CN106747345A - 氧传感器ysz陶瓷层的制备方法 - Google Patents

氧传感器ysz陶瓷层的制备方法 Download PDF

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CN106747345A
CN106747345A CN201611014995.2A CN201611014995A CN106747345A CN 106747345 A CN106747345 A CN 106747345A CN 201611014995 A CN201611014995 A CN 201611014995A CN 106747345 A CN106747345 A CN 106747345A
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王耀斌
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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

氧传感器YSZ陶瓷层的制备方法
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系统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。
CN201611014995.2A 2016-11-18 2016-11-18 氧传感器ysz陶瓷层的制备方法 Pending CN106747345A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108736124A (zh) * 2018-04-03 2018-11-02 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

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108736124A (zh) * 2018-04-03 2018-11-02 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
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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