CN110698199A - 一种采用分步预烧法制备的低损耗微波介质陶瓷 - Google Patents

一种采用分步预烧法制备的低损耗微波介质陶瓷 Download PDF

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CN110698199A
CN110698199A CN201910976516.2A CN201910976516A CN110698199A CN 110698199 A CN110698199 A CN 110698199A CN 201910976516 A CN201910976516 A CN 201910976516A CN 110698199 A CN110698199 A CN 110698199A
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dielectric ceramic
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李玲霞
乔坚栗
杜明昆
罗伟嘉
彭伟
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Abstract

本发明公开了一种采用分步预烧法制备的低损耗微波介质陶瓷，先将MgO、Nb2O6按化学计量式MgNb2O6配料，经球磨、烘干、过筛后于1200℃～1300℃预烧；再将TiO2、ZrO2与合成的MgNb2O6按化学计量式(Ti0.8Zr0.2)0.35(Mg1/ 3Nb2/3)0.65O2配料，再经球磨、烘干、过筛后于1050℃二次预烧，经过筛、球磨后进行造粒，再压制成生坯；生坯于1175℃～1275℃烧结，制成低损耗微波介质陶瓷。本发明介电常数εr为27.34～31.09，品质因数Qf为57389～73554GHz，谐振频率温度系数τf为‑25.34～‑31.28×10‑6/℃。该制备方法工艺简单，采用中温烧结，应用前景广泛。

Description

一种采用分步预烧法制备的低损耗微波介质陶瓷
技术领域
本发明属于一种以成分为特征的陶瓷组合物，尤其涉及一种采用分步预烧法制备的(Ti0.8Zr0.2)0.35(Mg1/3Nb2/3)0.65O2为化学式的微波介质陶瓷材料及其制备方法。
背景技术
微波介质陶瓷是介质谐振器、介质滤波器、介质天线、双工器等微波电子元器件的核心材料。其工作在微波频段，具有介电常数高、损耗低、温度特性好、质量轻、成本低等特点。随着现代通信系统向小型化、集成化、多功能化、低成本化发展，对微波器件的性能(灵敏度、信噪比、覆盖范围、通信容量等)和尺寸提出了新的要求。在这一技术背景的推动下，人们迫切需要具有高介电常数，低介电损耗，近零谐振频率温度系数的微波介质陶瓷材料。
具有类金红石结构的ANb2O6-TiO2(A＝Zn,Mg,Co)是一种新型微波介质陶瓷材料，其具有烧结温度适中，介电常数较高，损耗低，谐振频率温度系数可调的优点。然而，相比于ZnNb2O6-TiO2体系，MgNb2O6-TiO2体系的Qf值较低，这是由于在烧结过程中容易形成第二相Mg4Nb2O9，限制了该体系的进一步发展。
发明内容
本发明的目的，是为了改善MgNb2O6-TiO2系微波介质陶瓷在烧结中容易形成第二相的问题，改善材料品质因数，以适应电子信息技术高频化和数字化的发展方向。以MgO、TiO2、Nb2O5、ZrO2为原料，采用分步预烧法，制备一种具有高品质因数的(Ti0.8Zr0.2)0.35(Mg1/ 3Nb2/3)0.65O2微波介质陶瓷材料。
本发明通过如下技术方案与已实现。
一种采用分步预烧法制备的低损耗微波介质陶瓷，以MgO、TiO2、Nb2O5、ZrO2为原料，目标合成物表达式为(Ti0.8Zr0.2)0.35(Mg1/3Nb2/3)0.65O2；
上述低损耗微波介质陶瓷的制备方法，具体实施步骤如下：
(1)将MgO、Nb2O6分别按化学计量式MgNb2O6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)将步骤(2)过筛后的粉料放入中温炉中，于1200℃～1300℃预烧，保温2～8小时，然后过40目筛；
(4)将TiO2、ZrO2及步骤(3)合成的MgNb2O6按化学计量式(Ti0.8Zr0.2)0.35(Mg1/ 3Nb2/3)0.65O2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；
(5)将步骤(4)球磨后的原料放入干燥箱中于80～120℃烘干，然后过40目筛；
(6)将步骤(5)过筛后的粉料放入中温炉中，于1050℃预烧，保温2～8小时，然后过40目筛；
(7)在步骤(6)预烧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；
(8)将步骤(7)球磨后的原料放入干燥箱烘干后加入5％的聚乙烯醇水溶液作为粘合剂进行造粒，过80目筛，再用粉末压片机以4～8MPa的压力压制成生坯；
(9)将步骤(4)的生坯于1175℃～1275℃烧结，保温2～8小时，制成低损耗微波介质陶瓷。
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(8)的生坯直径为10mm，厚度为5mm。
所述步骤(9)是在空气氛围中烧结
本发明通过简单固相合成法，制备了一种采用分步预烧法制备的低损耗微波介质陶瓷材料(Ti0.8Zr0.2)0.35(Mg1/3Nb2/3)0.65O2。其介电常数εr为27.34～31.09，品质因数Qf为57389～73554GHz，谐振频率温度系数τf为-25.34～-31.28×10-6/℃。该制备方法工艺简单，采用中温烧结，应用前景广泛。
具体实施方式
实施例1
以纯度大于99％的TiO2(分析纯)、MgO(分析纯)、Nb2O5(分析纯)、ZrO2(分析纯)为初始原料，通过固相法制备微波介质材料。具体实施步骤如下：
(1)将MgO、Nb2O6分别按化学计量式MgNb2O6进行配料，将粉料放入聚酯罐中，粉料配比为3.4958gMgO、21.9293gNb2O5。将粉料放入聚酯罐中，加入200ml去离子水和150g锆球后，球磨6小时，转速为400转/分；
(2)将步骤(1)球磨后的原料放入干燥箱中于100℃烘干，然后过40目筛；
(3)将步骤(2)过筛后的粉料放入中温炉中，于1200℃预烧，保温4小时，然后过40目筛；
(4)将TiO2、ZrO2及步骤(3)合成的MgNb2O6按化学计量式(Ti0.8Zr0.2)0.35(Mg1/ 3Nb2/3)0.65O2进行配料，粉料配比为：5.3910gTiO2、0.9243gZrO2、22.8825g MgNb2O6。将粉料放入聚酯罐中，加入200ml去离子水和150g锆球后，球磨6小时，转速为400转/分；
(5)将步骤(4)球磨后的原料放入干燥箱中于100℃烘干，然后过40目筛；
(6)将步骤(5)过筛后的粉料放入中温炉中，于1050℃预烧，保温4小时，然后过40目筛；
(7)在步骤(6)煅烧后的粉料放入球磨罐中，加入200ml去离子水和150g氧化锆球，球磨12小时，转速为400转/分；
(8)将步骤(7)球磨后的原料放入干燥箱烘干后加入5％的聚乙烯醇水溶液作为粘合剂进行造粒，过80目筛，再用粉末压片机以4MPa的压力压制成生坯；
(9)将步骤(8)的生坯于1250℃烧结，保温6小时；
(10)通过网络分析仪测试所得样品的微波介电性能，εr＝29.56，Qf＝73554GHz，τf＝-26.00×10-6/℃。
实施例2～5
实施例2～5除烧结温度之外，其余实施步骤与工艺参数完全相同于实施例1。本发明具体实施例的主要参数及其微波介电性能详见表1。
表1

Claims (4)

1.一种采用分步预烧法制备的低损耗微波介质陶瓷，以MgO、TiO2、Nb2O5、ZrO2为原料，目标合成物表达式为(Ti0.8Zr0.2)0.35(Mg1/3Nb2/3)0.65O2。
上述低损耗微波介质陶瓷的制备方法，具体实施步骤如下：
(1)将MgO、Nb2O6分别按化学计量式MgNb2O6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)将步骤(2)过筛后的粉料放入中温炉中，于1200℃～1300℃预烧，保温2～8小时，然后过40目筛；
(4)将TiO2、ZrO2及步骤(3)合成的MgNb2O6按化学计量式(Ti0.8Zr0.2)0.35(Mg1/3Nb2/3)0.65O2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；
(5)将步骤(4)球磨后的原料放入干燥箱中于80～120℃烘干，然后过40目筛；
(6)将步骤(5)过筛后的粉料放入中温炉中，于1050℃预烧，保温2～8小时，然后过40目筛；
(7)在步骤(6)预烧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；
(8)将步骤(7)球磨后的原料放入干燥箱烘干后加入5％的聚乙烯醇水溶液作为粘合剂进行造粒，过80目筛，再用粉末压片机以4～8MPa的压力压制成生坯；
(9)将步骤(4)的生坯于1175℃～1275℃烧结，保温2～8小时，制成低损耗微波介质陶瓷。
2.根据权利要求1所述的一种采用分步预烧法制备的低损耗微波介质陶瓷，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所述的一种采用分步预烧法制备的低损耗微波介质陶瓷，其特征在于，所述步骤(8)的生坯直径为10mm，厚度为5mm。
4.根据权利要求1所述的一种采用分步预烧法制备的低损耗微波介质陶瓷，其特征在于，所述步骤(9)是在空气氛围中烧结。
CN201910976516.2A 2019-10-14 2019-10-14 一种采用分步预烧法制备的低损耗微波介质陶瓷 Pending CN110698199A (zh)

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CN114380594A (zh) * 2021-12-30 2022-04-22 安徽壹石通材料科技股份有限公司 一种Ba-Mg-Co-Ta基微波介质陶瓷

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CN113880573A (zh) * 2021-09-10 2022-01-04 天津大学 温度稳定型低介电损耗的微波介质陶瓷材料及其制备方法
CN114380594A (zh) * 2021-12-30 2022-04-22 安徽壹石通材料科技股份有限公司 一种Ba-Mg-Co-Ta基微波介质陶瓷
CN114380594B (zh) * 2021-12-30 2022-11-11 安徽壹石通材料科技股份有限公司 一种Ba-Mg-Co-Ta基微波介质陶瓷

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