CN110563448B - 一种三元石榴石微波介质材料的制备方法 - Google Patents

一种三元石榴石微波介质材料的制备方法 Download PDF

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CN110563448B
CN110563448B CN201910820411.8A CN201910820411A CN110563448B CN 110563448 B CN110563448 B CN 110563448B CN 201910820411 A CN201910820411 A CN 201910820411A CN 110563448 B CN110563448 B CN 110563448B
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周焕福
卢承铭
陈秀丽
张海林
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Abstract

本发明公开了一种三元石榴石微波介质材料的制备方法。以纯度≥99%的M盐、Al2O3和GeO2为主要原料，按M3Al2(GeO4)3配料，将物料湿式球磨混合4h，以无水乙醇为球磨介质，干燥后在1100℃空气气氛下预烧4h；将预烧后的粉体进行二次球磨后添加5 wt%聚乙烯醇进行造粒，造粒后压制成型，即制得三元石榴石微波介质材料。所述M盐为石榴石结构的盐，具体为CaCO3或MnO2。本发明方法操作简单，制备的三元石榴石微波介质材料的烧结温度处于1225~1350℃之间，介电常数低（5.8~7.3），Q×f值高（38085~104148GHz），谐振频率温度系数（τ f ）较小，可用于谐振器、天线、滤波器等微波器件的制造。

Description

一种三元石榴石微波介质材料的制备方法
技术领域
本发明属于电子陶瓷及其制造领域，涉及在微波频率使用的介质基板、天线和谐振器等微波元器件的三元石榴石微波介质材料的制备方法。
背景技术
微波介质材料是指应用于微波频段（300MHz~300GHz）电路中作为介质并完成一种或多种功能的陶瓷，主要用于制备谐振器、滤波器、介质天线、介质导波回路等微波元器件。近年来，随着微波元器件不断向低成本化、小型化以及轻量化方向的发展，这要求微波介质材料具有优良的微波介电性能（高的Q×f值，适中的介电常数、近零的τ f 值）、低的密度。尽管目前报道了很多性能优异的微波介电材料，比如：Ba(Zn1/3Nb2/3)O3，Ba(Mg1/3Nb2/3)O3，Ba(Y1/2Ta1/2)O3。但是高的烧结温度、大的密度以及较贵的生产原料限制了其在商业上的应用。随着微波通信技术向毫米波段延伸新型毫米波器件和系统快速发展并在雷达、通信、遥感和高速数据传输等领域获得广泛应用。在极高频的毫米波段下介质材料需具有较低的介电常数、极低的介质损耗和近零的谐振频率温度系数，以提高器件的信息传输速率、增强选频性和降低能耗、保证谐振与传输时信号的工作稳定性。低介电常数(τ f <15)、极低介质损耗(tanδ<2x10-4，f~10GHz)和谐振频率温度稳定性好的微波介质陶瓷的开发成为介质材料的研究热点。
我们对组成为Ca3Al2(GeO4)3和Mn3Al2(GeO4)3的陶瓷进行了烧结特性与微波介电性能研究，结果发现该类陶瓷具有优异的综合微波介电性能可广泛用于各种谐振器和滤波器等微波器件的制造，可满足微波多层器件的需要。
发明内容
本发明的目的是提供一种三元石榴石微波介质材料的制备方法。
具体步骤为：
以纯度≥99%的M盐、Al2O3和GeO2为主要原料，按M3Al2(GeO4)3配料进行称量，然后混料，得混合粉体；按照无水乙醇与混合粉体质量比为1:1的比例向混合粉体中加入无水乙醇，采用湿磨法混合4小时，然后在120~130℃下烘干，以80目的筛网过筛，过筛后压制成块状原料，然后以5℃/min的升温速率将压制的块状原料由室温升至1100℃并在此温度下保温4小时制成烧块，将烧块粉碎成粉料，按照无水乙醇与粉料质量比为1:1的比例向粉料中加入无水乙醇，放入尼龙罐中球磨4小时后取出，放入120~130℃烘炉内烘干，所得粉体添加5 wt%聚乙烯醇进行造粒，造粒后压制成直径为12mm、厚度为6mm的小圆柱，于500~600℃排胶4小时，随炉冷却后得到瓷料，再将瓷料在1225~1350℃下烧结4小时，即制得三元石榴石微波介质材料。
所述M盐为石榴石结构的盐，具体为CaCO3或MnO2。
本发明方法操作简单，制备的三元石榴石微波介质材料的微波性能优异：介电常数（ε r ）低，Q×f值高以及τ f 值小，可用于谐振器、天线、滤波器等微波器件的制造。
具体实施方式
实施例1:
以纯度=99%的CaCO3、Al2O3和GeO2为主要原料，按Ca3Al2(GeO4)3配料进行称量，然后混料，得混合粉体；按照无水乙醇与混合粉体质量比为1:1的比例向混合粉体中加入无水乙醇，采用湿磨法混合4小时，然后在125℃下烘干，以80目的筛网过筛，过筛后压制成块状原料，然后以5℃/min的升温速率将压制的块状原料由室温升至1100℃并在此温度下保温4小时制成烧块，将烧块粉碎成粉料，按照无水乙醇与粉料质量比为1:1的比例向粉料中加入无水乙醇，放入尼龙罐中球磨4小时后取出，放入125℃烘炉内烘干，所得粉体添加5 wt%聚乙烯醇进行造粒，造粒后压制成直径为12mm、厚度为6mm的小圆柱，于550℃排胶4小时，随炉冷却后得到瓷料，再将瓷料在1250℃下烧结4小时，即制得三元石榴石微波介质材料。
实施例2:
将最后的烧结温度改为1275℃，其他步骤同实施例1。
实施例3:
将最后的烧结温度改为1300℃，其他步骤同实施例1。
实施例4:
将最后的烧结温度改为1325℃，其他步骤同实施例1。
实施例5:
将最后的烧结温度改为1350℃，其他步骤同实施例1。
实施例6:
以纯度=99%的MnO2、Al2O3和GeO2为主要原料，按Mn3Al2(GeO4)3配料进行称量，然后混料，得混合粉体；按照无水乙醇与混合粉体质量比为1:1的比例向混合粉体中加入无水乙醇，采用湿磨法混合4小时，然后在125℃下烘干，以80目的筛网过筛，过筛后压制成块状原料，然后以5℃/min的升温速率将压制的块状原料由室温升至1100℃并在此温度下保温4小时制成烧块，将烧块粉碎成粉料，按照无水乙醇与粉料质量比为1:1的比例向粉料中加入无水乙醇，放入尼龙罐中球磨4小时后取出，放入125℃烘炉内烘干，所得粉体添加5 wt%聚乙烯醇进行造粒，造粒后压制成直径为12mm、厚度为6mm的小圆柱，于550℃排胶4小时，随炉冷却后得到瓷料，再将瓷料在1225℃下烧结4小时，即制得三元石榴石微波介质材料。
实施例7:
将最后的烧结温度改为1250℃，其他步骤同实施例6。
实施例8:
将最后的烧结温度改为1275℃，其他步骤同实施例6。
实施例9:
将最后的烧结温度改为1300℃，其他步骤同实施例6。
实施例10:
将最后的烧结温度改为1325℃，其他步骤同实施例6。
表1列出了实施例1~10的烧结温度以及制得的三元石榴石微波介质材料的微波介电性能。用圆柱介质谐振器法进行微波介电性能的评价。
本陶瓷可广泛用于各种介质基板、天线和滤波器等微波电子元器件的制造，满足现代移动通信系统的技术需要。
表1 三元石榴石微波介质材料的微波介电性能
Figure 156471DEST_PATH_IMAGE002
。

Claims (1)

1.一种三元石榴石微波介质材料的制备方法，其特征在于具体步骤为：
以纯度≥99%的M盐、Al2O3和GeO2为主要原料，按M3Al2(GeO4)3配料进行称量，然后混料，得混合粉体；按照无水乙醇与混合粉体质量比为1:1的比例向混合粉体中加入无水乙醇，采用湿磨法混合4小时，然后在120~130℃下烘干，以80目的筛网过筛，过筛后压制成块状原料，然后以5℃/min的升温速率将压制的块状原料由室温升至1100℃并在此温度下保温4小时制成烧块，将烧块粉碎成粉料，按照无水乙醇与粉料质量比为1:1的比例向粉料中加入无水乙醇，放入尼龙罐中球磨4小时后取出，放入120~130℃烘炉内烘干，所得粉体添加5 wt%聚乙烯醇进行造粒，造粒后压制成直径为12mm、厚度为6mm的小圆柱，于500~600℃排胶4小时，随炉冷却后得到瓷料，再将瓷料在1225~1350℃下烧结4小时，即制得三元石榴石微波介质材料；
所述M盐为石榴石结构的盐，具体为CaCO3或MnO2。
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