CN107162592A - 一种铌酸盐微波介质陶瓷材料及其制备方法 - Google Patents

一种铌酸盐微波介质陶瓷材料及其制备方法 Download PDF

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CN107162592A
CN107162592A CN201710282281.8A CN201710282281A CN107162592A CN 107162592 A CN107162592 A CN 107162592A CN 201710282281 A CN201710282281 A CN 201710282281A CN 107162592 A CN107162592 A CN 107162592A
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李玲霞
李江腾
张帅
吕笑松
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Abstract

本发明公开了一种铌酸盐微波介质陶瓷材料，合成物表达式为：ZnZr1‑xMnxNb2O8，其中x＝0.02～0.2。先将ZnO、ZrO2、Nb2O5、MnO2按化学计量式进行配料；经过球磨、烘干、过筛，再于950℃煅烧，造粒后压力成型为坯体，坯体于1100℃～1200℃烧结，制成所需微波介质陶瓷。本发明介电常数εr为24.23～29.29，品质因数Q×f为23652～57678GHz，谐振频率温度系数τf为‑30.24～‑4.37×10‑6/℃；且制备工艺简单，中温烧结，节约了制备成本，应用前景广泛。

Description

一种铌酸盐微波介质陶瓷材料及其制备方法
技术领域
本发明属于一种以成分为特征的陶瓷组合物，尤其涉及一种以ZnZr1-xMnxNb2O8为化学式的中温烧结、具有中介电常数的微波介质陶瓷材料及其制备方法。
背景技术
随着材料科学的快速发展，器件进一步小型化和高品质化的要求仍为未来的主旋律，但由于目前各频段对信号质量的需求不同，因此对于应用中微波介质材料实现器件小型化来说，重点是保证介质材料具有高的品质因数。而除此之外，优化材料的谐振频率温度系数，也是材料应用方面的重要课题。
微波介质材料以其系列化的介电常数(ε)、较高的品质因数(Qf)、相对较小的谐振频率温度系数(τf)被广泛应用于制作谐振器、滤波器、介质天线、介质导波等微波无源器件，满足了移动通讯、卫星通讯和军用雷达等发展的要求。这些无源器件在小型化、高品质化方面相较传统的无源器件有较大的提升。
ZnZrNb2O8作为一种新型微波介质陶瓷材料，因其具有适中的介电常数，较高的Qf值而受到广泛关注。纯相的ZnZrNb2O8材料的微波介电性能为：Qf＝61000GHz，εr＝30，τf＝-52×10-6/℃。其现有技术的缺点是，品质因数有待进一步提高，温度系数不可调节。
发明内容
本发明的目的，是为了进一步提高ZnZrNb2O8介质陶瓷材料的品质因数，并在一定程度上提升其温度稳定性，以适应电子信息技术高频化和数字化的发展方向。以ZnO、ZrO2、Nb2O5、MnO2为原料，采用简单固相法，制备一种具有高品质因数的ZnZr1-xMnxNb2O8微波介质陶瓷材料。
本发明通过如下技术方案予以实现。
一种铌酸盐微波介质陶瓷材料，合成物表达式为：ZnZr1-xMnxNb2O8，其中x＝0.02～0.2；
该铌酸盐微波介质陶瓷材料的制备方法，具体步骤如下：
(1)将ZnO、ZrO2、Nb2O5、MnO2按化学计量式ZnZr1-xMnxNb2O8，其中x＝0.02～0.2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4～8小时；
(2)将步骤(1)球磨后的原料放入干燥箱中，于80～120℃烘干，然后过40目筛；
(3)将烘干、过筛后的粉料放入中温炉中，于950℃煅烧5～8小时；
(4)在步骤(3)煅烧后的粉料中外加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，球磨9～12小时后烘干过筛，再用粉末压片机以4～8MPa的压力压制成坯体；
(5)将步骤(4)的坯体于1100℃～1200℃烧结，保温2～8小时，制成具有中介电常数的微波介质陶瓷。
所述步骤(1)采用行星式球磨机进行球磨，球磨机转速为600转/分。
所述步骤(1)的粉料与去离子水和锆球的质量比为1︰1︰1。
所述步骤(4)的坯体直径为10mm，厚度为5mm。
所述步骤(5)的优选的烧结温度为1150℃。
本发明通过简单固相合成法制备出一种新型的微波介质陶瓷材料ZnZr1-xMnxNb2O8(x＝0.02～0.2)。其介电常数εr为28.359～25.2946，品质因数Q×f为38906～57678GHz，谐振频率温度系数τf为-25.14～-7.76×10-6/℃。制备工艺简单，采用中温烧结，节约了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)、Nb2O5(分析纯)、ZrO2(分析纯)、MnO2(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、Nb2O5、ZrO2、MnO2按化学计量式ZnZr1-xMnxNb2O8(x＝0.02)进行配料，粉料配比为：2.4669gZnO、3.7340g ZrO2、7.9750g Nb2O5、0.0908gMnO2。将约20g粉料放入聚酯罐中，加入氧化锆球和去离子水，在行星式球磨机上球磨6小时，转速为600转/分；
2.将球磨后的粉料分别置于干燥箱中，于100℃烘干后过40目筛；
3.烘干过筛后的粉料放入中温炉，于950℃预烧，保温4小时；
4.在步骤3预烧后的粉料中加入1.1％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12小时，烘干后过80目筛，再用粉末压片机以6MPa的压力压制成坯体；
5.将生坯在1150℃烧结，保温6小时，制成中介电常数微波介质陶瓷。
通过网络分析仪测试所得制品的微波特性。
实施例2～3
实施例2～3的制备方法基本相同于实施例1，仅是x的取值不同。各个实施例的x的取值以及相关的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 (5)

1.一种铌酸盐微波介质陶瓷材料，合成物表达式为：ZnZr1-xMnxNb2O8，其中x＝0.02～0.2。
该铌酸盐微波介质陶瓷材料的制备方法，具体步骤如下：
(1)将ZnO、ZrO2、Nb2O5、MnO2按化学计量式ZnZr1-xMnxNb2O8，其中x＝0.02～0.2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4～8小时；
(2)将步骤(1)球磨后的原料放入干燥箱中，于80～120℃烘干，然后过40目筛；
(3)将烘干、过筛后的粉料放入中温炉中，于950℃煅烧5～8小时；
(4)在步骤(3)煅烧后的粉料中外加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，球磨9～12小时后烘干过筛，再用粉末压片机以4～8MPa的压力压制成坯体；
(5)将步骤(4)的坯体于1100℃～1200℃烧结，保温2～8小时，制成具有中介电常数的微波介质陶瓷。
2.根据权利要求1所述的一种铌酸盐微波介质陶瓷材料，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600转/分。
3.根据权利要求1所述的一种铌酸盐微波介质陶瓷材料，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︰1︰1。
4.根据权利要求1所述的一种铌酸盐微波介质陶瓷材料，其特征在于，所述步骤(4)的坯体直径为10mm，厚度为5mm。
5.根据权利要求1所述的一种铌酸盐微波介质陶瓷材料，其特征在于，所述步骤(5)的优选的烧结温度为1150℃。
CN201710282281.8A 2017-04-26 2017-04-26 一种铌酸盐微波介质陶瓷材料及其制备方法 Pending CN107162592A (zh)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109336596A (zh) * 2018-09-30 2019-02-15 天津大学 具有低介电常数和超低介电损耗的镁锆锗铌系微波介质陶瓷及制备方法和应用
CN115010490A (zh) * 2022-06-29 2022-09-06 安徽大学 一种超低损耗铌锆酸锌系微波介质陶瓷材料及其制备方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104310986A (zh) * 2014-10-09 2015-01-28 天津大学 一种高介电常数温度稳定型陶瓷电容器介质材料

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104310986A (zh) * 2014-10-09 2015-01-28 天津大学 一种高介电常数温度稳定型陶瓷电容器介质材料

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109336596A (zh) * 2018-09-30 2019-02-15 天津大学 具有低介电常数和超低介电损耗的镁锆锗铌系微波介质陶瓷及制备方法和应用
CN115010490A (zh) * 2022-06-29 2022-09-06 安徽大学 一种超低损耗铌锆酸锌系微波介质陶瓷材料及其制备方法

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