值非常稳定,且线性拟合度高,斜率为-28.16mV/pH。采用阳极氧化法制备时,对比了有机电解液和无机电解液对氧化膜表面纳米结构的影响。当采用无机电解液且第二步氧化时间为1h时,线性拟合度好,在pH为1.68～12.47范围内斜率达到了-31.51 mV/pH。
[Abstract]:The pH value is closely related to many fields and the determination of pH is also an indispensable process in these fields.Glass electrode is the most widely used pH sensor at present.Therefore, new non-glass-type pH sensors have been extensively studied in recent years. Among them, solid electrolyte pH sensors have high mechanical strength, strong corrosion resistance, and can be used in high temperature and high pressure environment, and metal / metal oxide pH sensors have good mechanical strength.It can be miniaturized and resistant to high temperature and high pressure.Based on the above advantages, two kinds of all-solid-state pH sensors, that is, barium zirconate doped ceramic pH sensor and Zr/ZrO_2PH sensor, were prepared in this paper.The main contents are as follows: (1) Barium Y zirconate powders were prepared by high temperature solid state reaction and solution chemistry respectively. The sintering characteristics of the powders were compared and it was found that the sintered properties of hollow spheres prepared by solution chemical method were poor.The powder prepared by high temperature solid-state reaction is fine and agglomeration, so it needs to be ground.The results of comparison between planetary ball milling and sand grinding show that the powders treated by sand grinding can obtain small and uniformly dispersed particles.When sintered at 1640 鈩，

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