CN109111225A - 通过镁铌组分调控微波介电性能的钛酸锂基微波介质材料 - Google Patents

通过镁铌组分调控微波介电性能的钛酸锂基微波介质材料 Download PDF

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CN109111225A
CN109111225A CN201810938077.1A CN201810938077A CN109111225A CN 109111225 A CN109111225 A CN 109111225A CN 201810938077 A CN201810938077 A CN 201810938077A CN 109111225 A CN109111225 A CN 109111225A
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microwave dielectric
lithium titanate
dielectric material
titanate base
powder
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李玲霞
杜明昆
于仕辉
许振鹏
乔坚栗
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Tianjin University
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Abstract

本发明公开了一种通过镁铌组分调控微波介电性能的钛酸锂基微波介质材料，目标合成物表达式为Li2Ti1‑z(MgxNby)zO3，x:y＝1～3，z＝0.15～0.95。先按化学计量式进行配料，经过球磨、烘干、过筛后于800～1000℃预烧，再进行造粒，压制成生坯，生坯于1200～1300℃烧结，制成钛酸锂基微波介质材料。本发明在微波频段下，测得Qf值高达到101,301～145,593GHz，具有较低的介电损耗，同时εr系列化14.98～19.54，τf连续可调‑15.62～+28.63ppm/℃，具有广泛的应用前景。

Description

通过镁铌组分调控微波介电性能的钛酸锂基微波介质材料
技术领域
本发明属于一种以成分为特征的陶瓷组合物，特别涉及一种通过镁铌组分调控微波介电性能钛酸锂基微波介质材料及其制备方法
背景技术
自从物联网提出以来，在家居、运输、医疗保健、军事和石油/天然气等诸多领域，它极大推动了无线连接设备的快速增长。由3G/4G发展到5G网络的移动通讯，不断提高数据的传输速率，这急需攻克微波电路中关键组件用材料，例如天线，滤波器和谐振器。其中，微波介质材料常用作上述关键组件的介质无源基板，需要优化三个微波介电参数：品质因数(Qf)、介电常数(εr)和谐振频率的温度系数(τf)。随着移动通讯频率的不断增加，具有高品质因数、介电常数系列化和谐振频率温度系数可调的微波介质材料体系变得尤为重要。
最近有研究表明，具有岩盐结构的钛酸锂基微波介质材料，具有较高的Qf值(～63,000)、适中的εr(～20)和τf(～+28ppm/℃)，且原料相对便宜，制备工艺简单易行。然而，目前关于Li2TiO3微波介电参数的可调性研究较少，尤其Qf值(<100,000GHz)无法降低关键组件在微波频段的插入损耗，且εr和τf值较为固定，无法适应复杂多变的外部环境，尚不能满足高性能关键组件的实现。因此，通过组分调控，改善Li2TiO3的Qf值至100,000GHz以上，实现对其εr系列化和τf连续可调的精准把控，成为亟待解决的问题。
发明内容
本发明的目的，是在Li2TiO3微波介质材料体系设计中，引入不同比例的MgO/Nb2O5，精准调控镁铌组分，对相组成、微观结构进行定向裁剪，从而调节Li2TiO3微波介质材料体系的宏观微波介电性能。最终，制备出具有高品质因数(>100,000GHz)、介电常数系列化(14.98～19.54)和谐振频率温度系数可调(-15.62～+28.63ppm/℃)的钛酸锂基微波介质材料。
本发明通过如下技术方案予以实现。
一种通过镁铌组分调控微波介电性能的钛酸锂基微波介质材料，目标合成物表达式为Li2Ti1-z(MgxNby)zO3，x:y＝1～3，z＝0.15～0.95。
上述钛酸锂基微波介质材料的制备方法，具体实施步骤如下：
(1)将Li2CO3、TiO2、MgO和Nb2O5按化学计量式Li2Ti1-z(MgxNby)zO3，x:y＝1～3，z＝0.15～0.95，进行配料，将粉料放入聚酯球磨罐中，加入无水乙醇和氧化锆球后，球磨4～24小时；
(2)将步骤(1)球磨后的原料放入干燥箱中，于100～120℃烘干，然后过40目筛；
(3)将步骤(2)过筛后的粉料放入氧化铝坩埚内置于中温炉中，于800～1000℃预烧，保温2～8小时，然后过40目筛；
(4)将步骤(3)过筛后的粉料外加质量百分比含量为0.7％的PVA粉末进行混合，放入聚酯球磨罐中，加入无水乙醇和氧化锆球后，球磨4～24小时进行造粒；
(5)将步骤(4)造粒后的的粉料放入干燥箱中，于100～120℃烘干4～6小时，然后过80目筛；
(6)将步骤(5)的粉料用粉末压片机压制成生坯；
(7)将步骤(6)的生坯于1200～1300℃烧结，2～8小时，制成通过镁铌组分调控微波介电性能的钛酸锂基微波介质材料。
所述步骤(1)、(4)均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)、(4)的原料与无水乙醇和氧化锆球的质量比为1:30:15。
所述步骤(6)的生坯直径为10mm，厚度为4～5mm。
所述步骤(6)的粉末压片机的压力为4～8MPa。
所述步骤(7)的生坯烧结温度为1280℃。
本发明以Li2CO3、TiO2、MgO和Nb2O5为原料制备通过镁铌组分调控微波介电性能的钛酸锂基微波介质材料Li2Ti1-z(MgxNby)zO3，x:y＝1～3，z＝0.15～0.95。该陶瓷体系制备工艺简单，微波频段下，材料制品在最佳烧结温度时，测得Qf值高达到101,301～145,593GHz，具有较低的介电损耗，同时εr系列化14.98～19.54，τf连续可调-15.62～+28.63ppm/℃，由其制作的微波介质器件具有广泛的应用前景。
具体实施方式
本发明以纯度大于99％的Li2CO3、TiO2、MgO、Nb2O5、Ta2O5和Sb2O5为初始原料，通过固相法制备微波介质材料。具体实施方案如下：
(1)将Li2CO3、TiO2、MgO和Nb2O5按化学计量式Li2Ti1-z(MgxNby)zO3，x:y＝1～3，z＝0.15～0.95进行配料。将13g粉料放入聚酯球磨罐中，原料与无水乙醇和氧化锆球的质量比为1:30:15，在行星式球磨机上球磨12小时，球磨转速为400/转分；
(2)将步骤(1)球磨后的原料分别放入干燥箱中，于110℃烘干5小时，然后过40目筛；
(3)将步骤(2)过筛后的粉料放入氧化铝坩埚内置于中温炉中，于800～1000℃预烧，保温4小时，然后过40目筛；
(4)将步骤(3)过筛后的粉料外加质量百分比含量为0.7％的PVA粉末进行混合，放入聚酯球磨罐中，原料与无水乙醇和氧化锆球的质量比为1:30:15，在行星式球磨机上球磨12小时，转速为400转/分进行造粒；
(5)将步骤(4)球磨后的原料分别放入干燥箱中，于110℃烘干5小时，然后过80目筛；
(6)将步骤(5)的粉料用粉末压片机以6MPa的压力制成生坯，生坯直径为10mm，厚度为4.3mm；
(7)将步骤(6)的生坯于1200～1300℃烧结，保温2～8小时；
(8)通过网络分析仪测试所得样品的微波介电性能。
具体实施例1-11为不同含量的Li2Ti1-z(MgxNby)zO3，z＝0.15～0.95，x:y＝1～3，其预烧温度、烧结温度、烧结时间及其介电性能详见表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)

1.一种通过镁铌组分调控微波介电性能的钛酸锂基微波介质材料，目标合成物表达式为Li2Ti1-z(MgxNby)zO3，x:y＝1～3，z＝0.15～0.95。
上述钛酸锂基微波介质材料的制备方法，具体实施步骤如下：
(1)将Li2CO3、TiO2、MgO和Nb2O5按化学计量式Li2Ti1-z(MgxNby)zO3，x:y＝1～3，z＝0.15～0.95，进行配料，将粉料放入聚酯球磨罐中，加入无水乙醇和氧化锆球后，球磨4～24小时；
(2)将步骤(1)球磨后的原料放入干燥箱中，于100～120℃烘干，然后过40目筛；
(3)将步骤(2)过筛后的粉料放入氧化铝坩埚内置于中温炉中，于800～1000℃预烧，保温2～8小时，然后过40目筛；
(4)将步骤(3)过筛后的粉料外加质量百分比含量为0.7％的PVA粉末进行混合，放入聚酯球磨罐中，加入无水乙醇和氧化锆球后，球磨4～24小时进行造粒；
(5)将步骤(4)造粒后的的粉料放入干燥箱中，于100～120℃烘干4～6小时，然后过80目筛；
(6)将步骤(5)的粉料用粉末压片机压制成生坯；
(7)将步骤(6)的生坯于1200～1300℃烧结，2～8小时，制成通过镁铌组分调控微波介电性能的钛酸锂基微波介质材料。
2.根据权利要求1所述的通过镁铌组分调控微波介电性保温能的钛酸锂基微波介质材料，其特征在于，所述步骤(1)、(4)均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所述的通过镁铌组分调控微波介电性能的钛酸锂基微波介质材料，其特征在于，所述步骤(1)、(4)的原料与无水乙醇和氧化锆球的质量比为1:30:15。
4.根据权利要求1所述的通过镁铌组分调控微波介电性能的钛酸锂基微波介质材料，其特征在于，所述步骤(6)的生坯直径为10mm，厚度为4～5mm。
5.根据权利要求1所述的通过镁铌组分调控微波介电性能的钛酸锂基微波介质材料，其特征在于，所述步骤(6)的粉末压片机的压力为4～8MPa。
6.根据权利要求1所述的通过镁铌组分调控微波介电性能的钛酸锂基微波介质材料，其特征在于，所述步骤(7)的生坯烧结温度为1280℃。
CN201810938077.1A 2018-08-16 2018-08-16 通过镁铌组分调控微波介电性能的钛酸锂基微波介质材料 Pending CN109111225A (zh)

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