CN108516807A - 一种汽车压力传感器用氧化铝陶瓷的制备方法 - Google Patents

一种汽车压力传感器用氧化铝陶瓷的制备方法 Download PDF

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CN108516807A
CN108516807A CN201810396729.3A CN201810396729A CN108516807A CN 108516807 A CN108516807 A CN 108516807A CN 201810396729 A CN201810396729 A CN 201810396729A CN 108516807 A CN108516807 A CN 108516807A
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方豪杰
贺亦文
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HUNAN MEICHENG CERAMIC TECHNOLOGY Co Ltd
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Abstract

本发明公开了一种汽车压力传感器用氧化铝陶瓷的制备方法，包括：A、将95～97wt％的α‑Al2O3，1～2wt％的高岭土，0.5～2wt％的碳酸钙，0.5～1wt％的二氧化硅和0.3～0.7wt％的硅酸锆配制成原料，再均匀混入PVA17‑99和正辛醇；B、球磨；C、喷雾造粒；D、干压成型，然后烧结；E、振磨；F、表面金属化等步骤，本发明采用氧化铝陶瓷作为基体；加入硅酸锆；改进球磨方式；表面二次金属化等方法，使得陶瓷成品密度达3.69g/cm3以上，弹性模量达310Gpa左右，热膨胀系数约为5x10‑6/℃(从25～500℃)，抗折强度约288Mpa。

Description

一种汽车压力传感器用氧化铝陶瓷的制备方法
技术领域
本发明涉及一种汽车压力传感器用氧化铝陶瓷的制备方法。
背景技术
现有的传感器大多是电阻应变式、硅扩散片式，多采用硅材料，存在体积大、蠕变大、抗冲击、抗过压能力较差、精度低的缺点；氧化铝陶瓷材料具备零力学滞后性能，作为传感器材料可大幅度改善蠕变性和力学滞后性。同时，氧化铝陶瓷具有极强的耐酸碱腐蚀能力，在强酸碱溶液中放置1000小时，氧化铝陶瓷的表面无任何变化，其应用领域较宽。但现有的氧化铝陶瓷制备工艺使得氧化铝陶瓷虽具有高的机械强度，但其抗折强度和断裂韧性仍然不高。因此，如何克服现有技术的不足，研发出一种高力学稳定性、高弹性模量、温度稳定性和精度的压力传感器是汽车电子元件技术领域急需解决的问题。
发明内容
本发明的目的在于提供一种高力学稳定性、高弹性模量、温度稳定性和精度的汽车压力传感器用氧化铝陶瓷的制备方法。
为了达到上述目的，本发明包括：
A、将95～97wt％的α-Al2O3，1～2wt％的高岭土，0.5～2wt％的碳酸钙，0.5～1wt％的二氧化硅和0.3～0.7wt％的硅酸锆配制成原料，再均匀混入占原料1～1.5wt％的PVA17-99作为粘结剂和占原料0.3～0.5wt％的正辛醇作为除泡剂；
B、球磨使得原料粒度达到1.3～1.8μm；
C、喷雾造粒，然后按重量将造粒粉100份、质量比为1∶2的油酸和煤油1.2～1.8份、液体石蜡0.4～0.7份以及脱模剂ZUSOPLASTO59 0.2～0.8份混合均匀；
D、在98～120MPa下干压成型，然后烧结，烧结工艺：一温区260℃，二温区430℃，三温区700℃，四温区1120℃，五温区1450℃，六温区1600℃，七温区1700～1730℃，八温区1730℃，八个温区升温速率均为10℃/min，一至七温区保温0.5～1.0小时，八温区保温2～4小时；
E、在振动抛光机中振磨0.5小时，去除产品的粘粉及毛刺；
F、表面金属化：
a、配制金属化膏剂：(1)将59～72wt％的Mo，11～15wt％的Mn，5～13wt％的Al2O3，6～12wt％的SiO2，0.5～1.0wt％的CaO，0.8～1.4wt％的TiO2烘干、球磨混合均匀后过360目筛；(2)将其与膏用添加剂按重量比(70～80)∶(20～30)混合，不断搅拌并超声分散1～2小时，其中膏用添加剂主要成分及比例：松油醇混合溶剂∶乙基纤维素＝(96～98)∶(2～4)；
b、配制辅助膏剂：(1)将88～96wt％的Mo，3～8wt％的Mn和1～4wt％的Al2O3烘干、球磨混合均匀后过360目筛；(2)将其与步骤a中膏用添加剂按重量比(70～80)∶(20～30)混合，超声分散1～2小时，期间不断搅拌；
c、一次印刷：将金属化膏剂印刷在氧化铝陶瓷上，膏剂涂层厚度为30～45μm，再烘干；
d、预烧：升温至1450℃，保温0.5～1小时，升温速度为10℃/min，随炉冷却至50～60℃；
e、二次印刷：将辅助膏剂印刷在经预烧的氧化铝陶瓷上，再烘干，经二次印刷后，膏剂涂层总厚度为52～60μm；
f、烧结：窑炉温度：一温区：1000℃，二温区：1400℃，三温区：1530℃，四温区：1550℃，四个温区升温速率10℃/min，高温保温1小时；冷却炉管温度50℃；气氛设定为：液氨分解出气口压力0.1～0.3MPa，流量3.5～5m3/h，其中湿氢占比88～92％；
G、在高精度双面平磨机上平磨，使得平面度和平行度达到0.005mm和0.01mm。
优选地，所述球磨采用硬质合金球。
本发明采用氧化铝陶瓷作为基体，具有高强度、抗磨损、耐腐蚀、无力学滞后、抗过压、抗干扰和精度高的特点。通过加入硅酸锆，起到增强增韧的效果，进一步提高制品力学性能；采用高速搅拌球磨和球磨机球磨相结合的方式，降低粉体粒度，提高粒度均匀性和球形度，从而使制品结构致密、细腻均匀，进而提高制品强度、耐化学腐蚀性和耐热性，同时起到节省球磨时间，节省能耗的作用。进行表面二次金属化，辅助膏剂对一次金属化层涂抹，锰形成的玻璃相迁移进入一次金属层，填充一次金属化层的气孔等缺陷，克服多个分装结构组合不稳定问题，实现真空封接，提高气密性及强度。采用本发明的方法制备氧化铝陶瓷，具有弹性模量高、抗压强度高、韧性好、高温蠕变小、热稳定性好的特点，用于压力传感器，工作温度范围高达-40～135℃，而且具有测量精度高，量程可以小到500Pa，抗过载能力可达量程的200倍，彻底解决了其它类型传感器没有小量程及在小量程时过载能力差的缺点。陶瓷成品密度达3.69g/cm3(25℃)以上，弹性模量达310Gpa左右，热膨胀系数约为5x10-6/℃(从25～500℃)，抗折强度约288Mpa。
具体实施方式：
实施例1：
A、将95wt％的α-Al2O3，2wt％的高岭土，2wt％的碳酸钙，0.5wt％的二氧化硅和0.5wt％的硅酸锆配制成原料，再均匀混入占原料1wt％的PVA17-99作为粘结剂和占原料0.3wt％的正辛醇作为除泡剂；
B、球磨使得原料粒度达到1.3μm；
C、喷雾造粒，然后按重量将造粒粉100份、质量比为1∶2的油酸和煤油1.2份、液体石蜡0.4份以及脱模剂ZUSOPLASTO59 0.2份混合均匀；
D、在98MPa下干压成型，然后烧结，其工艺为：一温区260℃，二温区430℃，三温区700℃，四温区1120℃，五温区1450℃，六温区1600℃，七温区1700℃，八温区1730℃，八个温区升温速率均为10℃/min，一至七温区保温0.5小时，八温区保温2小时；
E、在振动抛光机中振磨0.5小时，去除产品的粘粉及毛刺；
表面金属化：
a、配制金属化膏剂：(1)将59wt％的Mo，15wt％的Mn，13wt％的Al2O3，11wt％的SiO2，1.0wt％的CaO，1wt％的TiO2烘干、球磨混合均匀后过360目筛；(2)将其与膏用添加剂按重量比70∶30混合，不断搅拌并超声分散2小时；其中膏用添加剂主要成分及比例为松油醇混合溶剂∶乙基纤维素为96∶4；
b、配制辅助膏剂：(1)将88wt％的Mo，8wt％的Mn和4wt％的Al2O3烘干、球磨混合均匀后过360目筛；(2)将其与步骤a中膏用添加剂按重量比70∶30混合，超声分散2小时，期间不断搅拌；
c、一次印刷：将金属化膏剂印刷在氧化铝陶瓷上，膏剂涂层厚度为30μm，再烘干；
d、预烧：升温至1450℃，保温0.5小时，升温速度为10℃/min，随炉冷却至50℃；
e、二次印刷：将辅助膏剂印刷在经预烧的氧化铝陶瓷上，再烘干，经二次印刷后，膏剂涂层总厚度为52μm；
f、烧结：窑炉温度：一温区：1000℃，二温区：1400℃，三温区：1530℃，四温区：1550℃，四个温区升温速率10℃/min，高温保温1小时；冷却炉管温度50℃；气氛设定为：液氨分解出气口压力0.1MPa，流量3.5m3/h，其中湿氢占比88％；
G、在高精度双面平磨机上平磨，使得平面度和平行度达到0.005mm和0.01mm。
以上述方法制得陶瓷成品密度达3.70g/cm3(25℃)，弹性模量达320Gpa，热膨胀系数为5x10-6/℃(从25～500℃)，抗折强度290Mpa。
实施例2：
A、将97wt％的α-Al2O3，1wt％的高岭土，0.5wt％的碳酸钙，1wt％的二氧化硅和0.5wt％的硅酸锆配制成原料，再均匀混入占原料1.5wt％的PVA17-99作为粘结剂和占原料0.5wt％的正辛醇作为除泡剂；
B、球磨使得原料粒度达到1.8μm；
C、喷雾造粒，然后按重量将造粒粉100份、质量比为1∶2的油酸和煤油1.8份、液体石蜡0.7份以及脱模剂ZUSOPLASTO59 0.8份混合均匀；
D、在120MPa下干压成型，然后烧结，其工艺为：一温区260℃，二温区430℃，三温区700℃，四温区1120℃，五温区1450℃，六温区1600℃，七温区1720℃，八温区1730℃，八个温区升温速率均为10℃/min，一至七温区保温1.0小时，八温区保温4小时；
E、在振动抛光机中振磨0.5小时，去除产品的粘粉及毛刺；
表面金属化：
a、配制金属化膏剂：(1)将72wt％的Mo，11wt％的Mn，5wt％的Al2O3，10.7wt％的SiO2，0.5wt％的CaO，0.8wt％的TiO2烘干、球磨混合均匀后过360目筛；(2)将其与膏用添加剂按重量比80∶20混合，不断搅拌并超声分散1小时，其中膏用添加剂主要成分及比例为松油醇混合溶剂∶乙基纤维素＝98∶2；
b、配制辅助膏剂：(1)将96wt％的Mo，3wt％的Mn和1wt％的Al2O3烘干、球磨混合均匀后过360目筛；(2)将其与步骤a中膏用添加剂按重量比80∶20混合，超声分散1小时，期间不断搅拌；
c、一次印刷：将金属化膏剂印刷在氧化铝陶瓷上，膏剂涂层厚度为45μm，再烘干；
d、预烧：升温至1450℃，保温0.8小时，升温速度为10℃/min，随炉冷却至55℃；
e、二次印刷：将辅助膏剂印刷在经预烧的氧化铝陶瓷上，再烘干，经二次印刷后，膏剂涂层总厚度为60μm；
f、烧结：窑炉温度：一温区：1000℃，二温区：1400℃，三温区：1530℃，四温区：1550℃，四个温区升温速率10℃/min，高温保温1小时；冷却炉管温度50℃；气氛设定为：液氨分解出气口压力0.3MPa，流量5m3/h，其中湿氢占比92％；
G、在高精度双面平磨机上平磨，使得平面度和平行度达到0.005mm和0.01mm。
以上述方法制得陶瓷成品密度达3.72g/cm3(25℃)，弹性模量达319Gpa，热膨胀系数为5.2x10-6/℃(从25～500℃)，抗折强度292Mpa。
实施例3：
A、将96wt％的α-Al2O3，1.5wt％的高岭土，1.2wt％的碳酸钙，1wt％的二氧化硅和0.3wt％的硅酸锆配制成原料，再均匀混入占原料14wt％的PVA17-99作为粘结剂和占原料0.4wt％的正辛醇作为除泡剂；
B、球磨使得原料粒度达到1.5μm；
C、喷雾造粒，然后按重量将造粒粉100份、质量比为1∶2的油酸和煤油1.6份、液体石蜡0.5份以及脱模剂ZUSOPLASTO59 0.4份混合均匀；
D、在100MPa下干压成型，然后烧结，其工艺为：一温区260℃，二温区430℃，三温区700℃，四温区1120℃，五温区1450℃，六温区1600℃，七温区1700℃，八温区1730℃，八个温区升温速率均为10℃/min，一至七温区保温0.8小时，八温区保温3小时；
E、在振动抛光机中振磨0.5小时，去除产品的粘粉及毛刺；
表面金属化：
a、配制金属化膏剂：(1)将72wt％的Mo，12wt％的Mn，7.8wt％的Al2O3，6wt％的SiO2，0.8wt％的CaO，1.4wt％的TiO2烘干、球磨混合均匀后过360目筛；(2)将其与膏用添加剂按重量比75∶25混合，不断搅拌并超声分散1.5小时，其中膏用添加剂主要成分及比例为松油醇混合溶剂∶乙基纤维素＝97∶3；
b、配制辅助膏剂：(1)将92wt％的Mo，5wt％的Mn和3wt％的Al2O3烘干、球磨混合均匀后过360目筛；(2)将其与步骤a中膏用添加剂按重量比75∶25混合，超声分散1.5小时，期间不断搅拌；
c、一次印刷：将金属化膏剂印刷在氧化铝陶瓷上，膏剂涂层厚度为40μm，再烘干；
d、预烧：升温至1450℃，保温1小时，升温速度为10℃/min，随炉冷却至50℃；
e、二次印刷：将辅助膏剂印刷在经预烧的氧化铝陶瓷上，再烘干，经二次印刷后，膏剂涂层总厚度为55μm；
f、烧结：窑炉温度：一温区：1000℃，二温区：1400℃，三温区：1530℃，四温区：1550℃，四个温区升温速率10℃/min，高温保温1小时；冷却炉管温度50℃；气氛设定为：液氨分解出气口压力0.2MPa，流量4.5m3/h，其中湿氢占比90％；
G、在高精度双面平磨机上平磨，使得平面度和平行度达到0.005mm和0.01mm。
以上述方法制得陶瓷成品密度达3.70g/cm3(25℃)，弹性模量达322Gpa，热膨胀系数为5.1x10-6/℃(从25～500℃)，抗折强度289Mpa。
实施例4：
A、将96wt％的α-Al2O3，1wt％的高岭土，1.3wt％的碳酸钙，1wt％的二氧化硅和0.7wt％的硅酸锆配制成原料，再均匀混入占原料1.5wt％的PVA17-99作为粘结剂和占原料0.5wt％的正辛醇作为除泡剂；
B、球磨使得原料粒度达到1.8μm；
C、喷雾造粒，然后按重量将造粒粉100份、质量比为1∶2的油酸和煤油1.2份、液体石蜡0.5份以及脱模剂ZUSOPLASTO59 0.3份混合均匀；
D、在120MPa下干压成型，然后烧结，其工艺为：一温区260℃，二温区430℃，三温区700℃，四温区1120℃，五温区1450℃，六温区1600℃，七温区1730℃，八温区1730℃。八个温区升温速率均为10℃/min，一至七温区保温0.5小时，八温区保温2小时；
E、在振动抛光机中振磨0.5小时，去除产品的粘粉及毛刺；
F、表面金属化：
a、配制金属化膏剂：(1)将65wt％的Mo，15wt％的Mn，10wt％的Al2O3，8.7wt％的SiO2，0.5wt％的CaO，0.8wt％的TiO2烘干、球磨混合均匀后过360目筛；(2)将其与膏用添加剂按重量比80∶20混合，不断搅拌并超声分散2小时，其中膏用添加剂主要成分及比例为松油醇混合溶剂∶乙基纤维素＝96∶4；
b、配制辅助膏剂：(1)将90wt％的Mo，6wt％的Mn和4wt％的Al2O3烘干、球磨混合均匀后过360目筛；(2)将其与步骤a中膏用添加剂按重量比70∶30混合，超声分散2小时，期间不断搅拌；
c、一次印刷：将金属化膏剂印刷在氧化铝陶瓷上，膏剂涂层厚度为30μm，再烘干；
d、预烧：升温至1450℃，保温1小时，升温速度为10℃/min，随炉冷却至60℃；
e、二次印刷：将辅助膏剂印刷在经预烧的氧化铝陶瓷上，再烘干，经二次印刷后，膏剂涂层总厚度为60μm；
f、烧结：窑炉温度：一温区：1000℃，二温区：1400℃，三温区：1530℃，四温区：1550℃，四个温区升温速率10℃/min，高温保温1小时；冷却炉管温度50℃；气氛设定为：液氨分解出气口压力0.2MPa，流量5m3/h，其中湿氢占比92％；
G、在高精度双面平磨机上平磨，使得平面度和平行度达到0.005mm和0.01mm。
以上述方法制得陶瓷成品密度达3.73g/cm3(25℃)，弹性模量达324Gpa，热膨胀系数为5x10-6/℃(从25～500℃)，抗折强度294Mpa。

Claims (2)

1.一种汽车压力传感器用氧化铝陶瓷的制备方法，其特征是，包括以下步骤：
A、将95～97wt％的α-Al2O3，1～2wt％的高岭土，0.5～2wt％的碳酸钙，0.5～1wt％的二氧化硅和0.3～0.7wt％的硅酸锆配制成原料，再均匀混入占原料1～1.5wt％的PVA17-99作为粘结剂和占原料0.3～0.5wt％的正辛醇作为除泡剂；
B、球磨使得原料粒度达到1.3～1.8μm；
C、喷雾造粒，然后按重量将造粒粉100份、质量比为1∶2的油酸和煤油1.2～1.8份、液体石蜡0.4～0.7份以及脱模剂ZUSOPLASTO59 0.2～0.8份混合均匀；
D、在98～120MPa下干压成型，然后烧结，烧结工艺：一温区260℃，二温区430℃，三温区700℃，四温区1120℃，五温区1450℃，六温区1600℃，七温区1700～1730℃，八温区1730℃，八个温区升温速率均为10℃/min，一至七温区保温0.5～1.0小时，八温区保温2～4小时；
E、在振动抛光机中振磨0.5小时，去除产品的粘粉及毛刺；
F、表面金属化：
a、配制金属化膏剂：(1)将59～72wt％的Mo，11～15wt％的Mn，5～13wt％的Al2O3，6～12wt％的SiO2，0.5～1.0wt％的CaO，0.8～1.4wt％的TiO2烘干、球磨混合均匀后过360目筛；(2)将其与膏用添加剂按重量比(70～80)∶(20～30)混合，不断搅拌并超声分散1～2小时，其中膏用添加剂主要成分及比例：松油醇混合溶剂∶乙基纤维素＝(96～98)∶(2～4)；
b、配制辅助膏剂：(1)将88～96wt％的Mo，3～8wt％的Mn和1～4wt％的Al2O3烘干、球磨混合均匀后过360目筛；(2)将其与步骤a中膏用添加剂按重量比(70～80)∶(20～30)混合，超声分散1～2小时，期间不断搅拌；
c、一次印刷：将金属化膏剂印刷在氧化铝陶瓷上，膏剂涂层厚度为30～45μm，再烘干；
d、预烧：升温至1450℃，保温0.5～1小时，升温速度为10℃/min，随炉冷却至50～60℃；
e、二次印刷：将辅助膏剂印刷在经预烧的氧化铝陶瓷上，再烘干，经二次印刷后，膏剂涂层总厚度为52～60μm；
f、烧结：窑炉温度：一温区：1000℃，二温区：1400℃，三温区：1530℃，四温区：1550℃，四个温区升温速率10℃/min，高温保温1小时；冷却炉管温度50℃；气氛设定为：液氨分解出气口压力0.1～0.3MPa，流量3.5～5m3/h，其中湿氢占比88～92％；
G、在高精度双面平磨机上平磨，使得平面度和平行度达到0.005mm和0.01mm。
2.根据权利要求1所述的一种汽车压力传感器用氧化铝陶瓷的制备方法，其特征是，所述球磨采用的是硬质合金球。
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