CN107010942B - 一种高q值通信用陶瓷介质谐振器 - Google Patents

一种高q值通信用陶瓷介质谐振器 Download PDF

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CN107010942B
CN107010942B CN201710201508.1A CN201710201508A CN107010942B CN 107010942 B CN107010942 B CN 107010942B CN 201710201508 A CN201710201508 A CN 201710201508A CN 107010942 B CN107010942 B CN 107010942B
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陈功田
肖练平
吴娟英
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Chenzhou Gongtian Electronic Ceramic Technology Co ltd
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Abstract

本发明涉及一种高Q值通信用陶瓷介质谐振器。该微波介质陶瓷的制造原料含有:二氧化钛(TiO2),碳酸钙(CaCO3),氧化铝(Al2O3)和氧化钐(Sm2O3)氧化镧(La2O3)等以及微量掺杂添加物碳酸锂(Li2CO3)、氧化锰(MnO)、氧化铈(CeO2)等组分;将上述组分经过配料、混合球磨、造粒、成型、装钵、排胶和烧结的固相反应工序烧制成微波介质陶瓷。本发明具有较低的烧结温度、节能环保、中介电常数、高品质因数和稳定的谐振频率温度特性。

Description

一种高Q值通信用陶瓷介质谐振器
技术领域
本发明涉及一种高Q值通信用陶瓷介质谐振器,应用于L波段卫星通信与移动通信系统中介质谐振器、滤波器以及振荡器和GPS全球定位系统等微波元器件中。
背景技术
目前,随着我国航天科技、卫星通讯的快速发展,届时将形成多波段的固定广播通信卫星、专用广播卫星、直播卫星、移动广播卫星、移动通信卫星和专用GPS全球定位,安全导航卫星。以及以IP 业务为主的数据业务对传输带宽需求的进一步增长,更长波长的L 波段的开发和应用越来越成为人们关注的重点。同时也带动了对相应的微波谐振器、滤波器、振荡器、微波电容器等相关微波元器件的需求。卫星通讯广播通常应用的频率为S、L、C、Ku波段,对于应用于L波段的微波介质陶瓷要求具有高的介电常数(65~85)、高品质因数稳定的谐振频率温度特性和体积小,价格便宜等。
CaTiO3,SmAlO3及LaAlO3材料是一种性能优异的钛酸盐、铝酸盐微波陶瓷,通过掺杂及其它手段可以获得具有合适的且可调的介电常数,高品质因数和良好稳定的谐振频率温度特性。在现有技术中CaTiO3,SmAlO3及LaAlO3一般采用氧化物与添加剂混合固相高温反应法制备,经过配料、球磨、造粒、成型、装钵、排胶和烧结等工序,最后进行陶瓷性能的检测。该方法工艺简单,易于工业自动化生产,且材料性能稳定。
发明内容
本发明所要解决的技术问题是:提供一种高Q值通信用陶瓷介质谐振器,其具有较低的烧结温度、中介电常数、高品质因数和稳定的谐振频率温度特性。其应用于L波段介质谐振器、滤波器、振荡器、GPS全球定位,安全导航系统中,可以使体积小、价格便宜。
本发明解决的技术方案如下:
一种高Q值通信用陶瓷介质谐振器,制造原料中含有:二氧化钛( TiO2),碳酸钙(CaCO3),氧化铝(Al2O3)和氧化钐(Sm2O3)氧化镧(La2O3)以及微量掺杂添加物组分;其特征是:所述微量掺杂添加物是碳酸锂(Li2CO3)氧化锰(MnO)与氧化铈(CeO2)组分;各组分的含量的重量百分比为:
二氧化钛 20%~30%; 碳酸钙 28%~35%;
氧化铝 4%~10%; 氧化钐 17%~32 %;
氧化镧 8%~15%;
碳酸锂 0.05%~0.2%;
氧化锰 0.1%~0.45%;
氧化铈 0.1%~0.3%;
将上述组分经过配料、混合球磨、造粒、成型、装钵、排胶和烧结的固相反应工序烧制成微波介质陶瓷。
一种高Q值通信用陶瓷介质谐振器的具体制造方法是:
①先将粉末状的 二氧化钛、碳酸钙、氧化铝、氧化钐、氧化镧以及微量掺杂添加物按组分要求配料,放入球磨机的料筒中搅拌球磨6-8小时;
②将搅拌球磨的料浆干燥造粒:加入总粉体重量的15%PVA水溶液搅拌均匀后进行喷雾造粒;
③干压成型,压制成型的成型压力700-1600MPa,并且装钵;
④在1430-1460℃下保温3~6小时,排胶烧结一次完成即制得高Q值通信用陶瓷介质谐振器。
本发明采用氧化物与添加剂混合固相反应法制备的CaTiO3,SmAlO3及LaAlO3的微晶体,并添加微量掺杂添加物制得的晶粒细小均匀、气孔率低和性能优良的微波介质陶瓷。本发明采用少量的添加碳酸锂(Li2CO3)作为烧结助剂加入配料中,其和TiO2组合形成底共熔点的物质Li2TiO3(900°C),在烧结中产生液相,湿润粉体颗粒,达到液相烧结的效促进烧结,可以降低烧结温度。本发明采用微量的氧化锰(MnO)作为改性剂的加入,Mn离子在高温下不稳定,容易变为+4、+2、+3价的形态存在于晶界上,这种变价离子的存在能很好地中和材料制备过程中引入的施主杂质。在高温烧结过程中,添加微量Mn的钛酸盐中的锰离子可以作为氧化剂,在冷却过程中,Mn3+和Mn4+可以抑制Ti3+的存在。在此过程中Mn3+和Mn4+比Ti4+更容易被还原,有利于改善材料结构,提高Q值。而且氧化锰在高温条件下会产生液相,促进烧结,极大的降低烧结温度,使瓷体致密度增加。因此,适量地掺杂二氧化锰,不仅能促进材料的烧结,还能改善材料的结构,从而提高材料的微波性能,起到改性和助熔的双重作用。本发明采用微量的氧化铈(CeO2)在高温烧结过程中与氧化铝(Al2O3)反应:2CeO2+Al2O3─2CeAlO3+1/2O2(氧产生),在烧结氧缺乏的过程中有氧气氛下烧结可以抑制Ti4+变价,提高陶瓷的介电性能。
经检测试验:本发明上述各添加剂的添加范围内都可以获得很好的微波特性。且国内原料成本低,可进一步加强和国外微波陶瓷的竞争力,加速国产微波陶瓷的大量应用。
与现有技术相比,本发明具有以下特点:
1)本发明的配方组成不含有铅、铬、汞等重金属成分,即本发明提供的是一种环保微波介质陶瓷。符合绿色环保的无污染要求。且符合欧共体最新出台的无铅标准和废旧电器回收标注的RHOS和WEEE的严格标准要求。可以在高频领域产品中应用;能够将产品进行出口到世界的任何国家。
2)由传统的煅烧二步工艺优化成一步法工艺(省去压滤、煅烧工序)大大降低制造成本。
3)由传统的烧结工艺1500-1550℃,降到1450℃以下,烧结温度的进一步降低,具有节能的更大优势。
4)性能上有较大提升:传统技术配方在L波段的介电常数65-80,Q值只有1000-1500,谐振频率温度系数大于±20PPm以上。本发明的材料配方在L波段的介电常数45±1,Q值高达22000以上,谐振频率温度系数小于±3PPm以内。
5)本发明可作为L波段用环保微波用通信谐振器、滤波器和振荡器等电子元器件的关键核心材料使用,而广泛应用于移动通信、卫星通信、全球卫星定位系统(GPS)、蓝牙技术以及无线局域网(WLA)等现代通信行业,具有重要工业应用价值。
附图说明
图1为温度与谐振频率关系特性趋势图。
图2为谐振频率与品质因数图。
图3为品质因数Q值与烧结温度的关系图。
具体实施方式
下面结合附图用具体实施方式详细描述本发明。
一种高Q值通信用陶瓷介质谐振器,微波介质陶瓷的制造原料中含有成分:二氧化钛、碳酸钙、氧化铝、氧化钐、氧化镧,以及微量掺杂添加物组分;其特征是:所述微量掺杂添加物中还含有碳酸锂(Li2CO3)氧化锰(MnO)与氧化铈(CeO2)组分。根据该主成分和微量添加物的配比以及制造方法,表1给出各实施例的数据,表2给出各实施例的性能。
表 1:各原料配比与搅拌时间、烧结温度/时间及Q值数据汇总表
Figure 144848DEST_PATH_IMAGE002
表2:各规格通信谐振器主要性能
Figure 999672DEST_PATH_IMAGE004
从表1中可以明显看出:第1、2、3、5、6、8、9、10号配方掺杂碳酸锂、氧化锰和氧化铈其烧结温度均低于1450℃,而且Q值均高于15000(1.8G),但第4号配方框图未掺杂碳酸锂的烧结温度却高达1550℃,而且Q值明显下降至13000(1.8G),第7号配方未掺杂氧化锰的烧结温度高达1520℃,Q值勤也明显下降至12500(1.8G),所以配方的掺杂改性尤为重要。
图1~3总结出配方和性能的变化趋势,可以方便调整配方,获得所需要性能的微波介质陶瓷。
图1中的温度与谐振频率偏移关系特性趋势图表示谐振频率在-40℃~+90℃间变化,谐振频率为1.8GHz的介质频率偏在0.5MHz以内(Tf< 3ppm/℃),频率稳定特性很好。上面的Tf表示谐振频率温度系数;△f表示谐振频偏;T表示温度。
图2中的谐振频率与品质因数Q值的关系曲线,随频率的升高,Q值会下降,到频率10GHz后,Q值降到1000以下,随着频率的继续升高,Q值会急剧下降,说明此配方介质陶瓷可以用到谐振频率10GHz以下的谐振电路中是比较合适。
图3中的品质因数Q值与烧结温度的关系曲线图,说明最佳的烧结温度在1450℃左右,具有较宽的烧结温度范围。且该介质陶瓷适合低中温烧结,烧结温度不宜过高。

Claims (1)

1.一种高Q值通信用陶瓷介质谐振器,制造原料中含有:二氧化钛,碳酸钙,氧化铝和氧化钐氧化镧以及微量掺杂添加物组分;其特征是:所述微量掺杂添加物是碳酸锂氧化锰与氧化铈组分;各组分的含量的重量百分比为:
二氧化钛 20%; 碳酸钙 29.5%;
氧化铝 10%; 氧化钐 32%;
氧化镧 8%; 碳酸锂 0.10%;
氧化锰 0.30%; CeO2 0.10%;
将上述组分经过配料、混合球磨、造粒、成型、装钵、排胶和烧结的固相反应工序烧制成微波介质陶瓷。
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