CN114702306B - 一种95氧化铝陶瓷基片的制备方法及其产品 - Google Patents
一种95氧化铝陶瓷基片的制备方法及其产品 Download PDFInfo
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Abstract
本发明公开了一种95氧化铝陶瓷基片的制备方法及其产品。通过溶剂、分散剂、增塑剂、粘合剂和表面活性剂先混合,然后加入氧化铝和烧结助剂,继续球磨,流延、干燥,排胶,烧结等步骤得到氧化铝陶瓷基片,通过先将配料混合很好的节省了球磨时间、提高了浆料的配制效率,而且分两次球磨能够使使增塑剂能够充分地插入到粘接剂的双键中,粘接剂的双键打开较好;且表面润滑剂也均匀的分布在溶剂体系中,使得在后面加入粉体时,可有效的侵润保护粉体;而且本配制的流延浆料,在电子陶瓷生坯流延成型时不出现团聚,电子陶瓷生坯烧制好以后,产品的纹路均匀清晰,显微结构良好。
Description
技术领域
本发明属于陶瓷制备领域,具体涉及一种95氧化铝陶瓷基片的制备方法及其产品。
背景技术
陶瓷基板由于其优异的热学、力学、化学和介电性能,从而在半导体芯片封装、传感器、通讯电子、手机等智能终端、仪器仪表、新能源、新光源、汽车高铁、风力发电、机器人、航天航空和国防军工等高科技领域获得广泛的应用。在产品研发过程中突破部分关键技术,解决产业化过程中的一些技术难题,确保产品的均匀性和特异环境下的可靠性,实现产品创新及产业化。
为了获得高质量(分散均匀、致密、良好的表面光洁性及柔韧性、无针孔、重复性好)的陶瓷基片,必须使陶瓷浆料具有良好的流动性、适当的挥发速度以及在膜坯的厚度方向有足够的堆积个数,因此选择对氧化铝瓷粉及粘结剂具有良好润湿性、相容性、分散性的溶剂配方,极为重要。
周丽敏等对氧化铝浆料的稳定机制进行了总结,分析了溶剂种类、分散剂种类以及微量水的存在对氧化铝浆料稳定性的影响。于国强等研究了粉体固含量,溶剂配比,粘结剂与增塑剂比值等对氧化铝浆料黏度的影响。
上述研究仅对氧化铝浆料中单个或多个添加剂对浆料性能的影响,但是对其性能的提高并不是特别明显,而且也没有记载如何减少球磨时间,如何使得产品的纹路均匀清晰,显微结构良好,性能优异,因而急需开发一种新的制备工艺来解决上述存在的技术问题。
发明内容
本发明所要解决的技术问题在于针对上述现有技术中的不足,提供一种95氧化铝陶瓷基片的制备方法及其产品,而且本申请的制备工艺简单,具体是通过先将配料混合很好的节省了球磨时间、提高了浆料的配制效率,而且分两次球磨能够使使增塑剂能够充分地插入到粘接剂的双键中,粘接剂的双键打开较好;且表面润滑剂也均匀的分布在溶剂体系中,使得在后面加入粉体时,可有效的侵润保护粉体;而且本配制的流延浆料,在电子陶瓷生坯流延成型时不出现团聚,电子陶瓷生坯烧制好以后,产品的纹路均匀清晰,显微结构良好。
本发明采用以下技术方案:
一种95氧化铝陶瓷基片的制备方法,包括以下步骤:
(1)首先将95氧化铝(粒径为0.75μm)和烧结助剂分别进行真空干燥;所述烧结助剂为纳米MgO、纳米Ho2O3和纳米Yb2O3;
(2)将溶剂、分散剂、增塑剂、粘合剂和表面活性剂加入到球磨罐中进行球磨得到混合溶液;并通过添加氨水控制混合溶液的pH值为8~9;所述溶剂为水和乙醇混合液;所述分散剂为聚丙烯酸、蓖麻油或磷酸酯中的任意两种;所述增塑剂为丁基苄基邻苯二甲酸酯、二丁基邻苯二甲酸酯、邻苯二甲酸二辛酯中任意两种;粘合剂为羟基乙基纤维素、聚乙烯醇缩丁醛、异氰酸酯中任意两种;所述表面活性剂为非离子型辛基苯氧基乙醇;
(3)然后将步骤(1)干燥得到的粉体加入到步骤(2)得到的混合溶液中,继续球磨26~32h;然后加入消泡剂,进行真空除泡处理;
(4)然后在大型流延机上进行流延,然后在80~100℃下干燥3~4h,制备成氧化铝陶瓷生胚,然后以2~4℃的升温速率从室温升到400~600℃,保温3~4h,然后以5~8℃的升温至900~1000℃保温1~2h,然后以8~10℃升温至1550~1650℃烧结3~5h,然后随炉冷却至室温得到95氧化铝陶瓷基片;
其中,以95氧化铝粉体重量为基础计算按重量百分比加入溶剂为50~60wt%;分散剂0.5~1wt%;增塑剂为3~6wt%;粘结剂为4~6wt%;消泡剂为0.02~0.04wt%;表面活性剂为0.2~0.4wt%;所述纳米MgO 0.5~1.5wt%;所述纳米Ho2O3为0.25~0.75wt%;所述纳米Yb2O3为0.25~0.75wt%。
优选的,所述氧化铝的平均粒径为0.75μm;所述纳米MgO的粒径为10~20nm;所述纳米Ho2O3的粒径为20~50nm;所述纳米Yb2O3的粒径为20~50nm。
优选的,在步骤(1)中,所述干燥条件为在70~80℃下干燥10~12h。
优选的,在步骤(2)中,所述水和乙醇的体积比为1:1。
优选的,在步骤(2)中,所述分散剂中任意两种的重量比为1:1;所述增塑剂中任意两种的重量比为1:1;所述粘合剂中任意两种的重量比为1:1。
优选的,在步骤(2)中,所述球磨转速为200~400r/min,球磨时间为2~4h。
优选的,在步骤(3)中,所述继续球磨时间为26~32h,所述真空处理时间为20~40min。
本发明的另一个技术方案是,基于上述制备方法制备的95氧化铝陶瓷基片。
优选的,所述陶瓷基片具有以下性能参数:(1)抗折强度≥320MPa;(2)体积密度≥3.71g/cm³;(3)击穿强度≥32KV/mm;(4)体积电阻率≥1015Ω•cm;(5)线膨胀系数≤6.5×10-6•K-1;(6)介质损耗角正切值≤2×10-4。
与现有技术相比,本发明至少具有以下有益效果:
1)通过溶剂、分散剂、增塑剂、粘合剂和表面活性剂先混合,然后加入氧化铝和烧结助剂,继续球磨,流延、干燥,排胶,烧结等步骤得到氧化铝陶瓷基片,通过先将配料混合很好的节省了球磨时间、提高了浆料的配制效率,而且分两次球磨能够使使增塑剂能够充分地插入到粘接剂的双键中,粘接剂的双键打开较好;且表面润滑剂也均匀的分布在溶剂体系中,使得在后面加入粉体时,可有效的侵润保护粉体;而且本配制的流延浆料,在电子陶瓷生坯流延成型时不出现团聚,电子陶瓷生坯烧制好以后,产品的纹路均匀清晰,显微结构良好。
2)由于采用纳米MgO、纳米Ho2O3和纳米Yb2O3,相对于微米级的烧结助剂,更加能够提高氧化铝陶瓷基片的致密性,提高氧化铝陶瓷基片的综合性能,而且利用了烧结助剂三者之间的协同作用,促使了氧化铝陶瓷的致密性得到显著提高,进而提高了弯曲强度等性能。
3)通过控制排胶速率和排胶温度,使其具有良好的烧结特性,陶瓷材料的孔隙率得到进一步降低,致密性得到提高,而且通过两步煅烧促使氧化铝陶瓷基片的性能进一步得到的提高。
4)通过本申请的制备方法制备的氧化铝陶瓷基片其具有抗折强度≥320MPa;体积密度≥3.71g/cm³;击穿强度≥32KV/mm;体积电阻率≥1015Ω•cm;线膨胀系数≤6.5×10-6•K-1;介质损耗角正切值≤2×10-4,即本申请的氧化铝陶瓷基片性能优异能够满足实际生产的需求。
综上所述,本发明制备的一种氧化铝陶瓷,由于致密性好,具有较高的弯曲强度、断裂韧性和硬度,是一种用于制备阀芯瓷片的理想材料。
下面通过实施例,对本发明的技术方案做进一步的详细描述。
具体实施方式
本发明提供的一种95氧化铝陶瓷基片的制备方法,包括以下步骤:
(1)首先将95氧化铝(粒径为0.75μm)和烧结助剂分别进行真空70~80℃下干燥10~12h;所述烧结助剂为纳米MgO(粒径为10~20nm)、纳米Ho2O3(粒径为20~50nm)和纳米Yb2O3(粒径为20~50nm)。
(2)将溶剂、分散剂、增塑剂、粘合剂和表面活性剂加入到球磨罐中进行球磨得到混合溶液;所述球磨转速为200~400r/min,球磨时间为2~4h,并通过添加氨水控制混合溶液的pH值为8~9;所述溶剂为水和乙醇混合液;所述分散剂为聚丙烯酸、蓖麻油或磷酸酯中的任意两种;所述增塑剂为丁基苄基邻苯二甲酸酯、二丁基邻苯二甲酸酯、邻苯二甲酸二辛酯中任意两种;粘合剂为羟基乙基纤维素、聚乙烯醇缩丁醛、异氰酸酯中任意两种;所述表面活性剂为非离子型辛基苯氧基乙醇;所述分散剂中任意两种的重量比为1:1;所述增塑剂中任意两种的重量比为1:1;所述粘合剂中任意两种的重量比为1:1。
(3)然后将步骤(1)干燥得到的粉体加入到步骤(2)得到的混合溶液中,继续球磨26~32h;然后加入消泡剂,进行真空除泡处理;所述真空处理时间为20~40min。
(4)然后在大型流延机上进行流延,然后在80~100℃下干燥3~4h,制备成氧化铝陶瓷生胚,然后以2~4℃的升温速率从室温升到400~600℃,保温3~4h,然后以5~8℃的升温至900~1000℃保温1~2h,然后以8~10℃升温至1550~1650℃烧结3~5h,然后随炉冷却至室温得到95氧化铝陶瓷基片。
其中,以95氧化铝粉体重量为基础计算按重量百分比加入溶剂为50~60wt%;分散剂0.5~1wt%;增塑剂为3~6wt%;粘结剂为4~6wt%;消泡剂为0.02~0.04wt%;表面活性剂为0.2~0.4wt%;所述纳米MgO为0.5~1.5wt%;所述纳米Ho2O3为0.25~0.75wt%;所述纳米Yb2O3为0.25~0.75wt%。
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。通常在所示的本发明实施例的组件可以通过各种不同的配置来布置和设计。因此,以下对本发明的实施例的详细描述并非旨在限制要求保护的本发明的范围,而是仅仅表示本发明的选定实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
一种95氧化铝陶瓷基片的制备方法,包括以下步骤:
(1)首先将95氧化铝(粒径为0.75μm)和烧结助剂分别进行真空75℃下干燥11h;所述烧结助剂为纳米MgO(粒径为15nm)、纳米Ho2O3(粒径为30nm)和纳米Yb2O3(粒径为30nm)。
(2)将溶剂、分散剂、增塑剂、粘合剂和表面活性剂加入到球磨罐中进行球磨得到混合溶液;所述球磨转速为300r/min,球磨时间为3h,并通过添加氨水控制混合溶液的pH值为9;所述溶剂为水和乙醇混合液;所述分散剂为聚丙烯酸和磷酸酯;所述增塑剂为丁基苄基邻苯二甲酸酯和邻苯二甲酸二辛酯;粘合剂为羟基乙基纤维素和聚乙烯醇缩丁醛;所述表面活性剂为非离子型辛基苯氧基乙醇;所述聚丙烯酸和磷酸酯的重量比为1:1;所述丁基苄基邻苯二甲酸酯和邻苯二甲酸二辛酯的重量比为1:1;所述羟基乙基纤维素和聚乙烯醇缩丁醛的重量比为1:1。
(3)然后将步骤(1)干燥得到的粉体加入到步骤(2)得到的混合溶液中,继续球磨30h;然后加入消泡剂,进行真空除泡处理;所述真空处理时间为30min。
(4)然后在大型流延机上进行流延,然后在90℃下干燥4h,制备成氧化铝陶瓷生胚,然后以3℃的升温速率从室温升到550℃,保温4h,然后以6℃的升温至950℃保温2h,然后以9℃升温至1600℃烧结4h,然后随炉冷却至室温得到95氧化铝陶瓷基片。
其中,以95氧化铝粉体重量为基础计算按重量百分比加入溶剂为55wt%;分散剂0.75wt%;增塑剂为5wt%;粘结剂为5wt%;消泡剂为0.03wt%;表面活性剂为0.3wt%;所述纳米MgO为1wt%;所述纳米Ho2O3为0.5wt%;所述纳米Yb2O3为0.5wt%。
实施例2
一种95氧化铝陶瓷基片的制备方法,包括以下步骤:
(1)首先将95氧化铝(粒径为0.75μm)和烧结助剂分别进行真空80℃下干燥10h;所述烧结助剂为纳米MgO(粒径为10nm)、纳米Ho2O3(粒径为50nm)和纳米Yb2O3(粒径为20nm)。
(2)将溶剂、分散剂、增塑剂、粘合剂和表面活性剂加入到球磨罐中进行球磨得到混合溶液;所述球磨转速为400r/min,球磨时间为2h,并通过添加氨水控制混合溶液的pH值为8;所述溶剂为水和乙醇混合液;所述分散剂为聚丙烯酸和蓖麻油;所述增塑剂为丁基苄基邻苯二甲酸酯和二丁基邻苯二甲酸酯;粘合剂为聚乙烯醇缩丁醛和异氰酸酯;所述表面活性剂为非离子型辛基苯氧基乙醇;所述聚丙烯酸和蓖麻油的重量比为1:1;所述丁基苄基邻苯二甲酸酯和二丁基邻苯二甲酸酯的重量比为1:1;所述聚乙烯醇缩丁醛和异氰酸酯的重量比为1:1。
(3)然后将步骤(1)干燥得到的粉体加入到步骤(2)得到的混合溶液中,继续球磨32h;然后加入消泡剂,进行真空除泡处理;所述真空处理时间为20min。
(4)然后在大型流延机上进行流延,然后在100℃下干燥3h,制备成氧化铝陶瓷生胚,然后以4℃的升温速率从室温升到600℃,保温3h,然后以8℃的升温至900℃保温2h,然后以10℃升温至1650℃烧结3h,然后随炉冷却至室温得到95氧化铝陶瓷基片。
其中,以95氧化铝粉体重量为基础计算按重量百分比加入溶剂为60wt%;分散剂1wt%;增塑剂为3wt%;粘结剂为6wt%;消泡剂为0.04wt%;表面活性剂为0.2wt%;所述纳米MgO为0.5wt%;所述纳米Ho2O3为0.75wt%;所述纳米Yb2O3为0.25wt%。
实施例3
一种95氧化铝陶瓷基片的制备方法,包括以下步骤:
(1)首先将95氧化铝(粒径为0.75μm)和烧结助剂分别进行真空70℃下干燥12h;所述烧结助剂为纳米MgO(粒径为20nm)、纳米Ho2O3(粒径为20nm)和纳米Yb2O3(粒径为50nm)。
(2)将溶剂、分散剂、增塑剂、粘合剂和表面活性剂加入到球磨罐中进行球磨得到混合溶液;所述球磨转速为200r/min,球磨时间为4h,并通过添加氨水控制混合溶液的pH值为9;所述溶剂为水和乙醇混合液;所述分散剂为蓖麻油和磷酸酯;所述增塑剂为二丁基邻苯二甲酸酯和邻苯二甲酸二辛酯;粘合剂为羟基乙基纤维素和异氰酸酯;所述表面活性剂为非离子型辛基苯氧基乙醇;所述蓖麻油和磷酸酯的重量比为1:1;所述二丁基邻苯二甲酸酯和邻苯二甲酸二辛酯的重量比为1:1;所述羟基乙基纤维素和异氰酸酯的重量比为1:1。
(3)然后将步骤(1)干燥得到的粉体加入到步骤(2)得到的混合溶液中,继续球磨26h;然后加入消泡剂,进行真空除泡处理;所述真空处理时间为20min。
(4)然后在大型流延机上进行流延,然后在80℃下干燥4h,制备成氧化铝陶瓷生胚,然后以2℃的升温速率从室温升到600℃,保温3h,然后以8℃的升温至1000℃保温1h,然后以8℃升温至1550℃烧结5h,然后随炉冷却至室温得到95氧化铝陶瓷基片。
其中,以95氧化铝粉体重量为基础计算按重量百分比加入溶剂为50wt%;分散剂0.5wt%;增塑剂为6wt%;粘结剂为4wt%;消泡剂为0.02wt%;表面活性剂为0.4wt%;所述纳米MgO为0.5wt%;所述纳米Ho2O3为0.25wt%;所述纳米Yb2O3为0.75wt%。
对比例1
将步骤(2)中的原料和氧化铝粉体和烧结助剂直接混合,球磨时间为34h,其它制备过程和条件均与实施例1相同。
对比例2
烧结助剂的粒径均为1μm,其它制备过程和条件均与实施例1相同。
对比例3
增塑剂仅为丁基苄基邻苯二甲酸酯,其含量为5wt%;其它制备过程和条件均与实施例1相同。
对比例4
增塑剂仅为邻苯二甲酸二辛酯,其含量为5wt%;其它制备过程和条件均与实施例1相同。
对比例5
烧结助剂为纳米MgO(粒径为15nm)、纳米Ho2O3(粒径为30nm),其中所述纳米MgO 为1wt%;所述纳米Ho2O3为1wt%;其它制备过程和条件均与实施例1相同。
对比例6
烧结助剂为纳米MgO(粒径为15nm)、纳米Yb2O3(粒径为30nm),其中所述纳米MgO1wt%;所述纳米Yb2O3为1wt%;其它制备过程和条件均与实施例1相同。
对比例7
烧结助剂为纳米MgO(粒径为15nm),其中所述纳米MgO 2wt%;其它制备过程和条件均与实施例1相同。
对比例8
烧结助剂为纳米Yb2O3(粒径为30nm),其中所述纳米Yb2O3为2wt%;其它制备过程和条件均与实施例1相同。
对比例9
烧结助剂为纳米Ho2O3(粒径为30nm),其中所述纳米Ho2O3为2wt%;其它制备过程和条件均与实施例1相同。
对比例10
(4)然后在大型流延机上进行流延,然后在90℃下干燥4h,制备成氧化铝陶瓷生胚,然后以3℃的升温速率从室温升到550℃,保温4h,然后以9℃升温至1600℃烧结6h,然后随炉冷却至室温得到95氧化铝陶瓷基片,其它步骤和条件与实施例1相同。
将实施例1-3和对比例1-10的95氧化铝陶瓷基片按照国标GB/T14619-2013进行测试,具体结果见表1。
表1 实施例1-3和对比例1-11的性能参数
综上所述,本发明制备的95氧化铝陶瓷基片,制备方法简单,而且通过实施例1和对比例1-10的对比例可以发现,通过控制物料混合顺序、添加适宜的增塑剂和特定配比的烧结助剂以及两端煅烧可以很好的促使了氧化铝陶瓷的致密性得到提高,进而提高了95氧化铝陶瓷基片的综合性能。
以上内容仅为说明本发明的技术思想,不能以此限定本发明的保护范围,凡是按照本发明提出的技术思想,在技术方案基础上所做的任何改动,均落入本发明权利要求书的保护范围之内。
Claims (9)
1.一种95氧化铝陶瓷基片的制备方法,其特征在于:包括以下步骤:
(1)首先将95氧化铝和烧结助剂分别进行真空干燥;所述烧结助剂为纳米MgO、纳米Ho2O3和纳米Yb2O3;
(2)将溶剂、分散剂、增塑剂、粘合剂和表面活性剂加入到球磨罐中进行球磨得到混合溶液;并通过添加氨水控制混合溶液的pH值为8~9;所述溶剂为水和乙醇混合液;所述分散剂为聚丙烯酸、蓖麻油或磷酸酯中的任意两种;所述增塑剂为丁基苄基邻苯二甲酸酯、二丁基邻苯二甲酸酯、邻苯二甲酸二辛酯中任意两种;粘合剂为羟基乙基纤维素、聚乙烯醇缩丁醛、异氰酸酯中任意两种;所述表面活性剂为非离子型辛基苯氧基乙醇;
(3)然后将步骤(1)干燥得到的粉体加入到步骤(2)得到的混合溶液中,继续球磨26~32h;然后加入消泡剂,进行真空除泡处理;
(4)然后在大型流延机上进行流延,然后在80~100℃下干燥3~4h,制备成氧化铝陶瓷生胚,然后以2~4℃的升温速率从室温升到400~600℃,保温3~4h,然后以5~8℃的升温至900~1000℃保温1~2h,然后以8~10℃升温至1550~1650℃烧结3~5h,然后随炉冷却至室温得到95氧化铝陶瓷基片;
其中,以95氧化铝粉体重量为基础计算按重量百分比加入溶剂为50~60wt%;分散剂0.5~1wt%;增塑剂为3~6wt%;粘结剂为4~6wt%;消泡剂为0.02~0.04wt%;表面活性剂为0.2~0.4wt%;所述纳米MgO 0.5~1.5wt%;所述纳米Ho2O3为0.25~0.75wt%;所述纳米Yb2O3为0.25~0.75wt%。
2.根据权利要求1所述的制备方法,其特征在于:所述氧化铝的粒径为0.75μm;所述纳米MgO的粒径为10~20nm;所述纳米Ho2O3的粒径为20~50nm;所述纳米Yb2O3的粒径为20~50nm。
3.根据权利要求1所述的制备方法,其特征在于:在步骤(1)中,所述干燥条件为在70~80℃下干燥10~12h。
4.根据权利要求1所述的制备方法,其特征在于:在步骤(2)中,所述水和乙醇的体积比为1:1。
5.根据权利要求1所述的制备方法,其特征在于:在步骤(2)中,所述分散剂中任意两种的重量比为1:1;所述增塑剂中任意两种的重量比为1:1;所述粘合剂中任意两种的重量比为1:1。
6.根据权利要求1所述的制备方法,其特征在于:在步骤(2)中,所述球磨转速为200~400r/min,球磨时间为2~4h。
7.根据权利要求1所述的制备方法,其特征在于:在步骤(3)中,所述继续球磨时间为26~32h,所述真空处理时间为20~40min。
8.根据权利要求1-7任一项所述的制备方法制备的95氧化铝陶瓷基片。
9.根据权利要求8所述的95氧化铝陶瓷基片,其特征在于:所述陶瓷基片具有以下性能参数:(1)抗折强度≥320MPa;(2)体积密度≥3.71g/cm³;(3)击穿强度≥32kV/mm;(4)体积电阻率≥1015Ω•cm;(5)线膨胀系数≤6.5×10-6•K-1;(6)介质损耗角正切值≤2×10-4。
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