CN114213120A - 用于小尺寸mlcc的介质材料及其制备方法与电容器 - Google Patents

用于小尺寸mlcc的介质材料及其制备方法与电容器 Download PDF

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CN114213120A
CN114213120A CN202111430187.5A CN202111430187A CN114213120A CN 114213120 A CN114213120 A CN 114213120A CN 202111430187 A CN202111430187 A CN 202111430187A CN 114213120 A CN114213120 A CN 114213120A
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余强华
宋喆
虞成城
张倩
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Shenzhen Sunway Communication Co Ltd
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Abstract

本发明涉及片式多层陶瓷电容器技术领域，特别涉及用于小尺寸高容MLCC的陶瓷介质材料及其制备方法与电容器，包括将主晶相钛酸钡进行预处理的步骤；所述预处理的步骤为：将钛酸钡、碳酸氢钠、氧化锆、界面活性剂和水混合球磨6～10h后在980℃下煅烧3h。所述陶瓷介质材料包括如下质量百分数的组分：96.5～99％钛酸钡，0.1～0.5％副料，0.5～1.5％改性添加剂，0.5～1.3％掺杂剂，0.3～1.0％玻璃；所述副料包括如下质量百分数的组分：5～10％碳酸氢钠和90～95％氧化锆。本发明所提供的陶瓷介质材料可适用于制备小尺寸电容器且由该陶瓷介质材料制备得到的电容器符合X5R温度特性。

Description

用于小尺寸MLCC的介质材料及其制备方法与电容器
技术领域
本发明涉及片式多层陶瓷电容器技术领域，特别涉及一种用于小尺寸高容MLCC的陶瓷介质材料及其制备方法与电容器。
背景技术
片式多层陶瓷电容器(MLCC)是重要的电子元器件，主要用于移动电话、5G通信和汽车电子等领域，其由内电极、陶瓷层和端电极三部分组成。其中，介质材料与内电极以错位的方式堆叠后经过高温烧结烧制成块体，再在块体两端封上金属层以形成端电极。
随着电子信息产品的高速发展，MLCC朝向小尺寸、高容量、高可靠性、低成本等方向不断发展。
目前国内用于制作小尺寸高容量MLCC的纳米级BaTiO3基本从日本、美国进口，而国内生产的纳米介质材料，存在羟基残留、气孔等缺陷，掺杂改性后,介质材料介电常数低，且在与Ni电极共烧时抗还原性差等问题。
发明内容
为了克服上述现有技术的缺陷，本发明所要解决的技术问题是：提供一种羟基残留量低、气孔缺陷少且适用于小尺寸高容MLCC的陶瓷介质材料及其制备方法，以及由该陶瓷介质材料制备得到的电容器。
为了解决上述技术问题，本发明提供用于小尺寸MLCC的介质材料的制备方法，包括将主晶相钛酸钡进行预处理的步骤；
所述预处理的步骤为：将钛酸钡、碳酸氢钠、氧化锆、界面活性剂和水混合球磨6～10h后在980℃下煅烧3h。
进一步提供一种由前述制备方法制备得到的用于小尺寸MLCC的介质材料。
更进一步提供由前述用于小尺寸MLCC的介质材料制备得到的电容器。
本发明的有益效果在于：通过在对主晶相与其余改性添加剂、掺杂剂和玻璃进行混合球磨前，对主晶相进行预处理，可有效消除陶瓷介质材料残留的羟基和气孔缺陷，并且能够有效增加主晶相的抗还原性，同时可抑制晶粒生长，所制备得到的陶瓷介质材料粒度分布均匀、分散性好，适用于制备小尺寸高容MLCC。
附图说明
图1所示为本发明在检测例2中未经过预处理的陶瓷介质材料的SEM图片；
图2所示为本发明在检测例2中经过预处理的陶瓷介质材料的SEM图片。
具体实施方式
为详细说明本发明的技术内容、所实现目的及效果，以下结合实施方式并配合附图予以说明。
用于小尺寸MLCC的介质材料的制备方法，包括将主晶相钛酸钡进行预处理的步骤；
所述预处理的步骤为：将钛酸钡、碳酸氢钠、氧化锆、界面活性剂和水混合球磨6～10h后在980℃下煅烧3h。
其中，所述球磨为将物料放入球磨机中，以锆球进行研磨。
需要说明的是，在本文中，在没有特别说明的情况下，水均指代去离子水或更高纯度水。
其中，所述钛酸钡是通过水热法制备得到的，其粒径在0.12～0.15μm。
具体的，用于小尺寸MLCC的介质材料的制备方法包括如下步骤：
S1、对所述钛酸钡进行预处理，并进行微粉碎、球磨、烘干，获得粉体A；
S2、将玻璃和水进行球磨、过筛、在1250℃下煅烧至熔融后进行急冷，然后继续球磨、过筛，获得粉体B；
S3、将改性添加剂、掺杂剂、粉体A、粉体B和界面活性剂混合，以水为分散介质进行球磨10～12h、烘干后获得介电陶瓷材料。
其中，在预处理过程中的界面活性剂和S3中所添加的界面活性剂可以为相同或不同。所述界面活性剂的添加量在S3中为组合物总质量的3～5％，所述界面活性剂的添加量在预处理中添加量为组合物总质量的1～2％。
所述微粉碎用于将煅烧后轻微结块的粉体进行粉碎，并保持粉体的平均粒径在0.12～0.15μm。
用于小尺寸MLCC的介质材料，由前述用于小尺寸MLCC的介质材料的制备方法制备得到；
所述陶瓷介质材料包括如下质量百分数的组分：
96.5～99％钛酸钡，0.1～0.5％副料，0.5～1.5％改性添加剂，0.5～1.3％掺杂剂，0.3～1.0％玻璃；
所述副料包括如下质量百分数的组分：
5～10％碳酸氢钠和90～95％氧化锆。
其中，所述主晶相、副料、改性添加剂、掺杂剂和玻璃的各组成成分的纯度＞99.9％。
改性添加剂作为陶瓷介质材料的组成成分，可有效提高陶瓷介质材料的抗还原性，使陶瓷介质材料符合X5R的温度特性。
优选的，所述玻璃包括如下质量百分数的组分：
5～15％氧化硅、28～45％氧化硼、10～12％氧化铝和36～46％氧化铋。
进一步的，所述改性添加剂为镁和锰的氧化物或碳酸盐。
优选的，所述镁和锰的氧化物或碳酸盐的质量比为35～45:44～65。
进一步的，所述掺杂剂为稀土氧化物，所述稀土氧化物为镝、铈、钇、镱、钬中的至少一种。
优选的，所述掺杂剂包括质量百分数为70～100％的镝。
在一种实施方式中，所述掺杂剂由70～100％的镝的氧化物以及0～30％铈、钇、镱、钬中任一种稀土氧化物组成。
优选的，所述界面活性剂为聚丙烯酸铵盐。
一种电容器，由前述用于小尺寸MLCC的介质材料制备得到。
其中，由于制备得到的陶瓷介质材料经过预处理以及与其他组分进行混合，以使当陶瓷介质材料制备MLCC时无需经过氧化炉进行再氧化处理；并且由于陶瓷介质材料粒度分布均匀、分散性好且晶粒尺寸较小，可适用于流延处理，并经过与有机体系混合磨砂后，可通过流延工艺制备得到0.8～1.2μm的陶瓷膜片。
实施例1～9
用于小尺寸MLCC的介质材料，以100g为总重量，按如下表1配方将各组分加入球磨机中，并加入余量的聚丙烯酸铵盐和水，球磨(锆球)8h，并在空气环境下980℃煅烧3h，得粉体A-1、A-2、A-3；
表1
粉体A BaTiO<sub>3</sub>(g) NaHCO<sub>3</sub>(g) ZrO<sub>2</sub>(g)
A-1 97 0.01 0.09
A-2 98 0.03 0.27
A-3 99 0.05 0.45
按如下表2配方将各组分混合后，加入水，球磨10h后烘干，烘干完成后在1250℃下煅烧，待全部熔融后，将熔融体放入水中急冷，最后在球磨机中磨细、过筛，获得粉体B；
表2
粉体B SiO<sub>2</sub>(g) B<sub>2</sub>O<sub>3</sub>(g) Al<sub>2</sub>O<sub>3</sub>(g) Bi<sub>2</sub>O<sub>3</sub>(g)
B 15 40 10 35
按如下表3将粉体A、粉体B和其他组分进行混合，加入水和0.97～1.98g聚丙烯酸铵盐并球磨12h，烘干后获得陶瓷介质材料。
表3
Figure BDA0003379884370000051
实施例10～18
电容器，取陶瓷介质材料(实施例1～9)100g，加入无水乙醇、乙酸乙酯、PVB等有机物，在砂磨机中研磨形成稳定的浆料，采用流延机(平野R2)制作厚度为1.1～1.2μm的陶瓷膜带，然后用丝网印刷的方式将贱金属镍印刷在陶瓷膜带上，再经过叠层、温水压、切割、生晶片倒角、脱脂、烧结、Cu浆封烧端、外电极研磨，获得尺寸为英制0201的MLCC。
其中叠层层数为170～190层，脱脂分两次进行，第一次在温度210～340℃，50mm水柱压力的氮气气氛下进行，第二次在氮氢气氛(氢气相对氮气浓度为0.2％)下进行；烧结条件为：温度1180±20℃，保温0.75～2h，氮氢气氛，其中氢气相对于氮气的浓度为0.08～5％。
对比例1
用于小尺寸MLCC的介质材料，与实施例1的区别在于：A-1是未经过预处理的钛酸钡。
检测例1
对实施例10～18制备得到的电容器进行性能检测，检测结果如表4所示。
表4
Figure BDA0003379884370000061
从表4可以看出，实施例10～18所制备得到的MLCC性能优异，符合制备英制0201电容器的尺寸要求，且符合X5R温度特性。
检测例2
将实施例1和对比例2制备得到的陶瓷介质材料采用如实施例10～18中相同的工艺制备陶瓷烧成品分别进行SEM检测，结果如图1和图2所示。
从图1和图2可以看出，经过预处理的陶瓷介质材料表面气孔缺陷少，陶瓷膜带更为致密。
综上所述，通过在对主晶相与其余改性添加剂、掺杂剂和玻璃进行混合球磨前，对主晶相进行预处理，可有效消除陶瓷介质材料残留的羟基和气孔缺陷，并且能够有效增加主晶相的抗还原性，同时可抑制晶粒生长，所制备得到的陶瓷介质材料粒度分布均匀、分散性好，适用于制备小尺寸高容MLCC。
以上所述仅为本发明的实施例，并非因此限制本发明的专利范围，凡是利用本发明说明书及附图内容所作的等同变换，或直接或间接运用在相关的技术领域，均同理包括在本发明的专利保护范围内。

Claims (10)

1.用于小尺寸MLCC的介质材料的制备方法，其特征在于，包括将主晶相钛酸钡进行预处理的步骤；
所述预处理的步骤为：将钛酸钡、碳酸氢钠、氧化锆、界面活性剂和水混合球磨6～10h后在980℃下煅烧3h。
2.根据权利要求1所述用于小尺寸MLCC的介质材料的制备方法，其特征在于，包括如下步骤：
S1、对所述钛酸钡进行预处理，并进行微粉碎、球磨、烘干，获得粉体A；
S2、将玻璃和水进行球磨、过筛、在1250℃下煅烧至熔融后进行急冷，然后继续球磨、过筛，获得粉体B；
S3、将改性添加剂、掺杂剂、粉体A、粉体B和界面活性剂混合，以水为分散介质进行球磨10～12h、烘干后获得介电陶瓷材料。
3.用于小尺寸MLCC的介质材料，其特征在于，由权利要求1或2所述用于小尺寸MLCC的介质材料的制备方法制备得到；
所述陶瓷介质材料包括如下质量百分数的组分：
96.5～99％钛酸钡，0.1～0.5％副料，0.5～1.5％改性添加剂，0.5～1.3％掺杂剂，0.3～1.0％玻璃；
所述副料包括如下质量百分数的组分：
5～10％碳酸氢钠和90～95％氧化锆。
4.根据权利要求3所述用于小尺寸MLCC的介质材料，其特征在于，所述玻璃包括如下质量百分数的组分：
5～15％氧化硅、28～45％氧化硼、10～12％氧化铝和36～46％氧化铋。
5.根据权利要求3所述用于小尺寸MLCC的介质材料，其特征在于，所述改性添加剂为镁和锰的氧化物或碳酸盐。
6.根据权利要求5所述用于小尺寸MLCC的介质材料，其特征在于，所述镁和锰的氧化物或碳酸盐的质量比为35～45:44～65。
7.根据权利要求3所述用于小尺寸MLCC的介质材料，其特征在于，所述掺杂剂为稀土氧化物，所述稀土氧化物为镝、铈、钇、镱、钬中的至少一种。
8.根据权利要求3所述用于小尺寸MLCC的介质材料，其特征在于，所述掺杂剂包括质量百分数为70～100％的镝。
9.根据权利要求3所述用于小尺寸MLCC的介质材料，其特征在于，所述界面活性剂为聚丙烯酸铵盐。
10.一种电容器，其特征在于，由权利要求3～9任一项所述用于小尺寸MLCC的介质材料制备得到。
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