CN114685164A - 一种用于制备氧传感器芯片的流延膜片及其制备工艺 - Google Patents
一种用于制备氧传感器芯片的流延膜片及其制备工艺 Download PDFInfo
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Abstract
本发明公开了一种用于制备氧传感器芯片的流延膜片,氧化锆膜片按重量百分比的配方如下:氧化锆粉体:62~65wt%;分散剂:0.5~0.7wt%;消泡剂:0.3~0.4wt%;塑化剂:2.4~2.6wt%;黏结剂:4~6wt%;有机溶剂:25~30wt%,上述组分之和为100wt%;氧化铝膜片按重量百分比的配方如下:氧化铝粉体:40~43wt%;助熔剂:0.7~1.0wt%;分散剂:0.3~0.5wt%;消泡剂:0.2~0.3wt%;塑化剂:1.0~1.5wt%;黏结剂:7~8.5wt%;有机溶剂:45~50wt%,上述组分之和为100wt%。该膜片塑性强度高、加工性能良好,能够有效减少打孔、印刷及叠片过程中的破损率及暗裂纹的产生,提高芯片烧成良率。
Description
技术领域
本发明涉及氧传感器技术领域,尤其涉及一种用于制备氧传感器芯片的流延膜片及其制备工艺。
背景技术
随着环保政策及燃油车排放标准的愈发严苛,燃油车发动机的燃油燃烧技术和尾气催化技术也日益成熟,以应对新的排放标准以及电动车对燃油车市场的冲击。由于燃油车的燃烧系统和尾气催化系统由ECU进行闭环控制,其是通过各传感单元进行数据采集、经过程序计算后输出控制信号以控制过量空气系数的变化,这要求各传感单元的输出信号能及时反应出各检测量的变化情况,因此对前氧传感器和后氧传感器的测量精度和灵敏度要求也越来越高。
目前车用氧传感器芯片的敏感单元基本都是由氧化锆陶瓷作为固体电解质,利用其高温下(主要应用范围500~900℃)的离子导电性来反馈待测气体中的氧浓度。流延技术用于制备陶瓷生瓷片及印刷技术和HTCC、LTCC工艺的应用,在功能陶瓷器件体积微小型化的同时大幅提高元件的集成度和灵敏度。由于氧化锆在高温下呈现导电性,需要在传输电极同氧化锆基体间做好绝缘,避免传输信号受到干扰。而氧化铝传热快、绝缘性优异,可制备氧化铝膜片用作缘材料。
发明内容
本发明提出了一种用于制备氧传感器芯片的流延膜片及其制备工艺,以解决上述背景技术中提出的问题。
本发明提出了一种用于制备氧传感器芯片的流延膜片,氧化锆膜片按重量百分比的配方如下:氧化锆粉体:62~65wt%;分散剂:0.5~0.7wt%;消泡剂:0.3~0.4wt%;塑化剂:2.4~2.6wt%;黏结剂:4~6wt%;有机溶剂:25~30wt%,上述组分之和为100wt%;
氧化铝膜片按重量百分比的配方如下:氧化铝粉体:40~43wt%;助熔剂:0.7~1.0wt%;分散剂:0.3~0.5wt%;消泡剂:0.2~0.3wt%;塑化剂:1.0~1.5wt%;黏结剂:7~8.5wt%;有机溶剂:45~50wt%,上述组分之和为100wt%。
优选的,所述的氧化锆粉体为钇稳定氧化锆粉体,比表面积:8.61m2/g,粒径分布范围:0.11~0.71μm。
优选的,所述的氧化铝粉体纯度,比表面积:16m2/g,粒径分布范围:0.11~0.21μm。
优选的,所述的助熔剂由二氧化硅、二氧化钛、碳酸钙、氧化镁粉体组成,其中,二氧化硅、二氧化钛和碳酸钙为分析纯级试剂,氧化镁粒径30±5nm、纯度≥99%;各组分的质量百分比为:二氧化硅:40~42wt%;碳酸钙:40~45wt%;氧化镁:14~17wt%;二氧化钛:3~5wt%。
优选的,所述的有机溶剂由无水乙醇、甲苯、二甲苯中的2种或以上组合而成,各组分的质量百分比为:无水乙醇:35~40wt%;甲醇:5~10wt%;二甲苯:35~40wt%;环己酮:3~5%。
本发明还提供了一种用于制备氧传感器芯片的流延膜片的制备工艺,包括如下步骤:
S1、分别按质量百分比称取除黏结剂以外的氧化锆膜片或者氧化铝膜片各组分,倒入氧化锆球磨罐中,加入氧化锆球石,球石和原料的质量比为:3:1,并确保球磨罐中有1/3~1/2的剩余空间;
S2、球磨设备为卧式罐磨机,设定球磨转速为14.5r/min、初步球磨时间为24h;
S3、向步骤S2初步混合均匀的浆料中加入黏结剂,设定球磨转速为17r/min、球磨时间36h;
S4、使用蠕动泵将球磨好的浆料抽入筛网中进行过滤,筛网孔径为200目;
S5、过滤后的浆料放入真空除泡机中除去浆料中的空气,参数设定为:真空度:80KPa,搅拌转速:160r/min,除泡时间:8min;
S6、将处理好的浆料泵入到流延机的料盒中,控制料盒中的液面高度为10~14mm,流延速度:0.4~0.5m/min,膜带紧张力:25~30N;根据膜片种类不同,刮刀高度需单独调节,其中,氧化锆膜对应高度为4~4.5mm,氧化铝膜片对应高度为3~3.5mm;
S7、流延膜片的干燥:膜片流出后分别经过4个干燥区域,每个干燥区域的长度都为1.5m,温度依次设定为50℃、60℃、70℃、75℃;相对应地,流延环境控制范围:温度22~25℃、相对湿度:40~50%。
优选的,氧化铝膜片干燥后的厚度为0.7mm,氧化锆膜片干燥后的厚度为1.2mm,膜片表面平整度:±5μm。
本发明的技术关键之一是球磨转速和时间需设置合理,转速太慢球石无法随球磨罐一起运动从而沉积在底部,转速太快则球石吸附在罐壁无法下落,此两种情况下球石都不能对浆料起到剪切、分散作用。且因为氧化锆和氧化铝粉体的粒径<1μm,在浆料中容易团聚,需要足够的球磨时长来打开团聚状态。
本发明的技术关键之二是流延时通过液面高度、刮刀高度来控制膜片厚度时,需要与干燥制度相匹配,确保流延膜片在流出后能够均匀在PE膜带上铺开,通过在膜带底部加热,促进溶剂从膜片底部向上表面扩散及表面溶剂的挥发过程,且使两者速率保持动态平衡,防止因膜片过后或温度过高导致表面挥发速度远大于内部的扩散速度,致使膜片表面出现开裂、针孔缺陷。
与现有技术相比,本发明的有益效果在于:本发明所制备的氧化铝和氧化锆膜片厚度均匀,表面平整度控制在±5μm,可以满足精准电路的印刷和多层元件的组装精度要求,适用于制备氧传感器芯片、多层功能陶瓷等器件。
具体实施方式
以下结合实施例进一步对本发明进行说明,但本发明的内容不仅仅局限于下面的实施例。
实施例1
本实施例的流延浆料配比见表1以及表2,按照制备步骤进行球磨、过滤、脱泡后,所制备的浆料粘度为2351mPa·s。按照表3中的参数对流延设备进行调整,干燥后的氧化锆膜片厚度为1.21mm,表面平整度差值0.04mm,膜片表面光滑平整无裂纹,膜片拉伸断裂强度达到2.3MPa,浆料及膜片的具体性能参数见表4。
表1氧化锆膜片各组分质量百分比(单位:wt%)
表2氧化铝膜片各组分质量百分比(单位:wt%)
表3各实施例的流延设备参数
表4各实施例中浆料及膜片性能参数
注:实施例2至6的配比参数、流延参数、性能指标见表1至4。
由上可知,该膜片塑性强度高、加工性能良好,能够有效减少打孔、印刷及叠片过程中的破损率及暗裂纹的产生,提高芯片烧成良率。本发明所制备的氧化铝和氧化锆膜片厚度均匀,表面平整度控制在±5μm,可以满足精准电路的印刷和多层元件的组装精度要求,适用于制备氧传感器芯片、多层功能陶瓷等器件。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (7)
1.一种用于制备氧传感器芯片的流延膜片,其特征在于,氧化锆膜片按重量百分比的配方如下:氧化锆粉体:62~65wt%;分散剂:0.5~0.7wt%;消泡剂:0.3~0.4wt%;塑化剂:2.4~2.6wt%;黏结剂:4~6wt%;有机溶剂:25~30wt%,上述组分之和为100wt%;
氧化铝膜片按重量百分比的配方如下:氧化铝粉体:40~43wt%;助熔剂:0.7~1.0wt%;分散剂:0.3~0.5wt%;消泡剂:0.2~0.3wt%;塑化剂:1.0~1.5wt%;黏结剂:7~8.5wt%;有机溶剂:45~50wt%,上述组分之和为100wt%。
2.根据权利要求1所述的用于制备氧传感器芯片的流延膜片,其特征在于,所述的氧化锆粉体为钇稳定氧化锆粉体,比表面积:8.61m2/g,粒径分布范围:0.11~0.71μm。
3.根据权利要求1所述的用于制备氧传感器芯片的流延膜片,其特征在于,所述的氧化铝粉体纯度,比表面积:16m2/g,粒径分布范围:0.11~0.21μm。
4.根据权利要求1所述的用于制备氧传感器芯片的流延膜片,其特征在于,所述的助熔剂由二氧化硅、二氧化钛、碳酸钙、氧化镁粉体组成,其中,二氧化硅、二氧化钛和碳酸钙为分析纯级试剂,氧化镁粒径30±5nm、纯度≥99%;各组分的质量百分比为:二氧化硅:40~42wt%;碳酸钙:40~45wt%;氧化镁:14~17wt%;二氧化钛:3~5wt%。
5.根据权利要求1所述的用于制备氧传感器芯片的流延膜片,其特征在于,所述的有机溶剂由无水乙醇、甲苯、二甲苯中的2种或以上组合而成,各组分的质量百分比为:无水乙醇:35~40wt%;甲醇:5~10wt%;二甲苯:35~40wt%;环己酮:3~5%。
6.一种根据权利要求1-5任一项所述的用于制备氧传感器芯片的流延膜片的制备工艺,其特征在于,包括如下步骤:
S1、分别按质量百分比称取除黏结剂以外的氧化锆膜片或者氧化铝膜片各组分,倒入氧化锆球磨罐中,加入氧化锆球石,球石和原料的质量比为:3:1,并确保球磨罐中有1/3~1/2的剩余空间;
S2、球磨设备为卧式罐磨机,设定球磨转速为14.5r/min、初步球磨时间为24h;
S3、向步骤S2初步混合均匀的浆料中加入黏结剂,设定球磨转速为17r/min、球磨时间36h;
S4、使用蠕动泵将球磨好的浆料抽入筛网中进行过滤,筛网孔径为200目;
S5、过滤后的浆料放入真空除泡机中除去浆料中的空气,参数设定为:真空度:80KPa,搅拌转速:160r/min,除泡时间:8min;
S6、将处理好的浆料泵入到流延机的料盒中,控制料盒中的液面高度为10~14mm,流延速度:0.4~0.5m/min,膜带紧张力:25~30N;根据膜片种类不同,刮刀高度需单独调节,其中,氧化锆膜对应高度为4~4.5mm,氧化铝膜片对应高度为3~3.5mm;
S7、流延膜片的干燥:膜片流出后分别经过4个干燥区域,每个干燥区域的长度都为1.5m,温度依次设定为50℃、60℃、70℃、75℃;相对应地,流延环境控制范围:温度22~25℃、相对湿度:40~50%。
7.根据权利要求6所述的用于制备氧传感器芯片的流延膜片的制备工艺,其特征在于,氧化铝膜片干燥后的厚度为0.7mm,氧化锆膜片干燥后的厚度为1.2mm,膜片表面平整度:±5μm。
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