CN108793994A - 一种施主掺杂中介电常数微波介质陶瓷及其制备方法 - Google Patents

一种施主掺杂中介电常数微波介质陶瓷及其制备方法 Download PDF

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CN108793994A
CN108793994A CN201810930821.3A CN201810930821A CN108793994A CN 108793994 A CN108793994 A CN 108793994A CN 201810930821 A CN201810930821 A CN 201810930821A CN 108793994 A CN108793994 A CN 108793994A
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李玲霞
张博文
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Abstract

本发明公开了一种施主掺杂中介电常数微波介质陶瓷及其制备方法，合成物表达式为：Li2ZnTi3‑xNbxO8+x/2，其中x＝0.01～0.05。先将Li2CO3、ZnO、Nb2O5、TiO2按化学计量式进行配料，经球磨、烘干、过筛后，于925℃煅烧；再经造粒、压制成坯体，坯体于1080℃～1120℃烧结，制成微波介质陶瓷。本发明通过施主元素部分取代Ti4+，制备出了一种新型的微波介质陶瓷材料，其介电常数为24～26，品质因数Qf值为74000GHz～81000GHz，谐振频率温度系数τf为‑7ppm/℃～‑9ppm/℃。该体系制备工艺简单，采用中温烧结，节约了时间和能源成本，应用前景广泛。

Description

一种施主掺杂中介电常数微波介质陶瓷及其制备方法
技术领域
本发明属于一种以成分为特征的陶瓷组合物，尤其涉及一种施主掺杂高性能微波介质陶瓷材料及其制备方法。
背景技术
近年来微波技术迅猛发展，以手机、微信通信、GPS等为代表微波通讯产品已经深入到我们每个人的身边。微波通讯的发展离不开作为核心器件的滤波器。因而研发损耗低，频率特性好，性能稳定可靠，是具有自主知识产权的滤波器成为研究的热点。作为滤波器的一种—介质谐振滤波器，电磁波谐振就发生在介质材料内部，由于其所使用的陶瓷介质材料低损耗，小温度漂移，高介电常数、等不可比拟的优点，使得介质滤波器逐步取代金属腔滤波器在移动基站、卫星通讯等领域得到广泛采用。
介质滤波器的核心是陶瓷介质材料，微波介质陶瓷材料的性能成为制约介质滤波器性能的关键之一。本发明基于传统固相法制备工艺，通过简单的施主元素的引入，提升了体系的品质因数，制备出中温烧结、中介电常数、高Q值、谐振频率温度系数近零的Li2ZnTi3O8基陶瓷体系。最终获得的Li2ZnTi3-xNbxO8+x/2(x＝0.01～0.05)，烧结温度为1100℃，介电常数为25～26，品质因数(Qf)为74000～81000GHz，谐振频率温度系数为-7～-9ppm/℃。
发明内容
本发明的目的，是提供一种化学构成为Li2ZnTi3-xNbxO8+x/2(x＝0.01～0.05)，中温烧结、中介电常数、高Q值的施主掺杂中介电常数微波介质陶瓷材料，有望应用于5G移动通讯。
本发明通过如下技术方案予以实现。
一种施主掺杂中介电常数微波介质陶瓷，合成物表达式为：Li2ZnTi3-xNbxO8+x/2，其中x＝0.01～0.05。
上述施主掺杂中介电常数微波介质陶瓷的制备方法，具体实施步骤如下：
(1)将Li2CO3、ZnO、Nb2O5、TiO2按化学计量式Li2ZnTi3-xNbxO8+x/2其中x＝0.01～0.05进行配料；将粉料放入聚酯罐中，加入去离子水或无水乙醇和氧化锆球后，球磨6小时；
(2)将步骤(1)球磨后的原料放入红外干燥箱中，于80～120℃烘干，然后过40目筛；
(3)将过筛后的粉料放入中温马弗炉中，于925℃煅烧4小时；
(4)在步骤(3)煅烧后的粉料中外加质量百分比含量为0.9％～1.1％的聚乙烯醇作为粘合剂进行造粒，将混合后的粉料放入球磨罐中，加入氧化锆球或无水乙醇，球磨12小时后烘干过80目筛，再用粉末压片机压制成坯体；
(5)将步骤(4)的坯体于1080℃～1120℃烧结，保温6小时，制成Li2ZnTi3-xNbxO8+x/2其中x＝0.01～0.05微波介质陶瓷。
所述步骤(1)采用行星式球磨机进行球磨，球磨机转速为400转/分。
所述步骤(1)的粉料与无水乙醇或氧化锆球的质量比为1：10：6。
所述步骤(4)的生坯直径为10mm，厚度为4-6mm。
所述步骤(4)的粉末压片机的压力为200MPa。
所述步骤(5)的烧结温度为1100℃。
本发明通过施主元素部分取代Ti4+，制备出了一种新型的微波介质陶瓷材料Li2ZnTi3-xNbxO8+x/2(x＝0.01～0.05)。其介电常数为24～26，品质因数Qf值为74000GHz～81000GHz，谐振频率温度系数τf为-7ppm/℃～-9ppm/℃。该体系制备方法制备工艺简单，采用中温烧结，节约时间成本和能源成本，应用前景广泛。
具体实施方式
本发明以Li2CO3(Ar)、ZnO(PT)、Nb2O5(Ar)、TiO2(Ar)为初始原料，通过简单固相合成法制备微波介质陶瓷。实施方案如下：
1.将Li2CO3、ZnO、Nb2O5、TiO2按化学计量式Li2ZnTi3-xNbxO8+x/2(x＝0.01～0.05)进行配料。将15g粉料放入聚酯罐中，加入250ml去离子水(或无水乙醇)、150g氧化锆球后，在行星式球磨机上球磨6小时，球磨机转速为400转/分；
2.将球磨后的粉料置于干燥箱中，于100℃烘干后过40目筛；
3.将烘干过筛后的粉料放入中温炉中，于900℃预烧，保温4小时；
4.在步骤(3)预烧后的粉料中外加质量百分比含量为0.9％～1.1％的聚乙烯醇作为粘合剂进行造粒，将混合后的粉料放入球磨罐中，加入氧化锆球和去离子水(或无水乙醇)，球磨12小时，烘干后过80目筛，再用粉末压片机以200MPa的压力压制成坯体，坯体直径为10mm，厚度为4-6mm；
5.将坯体在1080℃～1120℃烧结，保温6小时，制成Li2ZnTi3-xNbxO8+x/2(x＝0.01～0.05)微波介质陶瓷。
通过网络分析仪测试所得制品的微波介电性能。
本发明具体实施例的相关工艺参数及其微波介电性能详见表1。
表1
本发明并不局限于上述实施例，很多细节的变化是可能的，但这并不因此违背本发明的范围和精神。

Claims (6)

1.一种施主掺杂中介电常数微波介质陶瓷，合成物表达式为：Li2ZnTi3-xNbxO8+x/2，其中x＝0.01～0.05。
上述施主掺杂中介电常数微波介质陶瓷的制备方法，具体实施步骤如下：
(1)将Li2CO3、ZnO、Nb2O5、TiO2按化学计量式Li2ZnTi3-xNbxO8+x/2其中x＝0.01～0.05进行配料；将粉料放入聚酯罐中，加入去离子水或无水乙醇和氧化锆球后，球磨6小时；
(2)将步骤(1)球磨后的原料放入红外干燥箱中，于80～120℃烘干，然后过40目筛；
(3)将过筛后的粉料放入中温马弗炉中，于925℃煅烧4小时；
(4)在步骤(3)煅烧后的粉料中外加质量百分比含量为0.9％～1.1％的聚乙烯醇作为粘合剂进行造粒，将混合后的粉料放入球磨罐中，加入氧化锆球或无水乙醇，球磨12小时后烘干过80目筛，再用粉末压片机压制成坯体；
(5)将步骤(4)的坯体于1080℃～1120℃烧结，保温6小时，制成Li2ZnTi3-xNbxO8+x/2其中x＝0.01～0.05微波介质陶瓷。
2.根据权利要求1所述的一种施主掺杂中介电常数微波介质陶瓷，其特征在于，所述步骤(1)采用行星式球磨机进行球磨，球磨机转速为400转/分。
3.根据权利要求1所述的一种施主掺杂中介电常数微波介质陶瓷，其特征在于，所述步骤(1)的粉料与无水乙醇或氧化锆球的质量比为1：10：6。
4.根据权利要求1所述的一种施主掺杂中介电常数微波介质陶瓷，其特征在于，所述步骤(4)的生坯直径为10mm，厚度为4-6mm。
5.根据权利要求1所述的一种施主掺杂中介电常数微波介质陶瓷，其特征在于，所述步骤(4)的粉末压片机的压力为200MPa。
6.根据权利要求1所述的一种施主掺杂中介电常数微波介质陶瓷，其特征在于，所述步骤(5)的烧结温度为1100℃。
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CN111704455A (zh) * 2020-06-15 2020-09-25 苏州瑞玛精密工业股份有限公司 一种锂锌钛微波介电陶瓷及其制备方法和应用
CN116768616A (zh) * 2023-05-11 2023-09-19 电子科技大学 一种高Q值Li6Zn7Ti11O32基微波介质陶瓷材料及其制备方法
CN116768616B (zh) * 2023-05-11 2024-04-12 电子科技大学 一种高Q值Li6Zn7Ti11O32基微波介质陶瓷材料及其制备方法

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