CN107382314A - 一种钡基复合钙钛矿结构的微波介质陶瓷 - Google Patents

一种钡基复合钙钛矿结构的微波介质陶瓷 Download PDF

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CN107382314A
CN107382314A CN201710516242.XA CN201710516242A CN107382314A CN 107382314 A CN107382314 A CN 107382314A CN 201710516242 A CN201710516242 A CN 201710516242A CN 107382314 A CN107382314 A CN 107382314A
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李玲霞
张博文
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Abstract

本发明公开了一种钡基复合钙钛矿结构微波介质陶瓷Ba3Zn(Nb2‑xMox)O9+x/2(x﹦0.006~0.009),材料介质体系组成简单,采用非化学计量比,内部含有微量的晶格缺陷,有助于烧结过程中的元素扩散与重排;煅烧过程采用煅烧+球磨+煅烧的预烧工艺,使得物相的合成更加完全,没有杂相;烧结温度为1400‑1450℃,烧结与退火过程采用同种组分埋烧并加盖烧,既防止了元素的挥发,又可避免不同组分埋烧带来的杂质元素的引入,保证了烧结过程体系化学组分的一致;采用后退火工艺进一步改善了体系内的元素有序分布状况,提高了体系的微波介电性能。本发明能够满足新兴的5G通讯网络28GHz的Ka波段通信需求,介电常数为36~39,品质因数(Qf)为90,000~110,000GHz,谐振频率温度系数为‑22~24ppm/℃。

Description

一种钡基复合钙钛矿结构的微波介质陶瓷
技术领域
本发明属于一种以成分为特征的介质材料组合物,特别涉及一种Ba3Zn(Nb2-xMox)O9+x/2(x﹦0.006~0.009)中介、高Q、B位有序的微波介质陶瓷及制备方法。
背景技术
近年来微波通讯技术迅猛发展,微波介质材料得到广泛的研究与应用。微波介质陶瓷是具有质量轻、成本低、介电常数高、损耗低、谐振频率温度系数小等特点,在制造介质谐振器、介质滤波器、介质振荡器、介质谐振天线、双工器、电容器、介质基板等微波电子元器件时得到大量的应用。现代通信技术不断发展,传统的2G~4G通信网络难以满足越来越高的信息传输速度的要求。最近,美国、日本、中国等国家纷纷开展5G通讯网络的研究与测试。与传统的2G~4G通信网络采用<2.5GHz通信频段不同,新兴的5G通讯网络将采用28GHz的Ka波段作为通信波段。一般而言微波介质陶瓷的Qf值为常数(其中Q=1/tanδ,f为测试频率),随着应用频率的提高,其Q值将反比例下降。因此考虑到5G的28GHz的通信频率,需要材料的Qf≥90,000GHz,然而目前的微波介质陶瓷体系大都很难满足这一要求。
本发明针对目前国内外急需高Qf微波介质材料的现象,采用传统固相法制备粉体,采用同种组分埋烧、盖烧,并结合退火工艺,制备出了中介、高Q有序微波介质陶瓷Ba3Zn(Nb2-xMox)O9+x/2,能够满足新兴的5G通讯网络28GHz的Ka波段通信需求。最终获得的B位有序Ba3Zn(Nb2-xMox)O9+x/2介质陶瓷具有优异的微波介电性能,介电常数为36~39,品质因数(Qf)为90,000~110,000GHz,谐振频率温度系数为-22~24ppm/℃。
发明内容
本发明的目的,是为满足新兴的5G通讯网络28GHz的Ka波段通信需求,提供一种中介、高Q、B位有序的微波介质陶瓷材料Ba3Zn(Nb2-xMox)O9+x/2(x﹦0.006~0.009)。
本发明的材料介质体系组成简单,采用非化学计量比,内部含有微量的晶格缺陷,有助于烧结过程中的元素扩散与重排;煅烧过程采用煅烧+球磨+煅烧的预烧工艺,使得物相的合成更加完全,没有杂相;烧结与退火过程采用同种组分埋烧加盖烧,既防止了元素的挥发,又可避免不同组分埋烧带来的杂质元素的引入,保证了烧结过程体系化学组分的一致;采用后退火工艺进一步改善体系内的元素有序分布状况,提高体系的微波介电性能。
本发明采用分析纯原料,具体实施步骤如下:
一种钡基复合钙钛矿结构的微波介质陶瓷,其化学式为Ba3Zn(Nb2-xMox)O9+x/2,其中x﹦0.006~0.009;
该钡基复合钙钛矿结构微波介质陶瓷的制备方法,具有如下步骤:
(1)将BaCO3、ZnO、Nb2O5、MoO3按质摩尔百分比3:1:2-x:x配料,与无水乙醇混合球磨8h后烘干并于1200℃预烧4h,制得Ba3Zn(Nb2-xMox)O9+x/2固体颗粒;
(2)将步骤(1)预烧所得Ba3Zn(Nb2-xMox)O9+x/2固体颗粒在无水乙醇中进行二次球磨,球磨时间8h,烘干后,过40目筛得到原料粉末;
(3)将步骤(2)所得Ba3Zn(Nb2-xMox)O9+x/2原料粉末于1200℃再次煅烧4h;
(4)将步骤(3)煅烧后所得Ba3Zn(Nb2-xMox)O9+x/2中外加质量分数为10%的PVA水溶液于无水乙醇中球磨12h;
(5)将步骤(4)球磨后所得粉料烘干,然后过1000孔/cm3分样筛,在200MPa压强下压制成生坯;
(6)将步骤(5)所得生坯使用相同组分埋烧并加盖烧的方式烧结,经3~4h升温至600℃排PVA,经过3h~4h升至1400-1450℃,保温6h,控制降温速率2℃/min降至1100℃,然后随炉冷却至室温;
(7)将步骤(6)所得制品进行后退火,退火过程仍然使用相同组分埋烧并加盖烧的方式,经4~5h升温至1300℃,保温10h,控制降温速率2℃/min降至1100℃,然后随炉冷却至室温,制成钡基复合钙钛矿结构微波介质陶瓷。
所述步骤(3)的PVA水溶液的质量浓度为5wt%。
所述步骤(6)的烧结温度为1435℃。
本发明提供的中介、高Q、B位有序的微波介质陶瓷Ba3Zn(Nb2-xMox)O9+x/2(x﹦0.006~0.009),成瓷致密度高,微波介电性能优异,能够满足新兴的5G通讯网络28GHz的Ka波段通信需求。介电常数为36~39,品质因数(Qf)为90,000~110,000GHz,谐振频率温度系数为-22~24ppm/℃。本发明配方简单,过程环保,微波传输新能优异,适用于5G通讯网络高速通信的发展要求。
具体实施方式
本发明具体实施方式如下:
(1)本发明采用分析纯原料,将BaCO3、ZnO、Nb2O5、MoO3按质摩尔百分比3:1:2-x:x配料,与无水乙醇混合球磨8h后烘干并于1200℃预烧4h,制得Ba3Zn(Nb2-xMox)O9+x/2(x﹦0.006~0.009)固体颗粒;
将步骤(1)预烧所得Ba3Zn(Nb2-xMox)O9+x/2(x﹦0.006~0.009)固体颗粒在无水乙醇中进行二次球磨,球磨时间8h,烘干后,过40目筛得到粉末;
将步骤(2)所得Ba3Zn(Nb2-xMox)O9+x/2(x﹦0.006~0.009)于1200℃再次煅烧4h;
将步骤(3)所得Ba3Zn(Nb2-xMox)O9+x/2(x﹦0.006~0.009)加入质量分数为10%的PVA水溶液(PVA水溶液浓度5wt%)于无水乙醇中球磨12h;
将步骤(4)所得粉料烘干,然后过1000孔/cm3分样筛,在200MPa压强下压制成生坯;
将步骤(5)所得生坯使用相同组分埋烧并加盖烧的方式烧结,经3~4h升温至600℃排PVA,经过3h~4h升至1400-1450℃,保温6h,控制降温速率2℃/min降至1100℃,然后随炉冷却至室温;
将步骤(6)所得制品进行后退火,退火过程仍然使用相同组分埋烧加盖烧的方式。经4~5h升温至1300℃,保温10h,控制降温速率2℃/min降至1100℃,然后随炉冷却至室温;
最后通过网络分析仪及相关测试夹具测试制品的微波介电性能。
具体实施例1~8的主要工艺指标及其微波介电性能的测试结果详见表1。
表1中谐振频率温度系数τf值的测定温区范围是25℃~85℃。
表1

Claims (3)

1.一种钡基复合钙钛矿结构的微波介质陶瓷,其化学式为Ba3Zn(Nb2-xMox)O9+x/2,其中x﹦0.006~0.009。
该钡基复合钙钛矿结构微波介质陶瓷的制备方法,具有如下步骤:
(1)将BaCO3、ZnO、Nb2O5、MoO3按质摩尔百分比3:1:2-x:x配料,与无水乙醇混合球磨8h后烘干并于1200℃预烧4h,制得Ba3Zn(Nb2-xMox)O9+x/2固体颗粒;
(2)将步骤(1)预烧所得Ba3Zn(Nb2-xMox)O9+x/2固体颗粒在无水乙醇中进行二次球磨,球磨时间8h,烘干后,过40目筛得到原料粉末;
(3)将步骤(2)所得Ba3Zn(Nb2-xMox)O9+x/2原料粉末于1200℃再次煅烧4h;
(4)将步骤(3)煅烧后所得Ba3Zn(Nb2-xMox)O9+x/2中外加质量分数为10%的PVA水溶液于无水乙醇中球磨12h;
(5)将步骤(4)球磨后所得粉料烘干,然后过1000孔/cm3分样筛,在200MPa压强下压制成生坯;
(6)将步骤(5)所得生坯使用相同组分埋烧并加盖烧的方式烧结,经3~4h升温至600℃排PVA,经过3h~4h升至1400-1450℃,保温6h,控制降温速率2℃/min降至1100℃,然后随炉冷却至室温;
(7)将步骤(6)所得制品进行后退火,退火过程仍然使用相同组分埋烧并加盖烧的方式,经4~5h升温至1300℃,保温10h,控制降温速率2℃/min降至1100℃,然后随炉冷却至室温,制成钡基复合钙钛矿结构微波介质陶瓷。
2.根据权利要求1所述的一种钡基复合钙钛矿结构微波介质陶瓷,其特征在于,所述步骤(3)的PVA水溶液的质量浓度为5wt%。
3.根据权利要求1所述的一种钡基复合钙钛矿结构微波介质陶瓷,其特征在于,所述步骤(6)的烧结温度为1435℃。
CN201710516242.XA 2017-06-29 2017-06-29 一种钡基复合钙钛矿结构的微波介质陶瓷 Pending CN107382314A (zh)

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