CN101565300A - 一种低损耗微波介质陶瓷 - Google Patents

一种低损耗微波介质陶瓷 Download PDF

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CN101565300A
CN101565300A CNA2008100610469A CN200810061046A CN101565300A CN 101565300 A CN101565300 A CN 101565300A CN A2008100610469 A CNA2008100610469 A CN A2008100610469A CN 200810061046 A CN200810061046 A CN 200810061046A CN 101565300 A CN101565300 A CN 101565300A
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陈湘明
范协诚
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Zhejiang University ZJU
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Abstract

本发明提供了一种低损耗微波介质陶瓷，所述低损耗微波介质陶瓷主要组分表达式为：xCaO.yLn2O3.zAl2O3.mTiO2，其中Ln为Nd或Sm，x、y、z、m依次为CaO、Ln2O3、Al2O3、TiO2的摩尔含量，25.0mol％≤x≤75.0mol％，10.0mol％≤y≤30.0mol％，10.0％≤z≤30.0mol％，0.8mol％≤m≤20.0mol％，x+y+z+m＝100mol％。本发明提供的低损耗微波介质陶瓷介电常数为18～25、Qf值高达80,000～200,000GHz，并具有近零谐振频率温度系数；利用本发明可使介质谐振器、滤波器及天线等微波元器件适合更高频率与更大功率的应用；还可应用于微波电容器、温度补偿电容器或微波基板等，在工业上有着极大的价值。

Description

一种低损耗微波介质陶瓷
(一)技术领域
本发明涉及一种低损耗微波介质陶瓷，尤其是用于微波介质谐振器、滤波器及天线等微波通讯系统中的关键元器件制作的低损耗微波介质陶瓷。
(二)背景技术
近年来，随着移动通讯与卫星通讯技术等微波通讯技术的迅速发展，对介质谐振器、滤波器以及微波天线等微波元器件用的微波介质陶瓷的需求正在日益增长。而微波通讯向微波高端的迅速发展，对低损耗微波介质陶瓷提出更高的要求，其基本性能要求为：介电常数 &epsiv; < 3 0 ~ , 以适合微波高端应用；品质因数Qf＞60,000GHz，以获得在微波频率下更好的选频性；谐振频率温度系数τf＝0±10ppm/℃，用于保证器件在温度波动时具有很好的稳定性。
另一方面，虽然目前已有Ba(Mg1/3Ta2/3)O3、CaTiO3-MgTiO3等低损耗微波介质陶瓷，但前者烧结温度高、制备困难、品质因数与温度系数随制备条件变化较大，而后者存在Qf值偏低的缺点。同时，前者还由于含贵金属、存在高成本问题。
因此，迫切需要开发一种制备简单、低成本、性能优良的低损耗微波介质陶瓷，以满足相关应用的需求。
(三)发明内容
本发明的目的是提供一种介电常数为18～25、同时具有低损耗(Qf＝80,000～200,000GHz)与良好的温度稳定性的微波介质陶瓷。
本发明采用的技术方案是：
一种低损耗微波介质陶瓷，所述低损耗微波介质陶瓷主要组分表达式为：xCaO.yLn2O3.zAl2O3.mTiO2，其中Ln为Nd或Sm，x、y、z、m依次为CaO、Ln2O3、Al2O3、TiO2在氧化物混合物中所占的物质的量百分含量，25.0mol％≤x≤75.0mol％，10.0mol％≤y≤30.0mol％，10.0mol％≤z≤30.0mol％，0.8mol％≤m≤20.0mol％，x+y+z+m＝100mol％。上述组分为所述低损耗微波介质陶瓷产品的主要有效成分，不包括制备过程中添加的粘结剂，以及原料本身含有的或制备过程中产生的微量物理杂质。
优选组分：45.0mol％≤x≤60.0mol％，15.0mol％≤y≤25.0mol％，15.0mol％≤z≤25.0mol％，4.0mol％≤m≤20.0mol％，x+y+z+m＝100mol％。
最佳组分：Ln为Sm，x＝54.55mol％，y＝18.18mol％，z＝18.18mol％，m＝9.09mol％。按此配方的得到的微波介质桃子具有最佳的微波介质性能：介电常数 &epsiv; = 21 . 5 ~ , 品质因数Qf＝200,000GHz，谐振频率温度系数τf＝+3ppm/℃。
本发明所述的低损耗微波介质陶瓷可按本领域常规方法制备，具体方法可如下：按组分中CaO、Ln2O3、Al2O3、TiO2的摩尔含量比例取原料CaCO3、Nd2O3或Sm2O3、Al2O3及TiO2，以蒸馏水为溶剂用湿式球磨法混合18～28小时，烘干后在1150～1250℃、大气气氛中预烧2～5小时得到预烧粉末，然后，在预烧粉末中添加粘结剂、造粒、制备陶瓷坯体，制得陶瓷坯体于1400～1550℃、大气气氛中烧结2～5小时，得到所述的低损耗微波介质陶瓷。所述粘结剂为本领域通常适用于陶瓷制备的粘结剂。
具体方法如下所述。按组分中CaO、Ln2O3、Al2O3、TiO2的摩尔含量比例取CaCO3、Nd2O3或Sm2O3、Al2O3及TiO2，以蒸馏水为溶剂用湿式球磨法混合24小时，烘干后在1150～1250℃、大气气氛中预烧3小时得到预烧粉末，然后，在预烧粉末中添加质量为预烧粉末总质量5～8％的粘结剂、造粒、于1000kg/cm2的压力下制备直径12mm、厚度4～6mm的陶瓷坯体，制得陶瓷坯体于1400～1550℃、大气气氛中烧结3小时，得到所述的低损耗微波介质陶瓷，本发明用的粘结剂是聚乙烯乙醇(PVA)水溶液。
本发明的有益效果主要体现在：提供了一种具有低损耗与近零谐振频率温度系数、同时介电常数为18-25的低损耗微波介质陶瓷。利用本发明提供的低损耗微波介质陶瓷，可使介质谐振器、滤波器及天线等微波元器件适合更高频率与更大功率的应用。同时，本发明提供的陶瓷亦可应用于微波电容器、温度补偿电容器或微波基板等。因此，本发明在工业上有着极大的价值。
(四)具体实施方式
下面结合具体实施例对本发明进行进一步描述，但本发明的保护范围并不仅限于此：
实施例1～16：
首先，将纯度为99.9％以上的CaCO3、Nd2O3或Sm2O3、Al2O3及TiO2按表1中各实施例的摩尔含量比例用湿式球磨法混合24小时(溶剂为蒸馏水)，烘干后在1150～1250℃、大气气氛中预烧3小时。然后，在预烧粉末中添加6wt％的聚乙烯乙醇(PVA)水溶液(浓度5wt％，所用PVA聚合度为1750)并造粒后，通过单轴压力成形在1000kg/cm2的压力下制备出直径12mm、厚度4～6mm的陶瓷坯体，最后在1400～1550℃、大气气氛中烧结3小时，得到所述的低损耗微波介质陶瓷。
用粉末X线衍射法对烧结后的陶瓷试样进行了物相分析，用介质谐振器法与谐振腔法在10GHz进行了微波介电性能的评价。
实施例中材料的微波介质陶瓷性能与组成的关系如表1所示。
表1：微波介质陶瓷组成与性能
从表可知，在本发明的陶瓷体系中，随着CaO、TiO2含量的增加与Ln2O3(Ln＝Nd或Sm)、Al2O3含量的减少，介电常数ε趋于增加，τf由负向正变化，而Qf值(Q为品质因数，f为谐振频率)则先增加后减小、当TiO2含量为9.09mol％时Qf取最大值。
实验证明，当x＜25.0mol％或x＞75.0mol％、y＜10.0mol％或y＞30.0mol％、z＜10.0mol％或z＞30.0mol％时、m＜0.8mol％或m＞20mol％时，Qf值将小于80,000GHz，或谐振频率温度系数将偏大(|τf|＞+10ppm/℃)。
在本实施例1～16的所有组分配方中，CaO＝54.55mol％、Sm2O3＝18.18mol％、Al2O3＝18.18mol％、TiO2＝9.09mol％的配方具有最佳的微波介电性能：ε＝21.5，Qf＝200,000GHz，τf＝+3ppm/℃。

Claims (3)

1.一种低损耗微波介质陶瓷，所述低损耗微波介质陶瓷主要组分表达式为：xCaO.yLn2O3.zAl2O3.mTiO2，其中Ln为Nd或Sm，x、y、z、m依次为CaO、Ln2O3、Al2O3、TiO2的摩尔含量，25.0mol％≤x≤75.0mol％，10.0mol％≤y≤30.0mol％，10.0％≤z≤30.0mol％，0.8mol％≤m≤20.0mol％，x+y+z+m＝100mol％。
2.如权利要求1所述的低损耗微波介质陶瓷，其特征在于：45.0mol％≤x≤60.0mol％，15.0mol％≤y≤25.0mol％，15.0mol％≤z≤25.0mol％，4.0mol％≤m≤20.0mol％。
3.如权利要求2所述的低损耗微波介质陶瓷，其特征在于：Ln为Sm，x＝54.55mol％，y＝18.18mol％，z＝18.18mol％，m＝9.09mol％。
CNA2008100610469A 2008-04-25 2008-04-25 一种低损耗微波介质陶瓷 Pending CN101565300A (zh)

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Cited By (14)

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CN101717242B (zh) * 2009-12-04 2012-07-18 安徽华东光电技术研究所 用于微波电真空器件的含TiO2衰减瓷及其制备方法
CN102603287A (zh) * 2012-03-15 2012-07-25 南京工业大学 一种中介电常数微波介质陶瓷及其制备方法
CN104270116A (zh) * 2014-09-16 2015-01-07 张家港保税区灿勤科技有限公司 调谐螺杆及其制备工艺与使用其的l波段lc可调滤波器
CN108821768A (zh) * 2018-08-02 2018-11-16 广东国华新材料科技股份有限公司 一种微波介质陶瓷材料及其制备方法
CN109704764A (zh) * 2019-01-15 2019-05-03 深圳顺络电子股份有限公司 中介电高q微波介电陶瓷材料、陶瓷体及其制备方法
CN110423117A (zh) * 2019-07-15 2019-11-08 深圳顺络电子股份有限公司 一种高q值微波介质陶瓷材料及其制备方法
CN110511028A (zh) * 2019-09-03 2019-11-29 浙江大学 超低损耗微波介质陶瓷
CN110950656A (zh) * 2019-12-18 2020-04-03 广东国华新材料科技股份有限公司 一种复合微波介质陶瓷及其制备方法
CN111574225A (zh) * 2020-05-30 2020-08-25 张保林 微波介质陶瓷滤波器干压一次成型方法及其陶瓷滤波器
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