CN106699150B - 一种低温烧结低介c0g微波介质材料及其制备方法 - Google Patents

一种低温烧结低介c0g微波介质材料及其制备方法 Download PDF

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CN106699150B
CN106699150B CN201710019409.1A CN201710019409A CN106699150B CN 106699150 B CN106699150 B CN 106699150B CN 201710019409 A CN201710019409 A CN 201710019409A CN 106699150 B CN106699150 B CN 106699150B
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宋蓓蓓
程华容
杨魁勇
齐世顺
杨喻钦
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Beijing Yuan Six Hongyuan Electronic Polytron Technologies Inc
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Abstract

本发明涉及微波介质材料技术领域，具体涉及一种低温烧结低介电常数C0G特性微波介质材料，主料为BaSi2O5；副料为Zn2SiO4；改性添加剂为Al2O3、MnO、CeO2、CoO、Nb2O5、ZrO2的一种或多种；烧结助剂为B2O3、SiO2、ZnO、Li2CO3、MgO中的一种或多种。能够在较低温度(850～950℃)下烧结，陶瓷粉具备成分均一、粒度分布窄、分散性好、成型性工艺好，烧结后瓷体致密、无杂质和缺陷少，其相对介电常数在10±2系列变化、室温损耗角正切＜4×10‑4、绝缘电阻>1×1012Ω、容量温度特性稳定、品质因数Q·f值高。

Description

一种低温烧结低介C0G微波介质材料及其制备方法
技术领域
本发明涉及微波介质材料技术领域，具体涉及一种低温烧结低介C0G微波介质材料及其制备方法。
背景技术
近年来，随着微波通讯技术的发展，对元器件的小型化、集成化以及模块化的要求也越来越迫切。低温共烧陶瓷LTCC以其优异的电学、机械、热学及工艺特性，已经成为电子器件模块化的主要技术之一，要实现无源元件的集成化、模块化，必须开发新的LTCC材料体系。LTCC技术必须满足以下几点要求：
首先烧结温度要低于960℃以便与银电极共烧，拥有一个低的介电常数避免信号传输延迟，其次需要拥有高的Q·f值以便满足工作频率的要求，最后温度系数要接近于0实现系数的稳定性。
射频微波多层片式电容器广泛应用于移动通讯的基站，直放站，军用电台、雷达，广播电视发射机，MRI磁共振医疗设备，大功率激光设备，同步加速器，高速铁路应答等设备，设备、微波多层片式瓷介电容器的特点是高Q值、低ESR、高FER(自谐振频率)、高可靠。
通常εr、Q·f和τf之间存在一定相互制约关系，高介电常数与高Q·f和低τf是相互矛盾的，器件的小型化要求材料的介电常数能够提高，材料的Q·f值将会降低，τf绝对值也会随之而增大。电容器的损耗由两部分组成，即介质损耗和金属损耗。30MHz以下介质损耗占主导地位，30MHz以上由于“趋肤效应”金属损耗变大，逐渐占主导地位。为了获得高频下更低的ESR，必须降低金属损耗，因此现在开始采用方阻更低的Ag或Cu作内部电极材料，由于Ag的熔点低(961℃)，必须要求陶瓷的烧结温度降低到950℃以下。因此低温烧结的高Q值、低介电常数介质材料成为材料研发工作者的一个热点研发方向。
发明内容
针对上述问题中存在的不足之处，本发明提供一种低温烧结低介电常数C0G特性微波介质材料。
为实现上述目的，本发明提供一种低温烧结低介电常数C0G特性微波介质材料，包括：主料、副料、改性添加剂和烧结助剂；其中，
所述主料为BaSi2O5；
所述副料为Zn2SiO4；
所述改性添加剂为Al2O3、MnO、CeO2、CoO、Nb2O5、ZrO2的一种或多种；
所述烧结助剂为B2O3、SiO2、ZnO、Li2CO3、MgO中的一种或多种。
上述的低温烧结低介电常数C0G特性微波介质材料中，优选为，各成分摩尔份数为：
所述BaSi2O5为65～85份；
所述Zn2SiO4为2～10份；
所述Al2O3为0～4份；
所述MnO为0.1～0.5份；
所述CeO2为0～0.5份；
所述CoO为0.1～1份；
所述Nb2O5为0～5份；
所述ZrO2为0～4份；
所述烧结助剂共6～20份。
上述的低温烧结低介电常数C0G特性微波介质材料中，优选为，各成分摩尔份数为：
所述BaSi2O5为70～75份；
所述Zn2SiO4为4～8份；
所述Al2O3为2份；
所述MnO为0.3份；
所述CeO2为0.3份；
所述CoO为0.5份；
所述Nb2O5为2份；
所述ZrO2为2份；
所述烧结助剂共10～15份。
一种低温烧结低介电常数C0G特性微波介质材料的制备方法，包括如下步骤：
将BaO的前驱体、SiO2的前驱体按比例混合，进行球磨、烘干、过筛后在1000℃～1100℃煅烧2.5～5小时后获得BaSi2O5；
将ZnO的前驱体、SiO2的前驱体按比例混合，进行球磨、烘干、过筛后在1150℃～1250℃煅烧2.5～5小时后获得Zn2SiO4；
所述BaSi2O5与所述Zn2SiO4，所述Al2O3、所述MnO、所述CeO2、所述CoO、所述Nb2O5、所述ZrO2的一种或多种，由所述B2O3、所述SiO2、所述ZnO、所述Li2CO3、所述MgO中的一种或多种，按比例混合、球磨、烘干、过筛后获得微波介质材料；
将微波介质材料造粒后在4～6MPa压力下制成坯体，再将坯体排胶，排胶温度为500℃、升温速率为2℃/min、保温1小时，再以3～8℃/min升温至850～950℃对排胶后的坯体进行烧结保温2～5小时后随炉自然冷却。
上述的低温烧结低介电常数C0G特性微波介质材料的制备方法中，优选为，
所述BaO的前驱体为BaO、Ba(OH)2、BaCO3中的一种或多种；
所述SiO2的前驱体为SiO2、H2SiO3中的一种或两种；
所述ZnO的前驱体为ZnO、Zn(OH)2、ZnCO3中的一种或多种。
上述的C0G微波介质材料的制备方法中，优选为，
将所述B2O3、所述SiO2、所述ZnO、所述Li2CO3、所述MgO中的一种或多种按比例混合，进行球磨、烘干、过筛后在500～700℃煅烧2.5～5小时后获得烧结助剂。
在上述技术方案中，本发明实施例提供的低温烧结低介电常数C0G特性微波介质材料及制备方法，与现有技术相比具有以下优点：
1、能够在较低温度(850～950℃)下烧结，陶瓷粉具备成分均一、粒度分布窄、分散性好、成型性工艺好，烧结后瓷体致密、无杂质和少缺陷，其相对介电常数在8～12系列变化、室温损耗角正切＜4×10-4、绝缘电阻>1×1012Ω、在-55～125℃范围内电容温度系数为0±30ppm/℃、容量温度特性稳定、品质因数Q·f值很高。
2、此C0G微波介质材料制备方法及工艺简单、设备成熟及投入成本较低、易于实现工业化生产，可快捷、稳定实现从材料配方向微波介质材料产品批量生产转化。
具体实施方式
下面结合具体实施方式对本发明做进一步说明。应该强调的是，下述说明仅仅是示例性的，而不是为了限制本发明的范围及其应用。
(1)主料的制备
主料BaSi2O5的制备方法：将纯度均为99.0％以上的BaCO3 0.1mol、SiO20.2mol混合，加入氧化锆球和去离子水进行球磨混合，球磨时间8小时，在120℃烘5小时至干燥，过40目筛后，在1050±50℃煅烧混合物2.5h，即得主成分BaSi2O5。
(2)副料的制备
副料Zn2SiO4的制备方法：将纯度均为99.0％以上的ZnO 0.2mol、SiO20.1mol混合，加入氧化锆球和去离子水进行球磨混合，球磨时间8小时，在120℃烘5小时至干燥，过40目筛后，在1200±50℃煅烧混合物2.5h，即得主成分Zn2SiO4。
(3)烧结助剂的制备
LBS烧结助剂的制备方法：按质量比例为1.5:1:1称取原料Li2CO3、H3BO3、SiO2混合，加入氧化锆球进行球磨，球磨时间为6小时，在80℃烘10小时至干燥，过100目筛后，在600℃煅烧4小时后获得。
LMZBS烧结助剂的制备方法：按质量比例为2.5:2.5:2:1:1称取原料Li2CO3、Mg(OH)2、H3BO3、ZnO、SiO2混合，加入氧化锆球进行球磨，球磨时间为6小时，在80℃烘10小时至干燥，过100目筛后，在560℃煅烧4小时后获得。
(4)配方设计及圆片性能
本低温烧结C0G特性微波介质材料配方如表1所示，按设计比例在主/副料中添加烧结助剂和改性添加剂，加入氧化锆球进行球磨，球磨时间为5小时，在120℃烘6小时至干燥，过100目筛后获得。
微波介质陶瓷材料的制备：将微波介质材料加入6.5wt％的PVA(聚乙烯醇)水溶液粘合造粒；分别在4Mpa和6MPa压力下压制成圆片和圆柱坯体，将坯体排胶，排胶温度为500℃、升温速率为2℃/min、保温1小时，去除粘合剂；将排胶后的坯体在850～950℃下烧结，保温2～5小时，随炉自然冷却降至室温，制得微波介质陶瓷材料。
将烧制完的圆片两表面涂覆银浆、烧制银电极，制成电容器后测试其室温电学性能，结果见表2：相对介电常数10±2，损耗角正切＜4×10-4，绝缘电阻>1×1012Ω，在-55～125℃范围内电容温度系数为-30～30ppm/℃。
所述圆柱样品的直径为8.4±0.5mm，厚度为5.0±1.0mm，圆柱样品的Q·f值为18296～38157GHz。
表1低温烧结C0G特性微波介质材料配方(mol％)
表2微波介质陶瓷材料的性能
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (4)

1.一种低温烧结低介电常数C0G特性微波介质材料，其特征在于，包括：主料、副料、改性添加剂和烧结助剂；其中，
所述主料BaSi2O5为65～85份；
所述副料Zn2SiO4为2～10份；
所述改性添加剂为Al2O3 0～4份、MnO 0.1～0.5份、CeO2 0～0.5份、CoO 0.1～1份、Nb2O5 0～5份、ZrO2 0～4份；
所述烧结助剂为B2O3、SiO2、ZnO、Li2CO3、MgO中的一种或多种，所述烧结助剂共6～20份。
2.一种如权利要求1所述的低温烧结低介电常数C0G特性微波介质材料的制备方法，其特征在于，包括如下步骤：
将BaO的前驱体、SiO2的前驱体按比例混合，进行球磨、烘干、过筛后在1000℃～1100℃煅烧2.5～5小时后获得BaSi2O5；
将ZnO的前驱体、SiO2的前驱体按比例混合，进行球磨、烘干、过筛后在1150℃～1250℃煅烧2.5～5小时后获得Zn2SiO4；
所述BaSi2O5与所述Zn2SiO4，所述Al2O3、所述MnO、所述CeO2、所述CoO、所述Nb2O5、所述ZrO2的一种或多种，所述B2O3、所述SiO2、所述ZnO、所述Li2CO3、所述MgO中的一种或多种，按比例混合、球磨、烘干、过筛后获得微波介质材料；
将微波介质材料造粒后在4～6MPa压力下制成坯体，再将坯体排胶，排胶温度为500℃、升温速率为2℃/min、保温1小时，再以3～8℃/min升温至850～950℃对排胶后的坯体进行烧结保温2～5小时后随炉自然冷却。
3.根据权利要求2所述的低温烧结低介电常数C0G特性微波介质材料的制备方法，其特征在于：
所述BaO的前驱体为BaO、Ba(OH)2、BaCO3中的一种或多种；
所述SiO2的前驱体为SiO2、H2SiO3中的一种或两种；
所述ZnO的前驱体为ZnO、Zn(OH)2、ZnCO3中的一种或多种。
4.根据权利要求2所述的低温烧结低介电常数C0G特性微波介质材料的制备方法，其特征在于：
将所述B2O3、所述SiO2、所述ZnO、所述Li2CO3、所述MgO中的一种或多种按比例混合，进行球磨、烘干、过筛后在500～700℃煅烧2.5～5小时后获得烧结助剂。
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