CN107739204B - 一种偏压特性优良的陶瓷介质材料及其制备方法 - Google Patents

一种偏压特性优良的陶瓷介质材料及其制备方法 Download PDF

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CN107739204B
CN107739204B CN201710949088.5A CN201710949088A CN107739204B CN 107739204 B CN107739204 B CN 107739204B CN 201710949088 A CN201710949088 A CN 201710949088A CN 107739204 B CN107739204 B CN 107739204B
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张军志
杨和成
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Xiamen Songyuan Electronics Co.,Ltd.
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Abstract

本发明提供一种偏压特性优良的陶瓷介质材料及其制备方法，涉及陶瓷介质技术领域。该陶瓷介质材料包括主晶相材料和改性添加物，主晶相材料的主要成分为(Ba1‑xSrx)TiO3，改性添加物包括Al2O3、MnCO3、NiO、MgO、Y2O3、Yb2O3、SiO2、Co3O4、Fe2O3中的两种或两种以上。经过合理设计配方，获得的陶瓷介质材料的介电常数介于900～1500之间，可以在1250℃～1350℃的温度范围内，与贱金属在还原气氛下烧结，用于制作MLCC产品，温度特性符合X7T要求，且满足了电容量随电压的变化量小的要求，偏压特性优良，能够应用于LED等照明灯具。

Description

一种偏压特性优良的陶瓷介质材料及其制备方法
技术领域
本发明涉及陶瓷介质领域，且特别涉及一种用于偏压特性优良的陶瓷介质材料及其制备方法。
背景技术
片式多层陶瓷电容器(MLCC)已经被广泛用作微型尺寸、高容量和高可靠性的电子元件，面临更小尺寸、更高容量、更低成本和更高可靠性的市场需求。MLCC是由印好电极(内电极)的陶瓷介质膜片以错位的方式叠合起来，经一次性高温烧结形成陶瓷芯片，再在芯片的两端封上金属层(外电极)，形成一个类似独石的结构体。适合在空气气氛中烧结的MLCC，是以贵金属钯或钯银合金做内电极；并且所用的陶瓷介质材料大多含有Pd、Cd等有害金属元素。由于贵金属价格较高，面对日益激烈的市场竞争及HSF的要求，近几年多层陶瓷电容器(MLCC)技术的发展主要集中在产品的高容量化、贱金属化、小型化及多功能化等方面。
以高介电常数陶瓷介质的多层陶瓷电容器在加载直流偏置电压时，其容量会随偏置电压的增大而下降，这种特性成为直流偏压特性，或简称偏压特性。当没有直流偏压加载时，陶瓷内部的偶极子可以自由翻转，从而介质的介电常数较大；而加载直流偏压时，直流偏压对极化机制的钳制作用使偶极子的自由翻转变得困难，介质的介电常数下降，从而电容器的容量减少。随着MLCC高容量迅速发展，介质厚度剧减，单位厚度的介质上承受的直流电压剧增，容量下降的问题日益突出。在电路应用中MLCC若不能提供足够的有效容量，就会导致储能能力下降或阻抗增大去耦效果变差等不良现象。
发明内容
本发明的目的在于提供一种偏压特性优良的陶瓷介质材料，此陶瓷介质材料以固相合成法得到的(Ba1-xSrx)TiO3为主晶相材料，并辅以一定的改性添加物，偏压特性优良，市场应用前景广阔。
本发明的另一目的在于提供一种偏压特性优良的陶瓷介质材料的制备方法，制备方法简单、易操作，适用于工业化大规模生产。
本发明解决其技术问题是采用以下技术方案来实现的。
本发明提出一种偏压特性优良的陶瓷介质材料，包括质量分数为96～98％的主晶相材料和质量分数为2～4％的改性添加物，主晶相材料的主要成分为(Ba1-xSrx)TiO3，其中，0.001≤x≤0.1，改性添加物包括Al2O3、MnCO3、NiO、MgO、Y2O3、Yb2O3、SiO2、Co3O4、Fe2O3中的两种或两种以上。
本发明提出上述的偏压特性优良的陶瓷介质材料的制备方法，包括以下步骤：将将主晶相材料和所述添加物进行湿法球磨，干燥得到陶瓷介质材料。
本发明实施例的偏压特性优良的陶瓷介质材料及其制备方法的有益效果为：
以(Ba1-xSrx)TiO3作为主晶相材料的主要成分，并通过优化改性添加物的选择和用量配比，获得陶瓷介质材料，制备过程简单，不含有毒物质，成本低廉，具有良好的分散性、均匀性和稳定性。并通过固相合成法合成(Ba1-xSrx)TiO3，并在固相合成过程中适当添加微量的辅助物，进一步对陶瓷材料的特性进行改善，获得偏压特性优良的陶瓷介质材料。该陶瓷介质材料能够在还原气氛中烧结，与铜、镍或其合金内电极匹配良好，瓷体致密，缺陷少，具有优良的介电性能。
附图说明
为了更清楚地说明本发明实施例的技术方案，下面将对实施例中所需要使用的附图作简单地介绍，应当理解，以下附图仅示出了本发明的某些实施例，因此不应被看作是对范围的限定，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他相关的附图。
图1为本发明实施例的陶瓷介质材料与对比例的陶瓷介质材料的偏压特性图。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将对本发明实施例中的技术方案进行清楚、完整地描述。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。
下面对本发明实施例偏压特性优良的陶瓷介质材料及其制备方法进行具体说明。
本发明实施例提供一种偏压特性优良的陶瓷介质材料，包括质量分数为96～98％的主晶相材料和质量分数为2～4％的改性添加物，主晶相材料的主要成分为(Ba1-xSrx)TiO3，其中，0.001≤x≤0.1，改性添加物包括Al2O3、MnCO3、NiO、MgO、Y2O3、Yb2O3、SiO2、Co3O4、Fe2O3中的两种或两种以上。
采用特殊的主晶相材料以及特定成分的辅助材料，能够对陶瓷介质材料进行有效改性，对于提高材料的偏压特性效果显著，且还能够保持陶瓷介质材料具有较高的介电常数。更为优选地，主晶相材料的主要成分(Ba1-xSrx)TiO3中，0.02≤x≤0.04。该主晶相成分能够在保证具有较高的介电常数的情况下具有更为有优良的偏压特性。
进一步地，在本发明较佳实施例中，主晶相材料通过固相合成法制备得到，包括以下步骤：按化学计量比将BaCO3、TiO2、SrCO3混合，并添加辅助物，然后经湿法球磨后在空气气氛下于1150～1250℃条件下煅烧2～4h。
进一步地，辅助物包括Ca、Sr、Zr、Ti、Y中的一种或多种元素的氧化物或碳酸盐。更为优选地，辅助物为Y2O3。更进一步地，辅助物的添加量为原料总质量的0.01～0.02％，在不影响(Ba1-xSrx)TiO3合成的情况下，在(Ba1-xSrx)TiO3中掺入微量的特定稀土氧化物。在固相合成主晶相材料的过程中，适当添加少量的辅助物，使得主晶相材料中掺有稀土氧化物，进一步改善材料的偏压特性。
进一步地，在本发明较佳实施例中，改性添加物中，各组分在所述陶瓷介质材料中的质量分数如下：Al2O3为0.0～0.8％、MnCO3为0.4～1.0％、NiO为0.0～0.2％、MgO为0.0～0.8％、Y2O3为0.0～1.2％、Yb2O3为0.0～0.4％、SiO2为0.6～1.0％、Co3O4为0.0～0.5％、Fe2O3为0.0～0.2％。
进一步地，在本发明较佳实施例中，改性添加物中，各组分在所述陶瓷介质材料中的质量分数如下：Al2O3为0.2～0.6％、MnCO3为0.4～1.0％、NiO为0.1～0.2％、MgO为0.2～0.8％、Y2O3为0.4～1.0％、Yb2O3为0.1～0.2％、SiO2为0.6～1.0％、Co3O4为0.0～0.3％、Fe2O3为0.0～0.2％。通过对改性添加物的选择和配比，能够进一步改善陶瓷介质材料的性能，特别是陶瓷介质的偏压特性。
进一步地，在本发明较佳实施例中，陶瓷介质材料在还原气氛中1250～1350℃条件下烧结制得多层陶瓷电容器，介电常数为900～1500，，且符合X7T温度特性要求。
进一步地，在本发明较佳实施例中，陶瓷介质材料陶瓷介质材料的粒径为400～800nm。该粒径下，陶瓷介质材料的分散性更好，保证制得的多层陶瓷电容器瓷体致密，缺陷少。
本发明还提供上述的偏压特性优良的陶瓷介质材料的制备方法，包括以下步骤：将主晶相材料和改性添加物进行湿法球磨，干燥得到陶瓷介质材料。
进一步地，在本发明较佳实施例中，主晶相材料根据以下步骤制备得到：按化学计量比将BaCO3、TiO2、SrCO3混合，并添加辅助物，经湿法球磨后在空气气氛下于1150～1250℃条件下煅烧2～4h。进一步地，辅助物为氧化钇。固相合成法制备工艺简单，产量大，成本低，得到的产品一致性更好，易于产生掺杂的钛酸钡粉体，产品质量更为优良。
以下结合实施例对本发明的特征和性能作进一步的详细描述。
实施例
(1)制备主晶相材料：把高纯、超细的BaCO3、SrCO3、Y2O3和TiO2按表1的组成比例置于球磨机中，湿法球磨混合均匀，在空气氛炉中1200℃的温度煅烧3小时，最终得到主要成分为(Ba1-xSrx)TiO3粉末A，其中0.001≤x≤0.1。
(2)按表2比例将主晶相材料与各种改性添加物，置于球磨机中，按重量比为物料：去离子水＝1：(0.6～1.0)的比例加入去离子水进行湿法球磨砂磨，混合均匀，砂磨至粉体平均颗粒尺寸400～800nm。砂磨完毕后用喷雾干燥塔或其他方法进行干燥，最后得到陶瓷介质材料粉末。
(3)制备陶瓷电容器试样：取上述方法获得的陶瓷介质材料粉末，按比例计算，于100g粉末中加入40-60g无水乙醇，30-45gPVB粘合剂，球磨均匀形成浆料，在经过流延获得厚度为15微米的陶瓷介质膜片生坯，用镍浆作为内电极进行叠印、等静压、切割、排胶、烧结、倒角、端铜或铜合金外部电极后得到多层陶瓷电容器；其中烧结条件是：还原气氛炉，于温度1250～1350℃烧结，保温1.5-6小时。
对比例
市售的应用于LED及节能灯上的多层陶瓷电容器。
表1主晶相材料的配比表
配方代号 BaTiO<sub>3</sub>(g) SrTiO<sub>3</sub>(g) TiO<sub>2</sub>(g) Y<sub>2</sub>O<sub>3</sub>(g)
BST1 65 1 34 0.01
BST2 64 2 34 0.01
表2陶瓷介质材料的配方表
Figure BDA0001432455300000081
表3性能测试结果表
Figure BDA0001432455300000082
如表3所示，经过上述过程制成的镍、铜内电极多层陶瓷电容器用的抗还原且偏压特性好的陶瓷介质材料，可以在1250℃～1350℃的温度范围内。通过调整材料合成的配比可形成室温介电常数介于900～1500，容量变化率介于+22％～-33％之间，符合X7T温度特性，室温介电损耗≤2.5％，连续可调系统介质陶瓷材料。以贱金属镍、铜或其合金代替贵金属银/钯电极，降低了生产成本，高介性能满足了多层陶瓷电容器抗还原且偏压特性好的要求。
此外，对比本发明实施例制得的陶瓷介质材料和对比例的陶瓷介质材料的偏压特定，结果如表4和图1所示。从图1中可以看出，本发明实施例制备得到的陶瓷介质材料的偏压特性远远优于对比例的陶瓷介质材料。
表4偏压特性对比情况表
Figure BDA0001432455300000091
以上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。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。

Claims (9)

1.一种偏压特性优良的陶瓷介质材料，其特征在于，符合X7T温度特性，包括质量分数为96～98％的主晶相材料和质量分数为2～4％的改性添加物，所述主晶相材料的主要成分为(Ba1-xSrx)TiO3，其中，0.001≤x≤0.1，所述改性添加物包括Al2O3、MnCO3、NiO、MgO、Y2O3、Yb2O3、SiO2、Co3O4、Fe2O3中的两种或两种以上；
所述改性添加物中，各组分在所述陶瓷介质材料中的质量分数如下：Al2O3为0.0～0.8％、MnCO3为0.4～1.0％、NiO为0.0～0.2％、MgO为0.0～0.8％、Y2O3为0.0～1.2％、Yb2O3为0.0～0.4％、SiO2为0.6～1.0％、Co3O4为0.0～0.5％、Fe2O3为0.0～0.2％；
所述陶瓷介质材料的制备方法为：将所述主晶相材料和所述改性添加物进行湿法球磨，干燥得到所述陶瓷介质材料。
2.根据权利要求1所述的偏压特性优良的陶瓷介质材料，其特征在于，所述主晶相材料通过固相合成法制备得到，包括以下步骤：按化学计量比将BaCO3、TiO2、SrCO3混合，并添加辅助物，然后经湿法球磨后在空气气氛下于1150～1250℃条件下煅烧2～4h。
3.根据权利要求2所述的偏压特性优良的陶瓷介质材料，其特征在于，所述辅助物包括Ca、Sr、Zr、Ti、Y中的一种或多种元素的氧化物或碳酸盐。
4.根据权利要求1所述的偏压特性优良的陶瓷介质材料，其特征在于，所述改性添加物中，各组分在所述陶瓷介质材料中的质量分数如下：Al2O3为0.2～0.6％、MnCO3为0.4～1.0％、NiO为0.1～0.2％、MgO为0.2～0.8％、Y2O3为0.4～1.0％、Yb2O3为0.1～0.2％、SiO2为0.6～1.0％、Co3O4为0.0～0.3％、Fe2O3为0.0～0.2％。
5.根据权利要求1所述的偏压特性优良的陶瓷介质材料，其特征在于，所述陶瓷介质材料在还原气氛中1250～1350℃条件下烧结制得多层陶瓷电容器，介电常数为900～1500，且符合X7T温度特性要求。
6.根据权利要求1所述的偏压特性优良的陶瓷介质材料，其特征在于，所述陶瓷介质材料的粒径为400～800nm。
7.一种如权利要求1所述的偏压特性优良的陶瓷介质材料的制备方法，其特征在于，包括以下步骤：将所述主晶相材料和所述改性添加物进行湿法球磨，干燥得到所述陶瓷介质材料。
8.根据权利要求7所述的制备方法，其特征在于，所述主晶相材料根据以下步骤制备得到：按化学计量比将BaCO3、TiO2、SrCO3混合，并添加辅助物，经湿法球磨后在空气气氛下于1150～1250℃条件下煅烧2～4h。
9.根据权利要求8所述的制备方法，其特征在于，所述辅助物为氧化钇。
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