新型全固態(tài)pH傳感器的研究
發(fā)布時間:2018-04-08 07:16
本文選題:砂磨 切入點(diǎn):全固態(tài)pH傳感器 出處:《華東師范大學(xué)》2017年碩士論文
【摘要】:pH值與許多領(lǐng)域都息息相關(guān),pH的測定也一直是這些領(lǐng)域不可缺少的過程。玻璃電極作為目前使用最廣泛的pH傳感器,其易破碎、測量環(huán)境局限性大的缺點(diǎn)日益突出。因此新型的非玻璃型的pH傳感器近年來得到廣泛研究,其中固體電解質(zhì)pH傳感器機(jī)械強(qiáng)度高、抗腐蝕性能強(qiáng)、且可用于高溫高壓環(huán)境;金屬/金屬氧化物pH傳感器機(jī)械強(qiáng)度好,可微型化、耐高溫高壓;谝陨蟽(yōu)點(diǎn),本論文制備了兩種全固態(tài)pH傳感器,即摻Y(jié)鋯酸鋇陶瓷pH傳感器以及Zr/ZrO_2PH傳感器,對制備方法及性能進(jìn)行了研究,主要內(nèi)容如下:(1)分別采用高溫固相反應(yīng)及溶液化學(xué)法制備了 Y鋯酸鋇粉體,并對粉體燒結(jié)特性進(jìn)行了對比,發(fā)現(xiàn)溶液化學(xué)法制備的空心球納米粉體燒結(jié)性能較差。而高溫固相反應(yīng)制備的粉體顆粒細(xì)但團(tuán)聚嚴(yán)重,需要進(jìn)行研磨處理。行星球磨和砂磨兩種方式對比結(jié)果表明,砂磨處理的粉體可以得到粒徑小且分散均勻的顆粒。在1640℃燒結(jié)15h就能得到相對致密度為99%且超細(xì)晶粒的陶瓷,該燒結(jié)條件比文獻(xiàn)中報(bào)道的低,且陶瓷電導(dǎo)率得到了顯著提高。并初步探討燒結(jié)致密的Y鋯酸鋇陶瓷對水蒸氣及氨氣的傳感性能。(2)以摻Y(jié)鋯酸鋇陶瓷為固體電解質(zhì)制備pH傳感器,研究不同固體質(zhì)子酸作為內(nèi)參比及工作溫度對傳感器性能的影響。結(jié)果表明,以磷酸為內(nèi)參比制備的摻Y(jié)鋯酸鋇陶瓷pH傳感器,在20℃下響應(yīng)較慢,但擬合度高,符合線性關(guān)系,斜率為-36.5 mV/pH。而在80℃下響應(yīng)較快,擬合度也較高,但斜率有所下降;以硅鎢酸為內(nèi)參比制備的摻Y(jié)鋯酸鋇陶瓷pH傳感器,20℃下響應(yīng)比磷酸快,擬合度高,達(dá)到了 99.18%,符合線性關(guān)系,斜率為-29.44mV/pH。(3)通過高溫氧化法和電化學(xué)氧化法制備了 Zr/ZrO_2PH傳感器,并調(diào)節(jié)制備條件,研究不同方法和不同條件下制備的傳感器性能之間的差異。采用高溫氧化法制備時,用Na2CO3熔鹽氧化制備的傳感器性能最佳。在pH為4~12.47范圍內(nèi),響應(yīng)值非常穩(wěn)定,且線性擬合度高,斜率為-28.16mV/pH。采用陽極氧化法制備時,對比了有機(jī)電解液和無機(jī)電解液對氧化膜表面納米結(jié)構(gòu)的影響。當(dāng)采用無機(jī)電解液且第二步氧化時間為1h時,線性擬合度好,在pH為1.68~12.47范圍內(nèi)斜率達(dá)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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