CN110803928B - 反铁电材料体系的异质堆叠多层陶瓷电容器的制备方法 - Google Patents
反铁电材料体系的异质堆叠多层陶瓷电容器的制备方法 Download PDFInfo
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Abstract
一种基于反铁电材料体系的异质堆叠多层陶瓷电容器的制备方法,属于电子信息材料与元器件技术领域。首先,分别按照Pb(1‑1.5x)LaxZr(1‑y1‑z1)Sny1Tiz1O3和Pb(1‑1.5x)LaxZr(1‑y2‑z2)Sny2Tiz2O3的结构式,称料混料,得到粉料A和B;然后,分别将粉料A和粉料B进行球磨、烘干、预烧、二次球磨、流延,得到单层膜A和单层膜B;将单层膜A和单层膜B按照“AB”或者“ABA”的方式进行复合,作为介质层,丝网印刷金属作为电极层,制备多层陶瓷电容器。本发明得到的多层陶瓷电容器具有界面增强效应,能够有效提高击穿强度和极化强度,进而提高电容器的储能密度。
Description
技术领域
本发明属于电子信息材料与元器件技术领域,具体涉及一种异质堆叠的反铁电材料体系多层陶瓷电容器的制备方法。
背景技术
脉冲功率电容器在电磁炮、激光点火、深井探测等方面都有着重要的作用。随着科技的发展,小型化和高功率化的趋势影响越来越显著,特别是对于舰载、车载、机载甚至星载的脉冲功率系统,提出了更高更明确的需求。
传统的锆锡钛酸镧铅体系,由于具有高的轿顽场,较高的极化强度,储能密度能达到4.2J/cc,薄膜能做到几十J/cc,具有良好的应用前景。但是,锆锡钛酸镧铅反铁电材料体系具有压电特性,在充放电过程中有一定的应变产生,是电容器失效和储能密度无法进一步提高的瓶颈问题。
发明内容
本发明的目的在于,针对背景技术存在的缺陷,提出了一种基于反铁电材料体系的异质堆叠多层陶瓷电容器的制备方法。本发明得到的多层陶瓷电容器中,引入复合结构,使得两种材料的界面处形成界面效应,这种效应能够起到应变缓冲效果,增强耐压,有效提高储能密度。
为实现上述目的,本发明采用的技术方案如下:
一种基于反铁电材料体系的异质堆叠多层陶瓷电容器的制备方法,其特征在于,包括以下步骤:
步骤1、按照Pb(1-1.5x)LaxZr(1-y1-z1)Sny1Tiz1O3的结构式,称取各原料,混料,得到混合粉料A,按照Pb(1-1.5x)LaxZr(1-y2-z2)Sny2Tiz2O3的结构式,称取各原料,混料,得到混合粉料B;其中,0.01≤x≤0.1,y1≥0.3,y2≥0.3,z1≤0.1,z2≤0.1;
步骤2、将步骤1配制得到的混合粉料A和混合粉料B分别进行球磨处理,控制粒度分布符合正态分布,D90为0.1~10μm;
步骤3、将步骤2球磨处理后得到的浆料A和浆料B分别进行烘干、预烧(预烧温度为800~950℃,时间为0.5~2h)、二次球磨处理,控制粒度分布符合正态分布,D90为0.1~10μm,最后烘干;
步骤4、将步骤3处理后得到的粉料A和粉料B分别进行流延处理,得到厚度为0.5~20μm的单层膜A和单层膜B;
步骤5、将单层膜A和单层膜B按照“AB”或者“ABA”的方式进行复合,得到复合膜AB或复合膜ABA;然后以复合膜AB或者复合膜ABA作为介质层,丝网印刷金属作为电极层,按照“介质层/(电极层/介质层)n”的方式,堆叠得到多层结构电容器生坯;其中n为大于1的正整数;
步骤6、将步骤5得到的多层结构电容器生坯进行温等静压处理,温度为50~80℃,压力为20~200MPa,时间为10~120min;
步骤7、将步骤6处理后的多层结构电容器生坯放置于烧结炉中,在温度为1000~1200℃的条件下烧结0.5~2h,烧结结束后,自然冷却至室温,取出,涂端、烧银、电镀,即可得到所述多层陶瓷电容器(与传统的MLCC工艺相同)。
进一步地,步骤1中包括三种情况:y1=y2且z1≠z2,z1=z2且y1≠y2,y1≠y2且z1≠z2。
进一步地,步骤4所述流延的配方为粉料、PVB胶、分散剂、消泡剂和溶剂;所述溶剂为乙醇和甲苯的混合溶剂、异丙醇和甲苯的混合溶剂、正丁醇和醚类的混合溶剂。
进一步地,步骤5中,n个电极层中相邻电极层交错设置,每个电极层与介质层边缘预留1mm以上的距离,以防止击穿。
进一步地,步骤7得到的所述多层陶瓷电容器中,分别将靠近左侧和右侧的电极层连接并引出,作为电容器的两极。
进一步地,步骤5中,所述电极层的厚度为0.1~5μm,采用丝网印刷方法得到。
与现有技术相比,本发明的有益效果为:
本发明提供的一种基于反铁电材料体系的异质堆叠多层陶瓷电容器的制备方法,得到的多层陶瓷电容器具有界面增强效应(附图2显示),能够有效提高击穿强度和极化强度,进而提高电容器的储能密度。另外,本发明方法工艺简单,生产工艺兼容性好,利于大规模工业化生产,可广泛应用于石油勘探、地震评估、脉冲系统、新概念武器、激光点火、微雷管等领域。
附图说明
图1为本发明提供的一种基于反铁电材料体系的异质堆叠多层陶瓷电容器的制备方法流程图;
图2为本发明实施例1步骤5得到的复合膜AB烧结后的断面SEM。
具体实施方式
下面结合附图和实施例,详述本发明的技术方案。
实施例1
步骤1、按照Pb0.94 La0.04Zr0.53Sn0.4Ti0.07O3的结构式中各元素的化学计量比,称取各原料PbO、La2O3、ZrO2、SnO2、TiO2,混料,得到混合粉料A;按照Pb0.94La0.04Zr0.43Sn0.5Ti0.07O3的结构式,称取各原料PbO、La2O3、ZrO2、SnO2、TiO2,混料,得到混合粉料B;
步骤2、将步骤1配制得到的混合粉料A和混合粉料B分别进行球磨处理,控制粒度分布符合正态分布,D90为4μm;
步骤3、将步骤2球磨处理后得到的浆料A和浆料B分别进行烘干、预烧(预烧温度为800℃,时间为2h)、二次球磨处理,控制粒度分布符合正态分布,D90为4μm,最后烘干;
步骤4、将步骤3处理后得到的粉料A和粉料B分别进行流延处理,得到厚度为10μm的单层膜A和单层膜B;
步骤5、将步骤4得到的单层膜A和单层膜B按照“AB”方式进行复合,得到复合膜AB;然后以复合膜AB作为介质层,丝网印刷2μm的钯银作为电极层,按照“介质层/(电极层/介质层)4”的方式,堆叠得到多层结构电容器生坯;
步骤6、将步骤5得到的多层结构电容器生坯进行温等静压处理,温度为80℃,压力为100MPa,时间为30min;
步骤7、将步骤6处理后的多层结构电容器生坯放置于烧结炉中,在温度为1200℃的条件下烧结2h,烧结结束后,自然冷却至室温,取出,涂端、烧银、电镀,即可得到所述多层陶瓷电容器(与传统的MLCC工艺相同)。
如图2所示,为实施例1步骤5得到的复合膜AB烧结后的断面SEM(烧结温度为1000℃,时间为1h),可以看出复合膜AB有明显的界面,使得基于复合膜AB制得的电容器具有界面增强效应,能够有效提高击穿强度和极化强度,进而提高电容器的储能密度。
实施例2
本实施例与实施例1相比,区别在于:步骤1按照Pb0.97La0.02Zr0.49Sn0.45Ti0.06O3的结构式中各元素的化学计量比,称取各原料PbO、La2O3、ZrO2、SnO2、TiO2,混料,得到混合粉料A;按照Pb0.97La0.02Zr0.47Sn0.45Ti0.08O3的结构式,称取各原料PbO、La2O3、ZrO2、SnO2、TiO2,混料,得到混合粉料B;其余步骤与实施例1相同。
Claims (3)
1.一种基于反铁电材料体系的异质堆叠多层陶瓷电容器的制备方法,其特征在于,包括以下步骤:
步骤1、按照Pb(1-1.5x)LaxZr(1-y1-z1)Sny1Tiz1O3的结构式,称取各原料,混料,得到混合粉料A,按照Pb(1-1.5x)LaxZr(1-y2-z2)Sny2Tiz2O3的结构式,称取各原料,混料,得到混合粉料B;其中,0.01≤x≤0.1,y1≥0.3,y2≥0.3,z1≤0.1,z2≤0.1;
步骤2、将步骤1配制得到的混合粉料A和混合粉料B分别进行球磨处理,控制粒度分布符合正态分布,D90为0.1~10μm;
步骤3、将步骤2球磨处理后得到的浆料A和浆料B分别进行烘干、预烧、二次球磨处理,控制粒度分布符合正态分布,D90为0.1~10μm,最后烘干;所述预烧温度为800~950℃,时间为0.5~2h;
步骤4、将步骤3处理后得到的粉料A和粉料B分别进行流延处理,得到厚度为0.5~20μm的单层膜A和单层膜B;
步骤5、将单层膜A和单层膜B按照“AB”或者“ABA”的方式进行复合,得到复合膜AB或复合膜ABA;然后以复合膜AB或者复合膜ABA作为介质层,丝网印刷金属作为电极层,按照“介质层/(电极层/介质层)n”的方式,堆叠得到多层结构电容器生坯;其中n为大于1的正整数;
步骤6、将步骤5得到的多层结构电容器生坯进行温等静压处理,温度为50~80℃,压力为20~200MPa,时间为10~120min;
步骤7、将步骤6处理后的多层结构电容器生坯放置于烧结炉中,在温度为1000~1200℃的条件下烧结0.5~2h,烧结结束后,自然冷却至室温,取出,涂端、烧银、电镀,即可得到所述多层陶瓷电容器;
步骤1中包括三种情况:y1=y2且z1≠z2,z1=z2且y1≠y2,y1≠y2且z1≠z2。
2.根据权利要求1所述的基于反铁电材料体系的异质堆叠多层陶瓷电容器的制备方法,其特征在于,步骤5中,n个电极层中相邻电极层交错设置,每个电极层与介质层边缘预留1mm以上的距离。
3.根据权利要求1所述的基于反铁电材料体系的异质堆叠多层陶瓷电容器的制备方法,其特征在于,步骤5中,所述电极层的厚度为0.1~5μm,采用丝网印刷方法得到。
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