CN110922186B - 一种中低温烧结高介电常数陶瓷介质材料及其制备方法 - Google Patents

一种中低温烧结高介电常数陶瓷介质材料及其制备方法 Download PDF

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CN110922186B
CN110922186B CN201911258099.4A CN201911258099A CN110922186B CN 110922186 B CN110922186 B CN 110922186B CN 201911258099 A CN201911258099 A CN 201911258099A CN 110922186 B CN110922186 B CN 110922186B
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仪凯
张庆猛
陈均优
杨志民
杨剑
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Abstract

本发明公开了属于电子材料制造技术领域的一种中低温烧结(烧结温度为900℃‑1200℃)高介电常数陶瓷材料及其制备方法。配方组成为：aBaO‑bMgO‑cAl2O3‑dTiO2‑eSiO2‑fNb2O5‑gSrO‑hPbO，其中的a、b、c、d、e、f、g、h表示各成分的摩尔比例，分别为：2≤a≤15，2≤b≤5，0≤c≤10，4≤d≤16，5≤e≤45，20≤f≤55，16≤g≤27，3≤h≤25。将原料混合均匀，高温熔融、搅拌，形成均匀的液体；将熔融液快速倒入去离子水中，得到玻璃渣；将玻璃渣球磨、烘干、过筛、造粒后，压制成型为坯体，再将坯体于900℃‑1200℃烧结，保温3小时，制得陶瓷电容器介质材料，该介质材料适用于单片陶瓷电容器和多层片式陶瓷电容器。

Description

一种中低温烧结高介电常数陶瓷介质材料及其制备方法
技术领域
本发明涉及一种应用于电子元器件的陶瓷材料及其制造方法，具体涉及一种中低温烧结、用于MLCC的高介电常数介质陶瓷材料及其制备方法。
背景技术
电子信息材料是电子材料及精细化工结合的技术产品，是汽车电子、消费电子、家用电器、信息通讯、航空航天、军工等领域发展的基础。电子信息材料的生产质量、技术创新及技术进步，直接影响了电子元器件及电子整机产品的升级换代水平及速度。
片式多层陶瓷电容器(MLCC)是目前用量最大、发展速度最快的片式元器件之一。目前MLCC行业最核心的主要是电介质陶瓷粉料的材料技术、介质薄层化技术、共烧技术等。从根本上可以归结为增大容量、降低成本两个方面。大容量的发展需求使得介质层数在不断增加的同时，介质层的厚度也在不断减薄，这意味电介质材料需要具有较高的介电常数；向着低成本方向发展，则要求降低制备介质陶瓷时的烧结温度来匹配廉价金属电极。
发明内容
本发明的目的在于提出一种具有较高介电常数、较低烧结温度且较小的介电常数温度系数电介质陶瓷。
本发明另一目的在于提供上述介电陶瓷的制备方法。
本发明的目的通过以下技术方案实现：
一种中低温烧结的高介电常数电介质陶瓷，其介质配方为：aBaO-bMgO-cAl2O3-dTiO2-eSiO2-fNb2O5-gSrO-hPbO，其中的a、b、c、d、e、f、g、h表示各成分的摩尔比例，分别为：2≤a≤15，2≤b≤5，0≤c≤10，4≤d≤16，5≤e≤45，20≤f≤55，16≤g≤27，3≤h≤25。
中低温烧结的高介电常数电介质陶瓷的制备方法：将BaCO3、MgO、Al2O3、TiO2、SiO2、Nb2O5、SrCO3、PbO按摩尔比配料，利用翻转混料机将原料混合3-5h个小时，然后将混合均匀的料在1400℃-1500℃保温5h-8h，形成玻璃液，快速倒入去离子水中得到玻璃渣。将制备的玻璃渣进行行星球磨，球磨速率为50-200r/min，球磨时间为8-24h。烘干，然后过200目的筛子，取筛下粉体进行下一步工序。将制备好的粉体经过造粒、单轴加压、冷等静压(压制压力为180MPa-200MPa)压制成直径为20mm±0.5mm，厚度为2mm±0.1mm的试样，在空气气氛中，900℃-1200℃烧结2h-5h，制得陶瓷样品。
所述的行星球磨所用球磨罐的材质是聚四氟乙烯，球磨介质为3mm-10mm的二氧化锆球，溶剂为去离子水，其中球：粉：水＝(1-3):(1.5-4):(2-3)。
所用的粘结剂为0.5wt％PVA-0.8wt％PVA溶液。
与现有技术相比，本发明的优点是：
本发明的烧结温度较低，开发低成本高介电常数低介电损耗的多层陶瓷电容器材料。
具体实施方式
下面通过具体的实施案例，进一步阐述本发明。
实施例1-12：
选择分析纯的BaCO3、MgO、Al2O3、TiO2、SiO2、Nb2O5、SrCO3、PbO为原料，按照表1中的摩尔比例分别进行配料，利用翻转混料机将原料混合3个小时，然后将混合均匀的料在1430℃保温5h，形成玻璃液，快速倒入去离子水中得到玻璃渣。将制备的玻璃渣进行行星球磨，球磨速率为150r/min，球磨时间为24h。(球磨介质为3mm的二氧化锆球，溶剂为去离子水，其中球：粉：水＝1:1.5:2烘干，然后过200目的筛子，取筛下粉体进行下一步工序。将制备好的粉体添加0.5wt％PVA溶液造粒、单轴加压、冷等静压(压制压力为200MPa)压制成直径为20mm，厚度为2mm的试样，在空气气氛中，900℃-1200℃烧结2h，制得陶瓷样品。
表1
Figure BDA0002310869580000031
样品的电极为纯银，采用丝网印刷工艺，在600℃保温30min，烧结陶瓷介电性能测试采用Agilent4282A，测试频率为1kHz。测试的温度范围为-55℃-125℃。测试结果如表2所示。
表2
样品标号 介电常数 介电损耗 介电常数温度系数ppm/℃
1 402 0.0002 -789
2 489 0.0007 -327
3 534 0.0006 -500
4 895 0.0021 -657
5 956 0.0018 -275
6 1030 0.0024 -538
7 1150 0.0036 -705
8 1235 0.0045 -298
9 1289 0.0056 -589
10 1352 0008 -459
11 1458 0.002 -387
12 1438 0.005 -608

Claims (5)

1.一种中低温烧结高介电常数陶瓷介质材料，其特征在于，所述陶瓷介质材料的配方组成为：aBaO-bMgO-cAl2O3-dTiO2-eSiO2-fNb2O5-gSrO-hPbO，其中的a、b、c、d、e、f、g、h表示各成分的摩尔比例，其数值范围为：2≤a≤15，2≤b≤5，0≤c≤10，4≤d≤16，5≤e≤45，20≤f≤55，16≤g≤27，3≤h≤25。
2.一种制备权利要求1所述的中低温烧结高介电常数陶瓷介质材料的方法，其特征在于，具体步骤如下：
（1）将BaCO3、MgO、Al2O3、TiO2、SiO2、Nb2O5、SrCO3、PbO按摩尔比配料，利用翻转混料机将原料混合3-5h个小时；
（2）将步骤（1）得到的混合料在1400℃-1500℃保温5h-8h，形成玻璃液，快速倒入去离子水中得到玻璃渣；
（3）将步骤（2）制备的玻璃渣进行行星球磨，球磨速率为50-200r/min，球磨时间为8~24h；
（4）将步骤（3）得到的粉体进行烘干，并将粉体过200目的筛子，取筛下粉末进行下一步工序；
（5）将步骤（4）得到的筛下粉末加入粘结剂进行造粒、单轴加压、冷等静压压制成直径为20mm±0.5mm，厚度为2mm±0.1mm的试样，在空气气氛中，900℃-1200℃烧结2h-5h，制得中低温烧结高介电常数陶瓷介质材料。
3.根据权利要求2所述的方法，其特征在于球磨介质为3mm-10mm的二氧化锆球，溶剂为去离子水，其中，球：粉：水=(1-3):(1.5-4):(2-3)。
4.根据权利要求2所述的方法，其特征在于，冷等静压压制压力为180MPa-200MPa。
5.根据权利要求2所述的方法，其特征在于，所用的粘结剂为0.5wt% -0.8wt%的PVA溶液。
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