CN110803929A - 一种谐振器用类金红石结构微波介质陶瓷 - Google Patents

一种谐振器用类金红石结构微波介质陶瓷 Download PDF

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CN110803929A
CN110803929A CN201911074765.9A CN201911074765A CN110803929A CN 110803929 A CN110803929 A CN 110803929A CN 201911074765 A CN201911074765 A CN 201911074765A CN 110803929 A CN110803929 A CN 110803929A
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microwave dielectric
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李玲霞
王顺
罗伟嘉
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Abstract

本发明公开了一种谐振器用类金红石结构微波介质陶瓷，合成物表达式为ZnO‑(0.97+x)TiO2‑0.03GeO2‑Nb2O5，其中x＝0.6～0.9。先将原料按化学计量式配料，经球磨、烘干、过筛、预烧后，初步合成锰钽矿型ZnO‑0.97TiO2‑0.03GeO2‑Nb2O5基体粉料，再将基体粉料中加入与基体摩尔比为x的TiO2，x＝0.6～0.9，经造粒，成型后，坯体于1090～1160℃烧结，得到类金红石结构微波介质陶瓷。本发明介电常数εr为39.2～46.3，品质因数Qf值为31030GHz～50800GHz，谐振频率温度系数τf为‑36.5～+17.0ppm/℃。制备工艺简单，原料低廉，采用中温烧结，应用前景广泛。

Description

一种谐振器用类金红石结构微波介质陶瓷
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ZnO-(0.97+x)TiO2-0.03GeO2-Nb2O5为化学式的中温烧结、具有良好微波介电性能的复合微波介质陶瓷材料及其制备方法。
背景技术
随着移动通信技术进入5G时代，小型化、高频化、高性能化已成为移动通信设备和便携式终端的发展趋势，相应的微波电路应具有高集成度、低功耗和高稳定性等特点。作为微波电路的重要组成部分，微波介质器件的尺寸、功耗以及稳定性直接影响电路的集成度和性能，如何实现器件小尺寸、低功耗与高稳定性的需求成为当前研究的热点。而高品质微波介质器件往往以高性能微波介质材料为依托。微波介质谐振器是该材料在移动通信领域的一种典型应用，较高介电常数，高Qf值与近零谐振频率温度系数是对微波介质谐振器用微波介质陶瓷材料性能的要求。但是，传统谐振器用微波介质材料如BaO-TiO2系和(Zr,Sn)TiO4系材料，存在烧结温度高，提升介电常数Qf值损失大，大多含有贵金属Ta等问题。
因此，寻找并制备出烧结温度低，介电常数高，同时保持高Qf值与较低谐振频率温度系数的微波介质材料是解决该问题的关键。本发明采用传统固相法，制备出中温烧结的ZnO-(0.97+x)TiO2-0.03GeO2-Nb2O5微波介质陶瓷，大大降低了制备成本，并测试了其微波介电性能，通过调节结构中金红石相的比例，在保持材料高介电常数，较高Qf值的同时，实现谐振频率温度系数近零的调节。
发明内容
本发明的目的，是针对传统谐振器用微波介质材料如BaO-TiO2系和(Zr,Sn)TiO4系材料，存在烧结温度高、提升介电常数Qf值损失大、大多含有贵金属Ta等问题，提供一种以ZnO、TiO2、GeO2、Nb2O5为原料，采用传统固相法，制备具有良好微波介电性能的新型锰钽矿-金红石复合结构ZnO-(0.97+x)TiO2-0.03GeO2-Nb2O5(x＝0.6～0.9)微波介质陶瓷。
本发明通过如下技术方案予以实现。
一种谐振器用类金红石结构微波介质陶瓷，合成物表达式为ZnO-(0.97+x)TiO2-0.03GeO2-Nb2O5，其中x＝0.6～0.9；
上述谐振器用类金红石结构微波介质陶瓷的制备方法，实施步骤如下：
(1)将ZnO、TiO2、GeO2、Nb2O5按化学计量式ZnO-0.97TiO2-0.03GeO2-Nb2O5进行配料，将粉料放入聚酯罐中，加入去离子水和锆球后，球磨4～8h；
(2)将步骤(1)球磨后的原料放入干燥箱中，于120℃烘干，然后过40目筛；
(3)将过筛后的粉料放入中温炉中，于950℃煅烧5～8h，初步合成锰钽矿型ZnO-0.97TiO2-0.03GeO2-Nb2O5基体粉料；
(4)在步骤(3)初步合成的基体粉料中加入与基体摩尔比为x的TiO2，x＝0.6～0.9，同时加入0.8wt％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，加入去离子水或无水乙醇，湿磨12h后烘干，反复过80目筛，保证粉体颗粒度均匀，再用粉末压片机以2MPa的压力压制成坯体；
(5)将步骤(4)的坯体于1090～1160℃烧结，保温5～8h，制成谐振器用类金红石结构微波介质陶瓷。
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)的粉料与去离子水和锆球的质量比为1︰10︰6。
所述步骤(4)的x＝0.8。
所述步骤(4)的生坯直径为10mm，厚度为5mm。
所述步骤(5)的烧结温度为1100℃。
本发明通过简单固相合成法制备了一种新型复合微波介质陶瓷材料ZnO-(0.97+x)TiO2-0.03GeO2-Nb2O5，x＝0.6～0.9。其介电常数εr为39.2～46.3，品质因数Qf值为31030GHz～50800GHz，谐振频率温度系数τf为-36.5～+17.0ppm/℃。该方法制备工艺简单，原料低廉，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ZnO(分析纯)、TiO2(分析纯)、GeO2(分析纯)、Nb2O5(分析纯)为初始原料，通过简单固相合成法制备微波介质陶瓷。
实施例1
1.将ZnO、TiO2、GeO2、Nb2O5按化学计量式ZnO-0.97TiO2-0.03GeO2-Nb2O5进行配料，粉料配比为：1.9348g ZnO、1.8412g TiO2、0.0739g GeO2和6.2550g Nb2O5。将约10g粉料放入聚酯罐中，加入250ml去离子水、150g锆球后，在行星式球磨机上球磨6h，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.过筛后的粉料放入中温炉，于950℃预烧，保温5h，初步合成ZnO-0.97TiO2
-0.03GeO2-Nb2O5基体粉料；
4.在步骤3预烧后的基体粉料中加入与基体摩尔比为0.6的TiO2，同时加入0.8wt％的聚乙烯醇作为粘合剂进行混合，放入球磨罐中，加入氧化锆球和去离子水，球磨12h，烘干后过80目筛，再用粉末压片机以2MPa的压力压制成生坯；
5.将生坯在1100℃烧结，保温6h，制成新型类金红石结构复合微波介质陶瓷。
6.通过网络分析仪测试步骤5得到制品的微波介电性能。
实施例2
1.将ZnO、TiO2、GeO2、Nb2O5按化学计量式ZnO-0.97TiO2-0.03GeO2-Nb2O5进行配料，粉料配比为：1.9348g ZnO、1.8412g TiO2、0.0739g GeO2和6.2550g Nb2O5。将约10g粉料放入聚酯罐中，加入250ml去离子水、150g锆球后，在行星式球磨机上球磨8h，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.过筛后的粉料放入中温炉，于950℃预烧，保温8h，初步合成ZnO-0.97TiO2-0.03GeO2-Nb2O5基体粉料；
4.在步骤3预烧后的基体粉料中加入与基体摩尔比为0.65的TiO2，同时加入0.8wt％的聚乙烯醇作为粘合剂进行混合，放入球磨罐中，加入氧化锆球和去离子水，球磨12h，烘干后过80目筛，再用粉末压片机以2MPa的压力压制成生坯；
5.将生坯在1100℃烧结，保温7h，制成新型类金红石结构复合微波介质陶瓷。
6.通过网络分析仪测试步骤5得到制品的微波介电性能。
实施例3～8
实施例3～8除x值和烧结温度之外，其它工艺参数完全相同于实施例1。本发明具体实施例的主要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)

1.一种谐振器用类金红石结构微波介质陶瓷，合成物表达式为ZnO-(0.97+x)TiO2-0.03GeO2-Nb2O5，其中x＝0.6～0.9；
上述谐振器用类金红石结构微波介质陶瓷的制备方法，实施步骤如下：
(1)将ZnO、TiO2、GeO2、Nb2O5按化学计量式ZnO-0.97TiO2-0.03GeO2-Nb2O5进行配料，将粉料放入聚酯罐中，加入去离子水和锆球后，球磨4～8h；
(2)将步骤(1)球磨后的原料放入干燥箱中，于120℃烘干，然后过40目筛；
(3)将过筛后的粉料放入中温炉中，于950℃煅烧5～8h，初步合成锰钽矿型ZnO-0.97TiO2-0.03GeO2-Nb2O5基体粉料；
(4)在步骤(3)初步合成的基体粉料中加入与基体摩尔比为x的TiO2，x＝0.6～0.9，同时加入0.8wt％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，加入去离子水或无水乙醇，湿磨12h后烘干，反复过80目筛，保证粉体颗粒度均匀，再用粉末压片机以2MPa的压力压制成坯体；
(5)将步骤(4)的坯体于1090～1160℃烧结，保温5～8h，制成谐振器用类金红石结构微波介质陶瓷。
2.根据权利要求1所述的谐振器用类金红石结构微波介质陶瓷，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所述的谐振器用类金红石结构微波介质陶瓷，其特征在于，所述步骤(1)的粉料与去离子水和锆球的质量比为1︰10︰6。
4.根据权利要求1所述的谐振器用类金红石结构微波介质陶瓷，其特征在于，所述步骤(4)的x＝0.8。
5.根据权利要求1所述的谐振器用类金红石结构微波介质陶瓷，其特征在于，所述步骤(4)的生坯直径为10mm，厚度为5mm。
6.根据权利要求1所述的谐振器用类金红石结构微波介质陶瓷，其特征在于，所述步骤(5)的烧结温度为1100℃。
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