CN106747345A - 氧传感器ysz陶瓷层的制备方法 - Google Patents
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Abstract
本发明涉及功能材料技术领域,具体涉及一种氧传感器YSZ陶瓷层的制备方法。氧传感器YSZ陶瓷层的制备方法,以98%纯ZrCl4与分析纯Y(NO3)3为原料,乙醇为溶剂,配制成0.4~1.2mol/L的溶液置于反应釜中,制备8%Y2O3稳定ZrO2前驱体,煅烧2h得到YSZ粉体;PVA造粒后置于模具中,干压成型;将标称粒径为30nm的Al2O3粉体与烧结助剂CaO、MgO、SiO2粉末混合,一部分干压成型,另一部分与造粒后YSZ粉体共同压制成双层陶瓷生坯;将陶瓷坯片置于高温电炉中,以升温速率3~5℃/min升至800℃保温2h,之后以同样的升温速率升至1300~1600℃保温2~3h后随炉冷却,制成氧传感器YSZ陶瓷层。本发明制成的氧传感器YSZ陶瓷层在较低温度下可以共烧得到无翘曲无开裂YSZ/Al2O3双层陶瓷,满足氧传感器的使用要求。
Description
技术领域
本发明涉及功能材料技术领域,具体涉及一种氧传感器YSZ陶瓷层的制备方法。
背景技术
氧传感器广泛应用于现代汽车电喷发动机控制***中用于检测发动机排气中氧的浓度并将输出信号反馈给电脑,从而控制喷油量的大小,使三元催化转换器得以保证最佳空气净化率。氧传感器中起关键作用的是多层陶瓷传感元件,简称氧传感元。第一支汽车氧传感器早在1946年由博世公司发明,形态为管式,主要包括固体电解质、反应电极、参比电极。
Y2O3稳定ZrO2 (Yttria-Stabilized Zirconia,YSZ)陶瓷因其具有高氧离子电导率、强稳定性以及高强度、耐腐蚀等性质,常用来做氧传感元的固体电解质层,在YSZ两侧由反应电极与参比电极构成回路。YSZ陶瓷在低于350℃时电阻率较大,不能正常工作,需要加热棒在发动机启动瞬间对其加热。
1988年,第一个片式氧传感元面世。主要结构包含固体电解质层、反应电极、参比电极与加热电极层。氧传感元的平板化不但减小了体积、节约了原料与成本、提高了氧敏响应速率,而且生产过程中的流延技术会大大提高生产效率。但平板化后加热电极与固体电解质直接接触,会干扰固体电解质产生的电压信号,故在两者之间必需增加绝缘层以绝缘。绝缘层常采用高温绝缘性良好的Al2O3陶瓷,而电极多使用兼具高温稳定性与催化作用的多孔铂电极。采用丝网印刷铂浆料制备的铂电极烧结温度一般在1500℃以下。高于1500℃时,铂会向周围陶瓷扩散、或与一些杂质发生低共熔而收缩形成“孤岛”使得铂电极无法导通。为保证铂电极正常工作,必须在1500℃以下实现YSZ陶瓷层与Al2O3陶瓷层的叠层共烧。一般YSZ的烧结温度在1550~1650℃,而Al2O3则高达1800~2200℃。由于YSZ的烧结致密度越高电阻率越低氧敏响应性能越好,因此在较低共烧温度范围内,必须保证YSZ陶瓷的致密度符合使用要求,同时在保证绝缘性与强度的前提下需调节Al2O3的烧结致密度与YSZ匹配。
发明内容
本发明旨在提出一种氧传感器YSZ陶瓷层的制备方法。
本发明的技术方案在于:
氧传感器YSZ陶瓷层的制备方法,包括如下步骤:
以98%纯ZrCl4与分析纯Y (NO3)3为原料,乙醇为溶剂,配制成0.4~1.2mol/L的溶液置于反应釜中,在100~160℃下反应,制备8%Y2O3稳定ZrO2前驱体,经600~800℃煅烧2h 得到YSZ粉体;
将YSZ粉体用质量分数6%~8%的PVA 造粒后置于模具中,采用压片机加载4~10MPa 干压成型;将标称粒径为30nm的Al2O3粉体与烧结助剂CaO、MgO、SiO2粉末混合,配方为95 Al2O3-0.7MgO-xCaO-(4.3-x ) SiO2用PVA 造粒后一部分干压成型,另一部分与造粒后YSZ粉体共同压制成双层陶瓷生坯;
将陶瓷坯片置于高温电炉中,以升温速率3~5℃/min升至800℃保温2h,之后以同样的升温速率升至1300~1600℃保温2~3h 后随炉冷却,制成氧传感器YSZ陶瓷层。
本发明的技术效果在于:
本发明利用溶剂热的方法,通过调控反应温度与反应物的浓度可以获得粒度较小的YSZ粉体,在1400℃下可实现致密烧结,并得到较低电阻率;通过烧结助剂可以降低Al2O3的烧结温度,以适应YSZ及之后与电极共烧的要求;同时通过调节Al2O3中α相与γ相的比例,可以调节Al2O3陶瓷在共烧温度下的烧结收缩率,使之与YSZ在同温度下的烧结收缩率相匹配,从而在较低温度下可以共烧得到无翘曲无开裂YSZ/ Al2O3双层陶瓷,满足氧传感器的使用要求。
具体实施方式
氧传感器YSZ陶瓷层的制备方法,包括如下步骤:
以98%纯ZrCl4与分析纯Y (NO3)3为原料,乙醇为溶剂,配制成0.4~1.2mol/L的溶液置于反应釜中,在100~160℃下反应,制备8%Y2O3稳定ZrO2前驱体,经600~800℃煅烧2h 得到YSZ粉体;
将YSZ粉体用质量分数6%~8%的PVA 造粒后置于模具中,采用压片机加载4~10MPa 干压成型;将标称粒径为30nm的Al2O3粉体与烧结助剂CaO、MgO、SiO2粉末混合,配方为95 Al2O3-0.7MgO-xCaO-(4.3-x ) SiO2用PVA 造粒后一部分干压成型,另一部分与造粒后YSZ粉体共同压制成双层陶瓷生坯;
将陶瓷坯片置于高温电炉中,以升温速率3~5℃/min升至800℃保温2h,之后以同样的升温速率升至1300~1600℃保温2~3h 后随炉冷却,制成氧传感器YSZ陶瓷层。
Claims (1)
1.氧传感器YSZ陶瓷层的制备方法,其特征在于:包括如下步骤:
以98%纯ZrCl4与分析纯Y (NO3)3为原料,乙醇为溶剂,配制成0.4~1.2mol/L的溶液置于反应釜中,在100~160℃下反应,制备8%Y2O3稳定ZrO2前驱体,经600~800℃煅烧2h 得到YSZ粉体;
将YSZ粉体用质量分数6%~8%的PVA 造粒后置于模具中,采用压片机加载4~10MPa 干压成型;将标称粒径为30nm的Al2O3粉体与烧结助剂CaO、MgO、SiO2粉末混合,配方为95 Al2O3-0.7MgO-xCaO-(4.3-x ) SiO2用PVA 造粒后一部分干压成型,另一部分与造粒后YSZ粉体共同压制成双层陶瓷生坯;
将陶瓷坯片置于高温电炉中,以升温速率3~5℃/min升至800℃保温2h,之后以同样的升温速率升至1300~1600℃保温2~3h 后随炉冷却,制成氧传感器YSZ陶瓷层。
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CN108736124B (zh) * | 2018-04-03 | 2020-11-10 | 苏州市协诚五金制品有限公司 | 一种基于陶瓷介质滤波器的制备工艺 |
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