CN116835982B - 一种层状结构微波介质谐振器的制备方法 - Google Patents
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Abstract
本发明提供了一种层状复合结构微波介质谐振器的制备方法，属于电子陶瓷技术领域。本发明提供的层状结构微波介质谐振器由上、中、下三层构成，组成表达式为yZnTi0.95Sc0.05Nb2O8‑xTiO2‑yZnTi0.95Sc0.05Nb2O8，式中x为0.03‑0.05g，y为(1‑x)/2g。本发明提供的介质谐振器温度稳定性好，同时可以保持适中的介电常数和较高的Qf值。
Description
技术领域
本发明涉及电子陶瓷技术领域，特别涉及一种层状结构微波介质谐振器的制备方法。
背景技术
随着第五代移动通信技术(5G)的发展成熟，对微波介质谐振器的性能提出了更高的要求。首先，近零的谐振频率温度系数(τf)可以保证器件的中心谐振频率不随环境温度变化而大幅度改变，减小温度变化和器件外壳热膨胀引起的中心频率漂移。其次，适中的介电常数可以匹配不同尺寸电路。最后，高的Qf值可满足器件的低损耗需求，提高器件选频特性。
发明内容
有鉴于此，本发明目的在于提供一种层状结构微波介质谐振器的制备方法，本发明提供的层状结构微波介质谐振器的温度稳定性好，且具有较高的高的Qf值和适中的介电常数。
为了实现上述目的，本发明提供以下技术方案：一种层状结构微波介质谐振器，其组成表达式为yZnTi0.95Sc0.05Nb2O8-xTiO2-yZnTi0.95Sc0.05Nb2O8，式中x为0.03-0.05g，y为(1-x)/2g。
本发明还提供了上述技术方案所述层状结构微波介质谐振器的制备方法，包括以下步骤：
1)将ZnO2、TiO2、Sc2O3、Nb2O5按照化学方程式ZnTi0.95Sc0.05Nb2O8称量所需原料，将所称取的物料混合后球磨、烘干、粉碎、过筛，然后进行预烧结，初步合成锰钽矿结构ZnTi0.95Sc0.05Nb2O8介质陶瓷粉体；
2)将TiO2按照化学方程式ZnTi0.95Sc0.05Nb2O8称量所需原料，将所称取的物料混合后球磨、烘干、粉碎、过筛，然后进行预烧结，初步合成金红石结构TiO2介质陶瓷粉体；
3)分别将步骤1)和步骤2)所得粉体加入聚乙烯醇后进行球磨、烘干、粉碎、过筛，得到造粒后的ZnTi0.95Sc0.05Nb2O8介质陶瓷和TiO2介质陶瓷粉体；
4)将步骤3)所得介质陶瓷粉体按照下层ZnTi0.95Sc0.05Nb2O8，中间层TiO2，上层ZnTi0.95Sc0.05Nb2O8的顺序加入到模具中，得到三层结构的陶瓷生坯；
5)将步骤4)所得陶瓷生坯在1100-1140℃烧结4-8h，得到层状复合结构微波介质谐振器。
优选地，步骤1)和步骤2)所述球磨还包括加入氧化锆球和去离子水或乙醇进行球磨；所述球磨转速为400转/min，球磨时间为5-8h。
优选地，步骤1)和步骤2)所述烘干温度为100℃；所述过筛为过40目筛。
优选地，步骤1)和步骤2)所述预烧结温度为900-950℃，预烧结时间为4-6h。
优选地，步骤3)所述聚乙烯醇的加入量为粉体质量的0.5％-2％。
优选地，步骤3)所述球磨时间为10-12h。
优选地，步骤3)所述过筛为过80目筛。
优选地，步骤4)所述陶瓷生坯直径为10mm，厚度为5mm。
有益技术效果：
本发明提供了一种层状结构微波介质谐振器的制备方法，本发明提供的层状结构微波介质谐振器组成表达式为yZnTi0.95Sc0.05Nb2O8-xTiO2-yZnTi0.95Sc0.05Nb2O8，式中x为0.03-0.05g，y为(1-x)/2g。本发明提供的层状结构微波介质谐振器温度稳定性好，即谐振频率温度系数近零，同时具有适中的介电常数和较高的Qf值。
附图说明
图1为实施例1所0.48ZnTi0.95Sc0.05Nb2O8-0.04TiO2-0.48ZnTi0.95Sc0.05Nb2O8微波介质陶瓷的XRD衍射图。
具体实施方式
为了更好地理解本发明，下面结合实施例进一步阐明本发明的内容，但本发明的内容不仅仅局限于下面的实施例。
实施例1
1)将ZnO、TiO2、Sc2O3、Nb2O5按化学计量式ZnTi0.95Sc0.05Nb2O8进行配料，粉料配比为：ZnO 1.1443g、TiO2 1.0768g、Sc2O3 0.0245g、Nb2O5 3.7816g，将粉料放入聚酯罐中，加入200ml去离子水、60g锆球后，使用行星式球磨机球磨6小时，转速为400转/分，单向运行，将球磨后的浆料转移至干燥箱中，于100℃烘干、粉碎后过40目筛，将过筛后的粉料放入烧结炉中，于950℃预烧结，保温6小时；
2)将5gTiO2按照与步骤1)相同的步骤依次进行球磨、干燥、过筛、预烧等步骤，得到金红石结构TiO2粉料；
3)分别向步骤1)得到的ZnTi0.95Sc0.05Nb2O8粉料和步骤2)得到的TiO2粉料中加入1.0wt％的聚乙烯醇，粉料与聚乙烯醇混合后放入球磨罐中，加入氧化锆球和去离子水，球磨12小时，烘干、粉碎后过80目筛；
4)将步骤3)所得介质陶瓷粉体按照下层0.48gZnTi0.95Sc0.05Nb2O8，中间层0.04gTiO2，上层0.48gZnTi0.95Sc0.05Nb2O8的顺序加入到模具中，得到三层结构的陶瓷生坯；
5)将步骤4)所得陶瓷生坯在1120℃烧结6h，得到层状复合结构微波介质谐振器。
将所得0.48ZnTi0.95Sc0.05Nb2O8-0.04TiO2-0.48ZnTi0.95Sc0.05Nb2O8微波介质陶瓷进行XRD表征，由图1可以看出，经过X射线粉末衍射分析，复合陶瓷的物相组成为锰钽矿ZnTi0.95Sc0.05Nb2O8与金红石TiO2两相共存。除此之外并未发现其他多余衍射峰，说明层状复合结构很大程度上限制了ZnTi0.95Sc0.05Nb2O8与TiO2两相之间发生化学反应，大幅度提高了TiO2的温度补偿效率。
实施例2
同实施例1，区别在于将层状复合结构陶瓷生坯按0.485ZnTi0.95Sc0.05Nb2O8-0.03TiO2-0.485ZnTi0.95Sc0.05Nb2O8进行压片。
实施例3
同实施例1，区别在于将层状复合结构陶瓷生坯按0.475ZnTi0.95Sc0.05Nb2O8-0.05TiO2-0.475ZnTi0.95Sc0.05Nb2O8进行压片。
对比例1
同实施例1，区别在于将层状复合结构陶瓷生坯按0.495ZnTi0.95Sc0.05Nb2O8-0.01TiO2-0.495ZnTi0.95Sc0.05Nb2O8进行压片。
对比例2
同实施例1，区别在于将层状复合结构陶瓷生坯按0.49ZnTi0.95Sc0.05Nb2O8-0.02TiO2-0.49ZnTi0.95Sc0.05Nb2O8进行压片。
将实施例1-3与对比例1-2的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，测试结果如表1所示。
表1实施例1-3和对比例1-2的微波介电性能
由表1可知，相较于对比例1-2的微波介质陶瓷，本发明实施例1-3的微波介质陶瓷具有近零的谐振频率温度系数，并兼具高的介电常数。此外实施例1-3的Qf值与对比例1-2相比，仅有小幅度下降。其中，实施例1的微波介质陶瓷的微波介电综合性能相对最佳。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。
Claims (8)
1.一种层状复合结构微波介质谐振器的制备方法，其特征在于，其组成表达式为yZnTi0.95Sc0.05Nb2O8-xTiO2-yZnTi0.95Sc0.05Nb2O8，式中x为0.03-0.05g，y为(1-x)/2g；
所述层状复合结构微波介质谐振器的制备方法采用以下步骤制得：
步骤1：将ZnO2、TiO2、Sc2O3、Nb2O5按照化学方程式ZnTi0.95Sc0.05Nb2O8称量所需原料，将所称取的物料混合后球磨、烘干、粉碎、过筛，然后进行预烧结，预烧结温度为900-950℃，预烧结时间为4-6h，初步合成锰钽矿结构ZnTi0.95Sc0.05Nb2O8介质陶瓷粉体；
步骤2：单独称量TiO2原料，依次进行球磨、烘干、粉碎、过筛，然后进行预烧结，预烧结温度为900-950℃，预烧结时间为4-6h，初步合成金红石结构TiO2介质陶瓷粉体；
步骤3：分别将步骤1和步骤2所得粉体加入聚乙烯醇后进行球磨、烘干、粉碎、过筛，得到造粒后的ZnTi0.95Sc0.05Nb2O8介质陶瓷和TiO2介质陶瓷粉体；
步骤4：将步骤3所得介质陶瓷粉体按照下层ZnTi0.95Sc0.05Nb2O8，中间层TiO2，上层ZnTi0.95Sc0.05Nb2O8的顺序加入到模具中，得到三层结构的陶瓷生坯；
步骤5：将步骤4所得陶瓷生坯在1100-1140℃烧结4-8h，得到层状复合结构微波介质谐振器。
2.根据权利要求1所述的一种层状复合结构微波介质谐振器的制备方法，其特征在于，所述组成表达式中，x为0.03、0.04或0.05g，y为(1-x)/2g。
3.根据权利要求1所述的一种层状复合结构微波介质谐振器的制备方法，其特征在于，步骤1和步骤2所述球磨还包括加入氧化锆球和去离子水或乙醇进行球磨；所述球磨转速为400转/min，球磨时间为5-8h。
4.根据权利要求1所述的一种层状复合结构微波介质谐振器的制备方法，其特征在于，步骤1和步骤2所述烘干温度为100℃；所述过筛为过40目筛。
5.根据权利要求1所述的一种层状复合结构微波介质谐振器的制备方法，其特征在于，步骤3所述聚乙烯醇的加入量为粉体质量的0.5%-2%。
6.根据权利要求1所述的一种层状复合结构微波介质谐振器的制备方法，其特征在于，步骤3所述球磨时间为10-12h。
7.根据权利要求1所述的一种层状复合结构微波介质谐振器的制备方法，其特征在于，步骤3所述过筛为过80目筛。
8.根据权利要求1所述的一种层状复合结构微波介质谐振器的制备方法，其特征在于，步骤3所述陶瓷生坯直径为10mm，厚度为5mm。
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