CN108569895A - 一种新能源电动汽车用氧化铝陶瓷的制备方法 - Google Patents
一种新能源电动汽车用氧化铝陶瓷的制备方法 Download PDFInfo
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Abstract
本发明公开了一种新能源电动汽车用氧化铝陶瓷的制备方法,包括:A、将92.5~93.0wt%的α‑Al2O3,1~1.5wt%的高岭土,3~3.5wt%的碳酸钙,1~1.5wt%的二氧化硅、0.5~1wt%的氧化镁和0.2~1wt%的氧化锆配制成原料,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,本发明选用氧化铝陶瓷作壳体材料,进行表面二次金属化,制备的氧化铝陶瓷密度为3.76g/cm3左右,抗折强度可达310MPa以上,击穿强度约为为32kV/mm,弹性模量达282GPa以上。
Description
技术领域
本发明涉及一种新能源电动汽车用氧化铝陶瓷的制备方法。
背景技术
电子陶瓷是使陶瓷具有电、磁性质,在能源、汽车、家电等方面有着广泛的应用。随着新能源汽车行业的高速发展,新能源汽车用氧化铝陶瓷具有广阔的应用前景。氧化铝陶瓷在高频下具有优良的电气性能,其介电损耗小、体积电阻大、强度高、硬度大,而且具有良好的耐磨及耐冲击性,是常用的真空封接用电子器件陶瓷。市场上常用的氧化铝陶瓷继电器内部采用绝缘材料,外部采用金属构成壳体,其外部金属壳体采用多个分装结构组合而成,这在使用过程中很容易导致粉状结构之间组合不稳定,导致继电器损坏,严重制约着继电器的使用寿命。由于新能源汽车用陶瓷继电器壳体及密封圈形状较为复杂,采用现有的氧化铝陶瓷制备工艺易导致陶瓷的开裂、分层现象,同时由于工艺稳定性较差,易使坯体产生缺陷。抗折强度仅为280MPa。
发明内容
本发明的目的在于提供一种具有高抗折强度的新能源电动汽车用陶瓷的制备方法。
为了达到上述目的,本发明的技术解决方案为:
A、将92.5~93.0wt%的α-Al2O3,1~1.5wt%的高岭土,3~3.5wt%的碳酸钙,1~1.5wt%的二氧化硅、0.5~1wt%的氧化镁和0.2~1wt%的氧化锆配制成原料,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2.0~2.5μm;
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1.2~1.8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,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1700~1730℃,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个小时,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%。
优选地,所述球磨采用硬质合金球。
本发明的有益效果是:选用氧化铝陶瓷作壳体材料,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;采用高速搅拌球磨和球磨机球磨相结合的方式,起到节省球磨时间,节省能耗的作用,并能得到球磨粒度均匀、球形度好,细度合格的粉料;烧结时采用8个保温温区,工艺稳定性更好。采用本发明的方法制备的氧化铝陶瓷综合性能高,使用寿命长,市场竞争力强,密度为3.76g/cm3左右,抗折强度可达310MPa以上,比市面上氧化铝陶瓷的抗折强度提高30~40MPa,击穿强度约为为32kV/mm,弹性模量达282GPa以上。
具体实施方式:
实施例1:
A、将92.5wt%的α-Al2O3,1.5wt%的高岭土,3.5wt%的碳酸钙,1.5wt%的二氧化硅、0.5wt%的氧化镁和0.5wt%的氧化锆配制成原料,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2.5μm;
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1.8份、液体石蜡0.7份以及脱模剂ZUSOPLASTO59 0.2份混合均匀;
D、在110MPa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0.50小时,八温区保温4小时;
E、在振动抛光机中振磨0.5个小时,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%;
制备得到的氧化铝陶瓷密度为3.72g/cm3,抗折强度为318MPa,击穿强度为40kV/mm,弹性模量为314GPa,具有良好的抗热震性。
实施例2:
A、将93.0wt%的α-Al2O3,1wt%的高岭土,3.5wt%的碳酸钙,1.3wt%的二氧化硅、1wt%的氧化镁和0.2wt%的氧化锆配制成原料,再均匀混入占原料1wt%的PVA17-99作为粘结剂和占原料0.5wt%的正辛醇作为除泡剂;
B、球磨使得原料粒度达到2.5μm;
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1.8份、液体石蜡0.5份以及脱模剂ZUSOPLASTO59 0.8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1730℃,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3.5小时;
E、在振动抛光机中振磨0.5个小时,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%;
制备得到的氧化铝陶瓷密度为3.76g/cm3,抗折强度为310MPa,击穿强度为32kV/mm,弹性模量为282GPa,具有良好的抗热震性。
实施例3:
A、将92.8wt%的α-Al2O3,1.2wt%的高岭土,3.2wt%的碳酸钙,1.4wt%的二氧化硅、0.8wt%的氧化镁和0.6wt%的氧化锆配制成原料,再均匀混入占原料1.3wt%的PVA17-99作为粘结剂和占原料0.36wt%的正辛醇作为除泡剂;
B、球磨使得原料粒度达到2.2μm;
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1.5份、液体石蜡0.6份以及脱模剂ZUSOPLASTO59 0.7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17200℃,八温区1730℃,八个温区升温速率均为10℃/min,一至七温区保温0.9小时,八温区保温2.5小时;
E、在振动抛光机中振磨0.5个小时,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%;
制备得到的氧化铝陶瓷密度为3.70g/cm3,抗折强度为328MPa,击穿强度为42kV/mm,弹性模量为320GPa,具有良好的抗热震性。
实施例4:
A、将92.9wt%的α-Al2O3,1.2wt%的高岭土,3.1wt%的碳酸钙,1.4wt%的二氧化硅、0.9wt%的氧化镁和0.5wt%的氧化锆配制成原料,再均匀混入占原料1.4wt%的PVA17-99作为粘结剂和占原料0.42wt%的正辛醇作为除泡剂;
B、球磨使得原料粒度达到2.35μm;
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0.6份以及脱模剂ZUSOPLASTO59 0.6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1729℃,八温区1730℃,八个温区升温速率均为10℃/min,一至七温区保温0.7小时,八温区保温3.5小时;
E、在振动抛光机中振磨0.5个小时,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%;
制备得到的氧化铝陶瓷密度为3.73g/cm3,抗折强度为329MPa,击穿强度为41kV/mm,弹性模量为300GPa,具有良好的抗热震性。
本发明的实施方式并不受上述实施例的限制。其他任何未背离本发明的原理下所做的改变、修饰、替代、组合、简化,均应视为等效置换方式,都包含在本发明的保护范围之内。
Claims (2)
1.一种新能源电动汽车用氧化铝陶瓷的制备方法,其特征是,包括以下步骤:
A、将92.5~93.0wt%的α-Al2O3,1~1.5wt%的高岭土,3~3.5wt%的碳酸钙,1~1.5wt%的二氧化硅、0.5~1wt%的氧化镁和0.2~1wt%的氧化锆配制成原料,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2.0~2.5μm;
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1.2~1.8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,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1700~1730℃,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个小时,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%。
2.根据权利要求1所述的一种新能源电动汽车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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