CN107253856A - 一种近零谐振频率温度系数的微波介质材料及其制备方法 - Google Patents

一种近零谐振频率温度系数的微波介质材料及其制备方法 Download PDF

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CN107253856A
CN107253856A CN201710496755.9A CN201710496755A CN107253856A CN 107253856 A CN107253856 A CN 107253856A CN 201710496755 A CN201710496755 A CN 201710496755A CN 107253856 A CN107253856 A CN 107253856A
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周焕福
黄瑾
陈秀丽
阮红
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Abstract

本发明公开了一种近零谐振频率温度系数的微波介质材料及其制备方法。该微波介质材料的化学组成式为:(1‑x)(3MgO‑Al2O3‑3TiO2)‑xCaTiO3,其中x为摩尔分数,且0.1≤x≤0.3。以纯度≥99%的Al2O3、MgO和TiO2为主要原料,按3MgO‑Al2O3‑3TiO2进行称量,混合制得3MgO‑Al2O3‑3TiO2粉体;以纯度≥99%的CaCO3和TiO2为主要原料,按CaTiO3进行称料,混合制得CaTiO3粉体。以3MgO‑Al2O3‑3TiO2粉体和CaTiO3粉体为原料,按(1‑x)(3MgO‑Al2O3‑3TiO2)‑xCaTiO3进行称料,经过混合、造粒后压制、排胶、随炉冷却、烧结等步骤制得近零谐振频率温度系数的微波介质材料。本发明方法操作简单,且制备的微波介质材料微波性能优异,可用于谐振器、天线、滤波器等微波器件的制造。

Description

一种近零谐振频率温度系数的微波介质材料及其制备方法
技术领域
本发明属于电子陶瓷及其制造领域,特别涉及一种近零谐振频率温度系数的微波介质材料及其制备方法,该微波介质材料用于制备介质基板、天线和谐振器等微波元器件。
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、高频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,低的介电常数、近零的τ f 值)、低的生产成本、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。但是较大的谐振频率温度系数限制了其在商业上的应用。目前最常用的调节温度系数的方法主要有以下三种:(1)添加具有相反温度系数的材料形成混合相;(2)添加具有相反温度系数的材料形成固溶体;(3)开发新体系。目前,使用最多的方法是添加具有相反温度系数的材料形成混合相。
发明内容
本发明的目的是提供一种近零谐振频率温度系数的微波介质材料及其制备方法。
本发明思路:3MgO-Al2O3-3TiO2体系具有优良的微波介电性能,但是温度系数较负,而CaTiO3具有正的τ f 值(~800 ppm/℃),通过向3MgO-Al2O3-3TiO2体系中添加CaTiO3调节3MgO-Al2O3-3TiO2材料的τ f 值,从而获得一种近零谐振频率温度系数的微波介质材料。本发明通过引入添加剂CaTiO3调节τ f 值,从而获得一种温度系数近零且性能优异的微波介质陶瓷材料。
本发明的近零谐振频率温度系数的微波介质材料的化学组成式为:(1-x)(3MgO-Al2O3-3TiO2)-xCaTiO3,其中x为摩尔分数,且0.1≤x≤0.3。
制备上述近零谐振频率温度系数的微波介质材料的具体步骤为:
(1)以纯度≥99%的Al2O3、MgO和TiO2为主要原料,先按3MgO-Al2O3-3TiO2进行称量,然后混合制得混合料;按照无水乙醇与混合料质量比为1:1的比例向混合料中加入无水乙醇,采用湿磨法混合4小时,磨细后在120~140℃下烘干,以60目的筛网过筛,过筛后压制成块状,然后以5℃/min的升温速率将压制的块状原料由室温升至1225℃并在此温度下保温4小时,制成3MgO-Al2O3-3TiO2样品,将制得的3MgO-Al2O3-3TiO2样品粉碎,分别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,放入烘炉内在120~140℃下烘干,制得3MgO-Al2O3-3TiO2粉体。
(2)以纯度≥99%的CaCO3和TiO2为主要原料,按CaTiO3进行称料,然后混合制得混合料;按照无水乙醇与混合料质量比为1:1的比例向混合料中加入无水乙醇,采用湿磨法混合4小时,磨细后在120~140℃下烘干,以60目的筛网过筛,过筛后压制成块状,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CaTiO3样品,将制得的CaTiO3样品粉碎,分别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,放入烘炉内在120~140℃下烘干,制得CaTiO3粉体。
(3)以步骤(1)制得的3MgO-Al2O3-3TiO2粉体和步骤(2)制得的CaTiO3粉体为原料,按(1-x)(3MgO-Al2O3-3TiO2)-xCaTiO3进行称料,其中x为摩尔分数,且0.1≤x≤0.3,然后混合制得混合料;按照无水乙醇与混合料质量比为1:1的比例向混合料中加入无水乙醇,采用湿磨法混合4小时,磨细后在120~140℃下烘干,制得混合粉体。
(4)将步骤(3)制得的混合粉体造粒后压制成直径为12mm,厚度为6mm的小圆柱,于500~600℃下排胶4小时,随炉冷却后得到瓷料,再将瓷料在1275~1350℃下烧结4小时即制得近零谐振频率温度系数的微波介质材料。
本发明方法操作简单,且制备的近零谐振频率温度系数的微波介质材料,微波性能优异:低的介电常数(ε r ),高的Q×f值以及较小的τ f 值;其中0.8(3MgO-Al2O3-3TiO2)+0.2CaTiO3组分在1325℃下烧结具有较好的性能(ε r ~17.6, Q × f∼36606 GHz, τ f ~ 4.63ppm/℃),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:
(1)以纯度≥99%的Al2O3、MgO和TiO2为主要原料,先按3MgO-Al2O3-3TiO2进行称量,然后混合制得混合料;按照无水乙醇与混合料质量比为1:1的比例向混合料中加入无水乙醇,采用湿磨法混合4小时,磨细后在130℃下烘干,以60目的筛网过筛,过筛后压制成块状,然后以5℃/min的升温速率将压制的块状原料由室温升至1225℃并在此温度下保温4小时,制成3MgO-Al2O3-3TiO2样品,将制得的3MgO-Al2O3-3TiO2样品粉碎,分别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,放入烘炉内在130℃下烘干,制得3MgO-Al2O3-3TiO2粉体。
(2)以纯度≥99%的CaCO3和TiO2为主要原料,按CaTiO3进行称料,然后混合制得混合料;按照无水乙醇与混合料质量比为1:1的比例向混合料中加入无水乙醇,采用湿磨法混合4小时,磨细后在130℃下烘干,以60目的筛网过筛,过筛后压制成块状,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CaTiO3样品,将制得的CaTiO3样品粉碎,分别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,放入烘炉内在130℃下烘干,制得CaTiO3粉体。
(3)以步骤(1)制得的3MgO-Al2O3-3TiO2粉体和步骤(2)制得的CaTiO3粉体为原料,按0.9(3MgO-Al2O3-3TiO2)-0.1CaTiO3进行称料,然后混合制得混合料;按照无水乙醇与混合料质量比为1:1的比例向混合料中加入无水乙醇,采用湿磨法混合4小时,磨细后在130℃下烘干,制得混合粉体。
(4)将步骤(3)制得的混合粉体造粒后压制成直径为12mm,厚度为6mm的小圆柱,于550℃下排胶4小时,随炉冷却后得到瓷料,再将瓷料在1275℃下烧结4小时即制得近零谐振频率温度系数的微波介质材料。用圆柱介质谐振器法对本实施例制得的微波介质材料进行微波介电性能的评价,结果见表1。
实施例2~12:
将3MgO-Al2O3-3TiO2简写为MAT,CaTiO3简写为CT。实施例2~12的制备步骤同实施例1,x的取值和步骤(4)中的烧结温度见表1,用圆柱介质谐振器法对实施例2~12制得的微波介质材料进行微波介电性能的评价,结果见表1。
实施例1~12中制得的微波介质材料能够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不同成分的12个具体实施例及其微波介电性能

Claims (2)

1.一种近零谐振频率温度系数的微波介质材料,其特征在于该近零谐振频率温度系数的微波介质材料的化学组成式为:(1-x)(3MgO-Al2O3-3TiO2)-xCaTiO3,其中x为摩尔分数,且0.1≤x≤0.3。
2.一种如权利要求1所述的近零谐振频率温度系数的微波介质材料的制备方法,其特征在于具体步骤为:
(1)以纯度≥99%的Al2O3、MgO和TiO2为主要原料,先按3MgO-Al2O3-3TiO2进行称量,然后混合制得混合料;按照无水乙醇与混合料质量比为1:1的比例向混合料中加入无水乙醇,采用湿磨法混合4小时,磨细后在120~140℃下烘干,以60目的筛网过筛,过筛后压制成块状,然后以5℃/min的升温速率将压制的块状原料由室温升至1225℃并在此温度下保温4小时,制成3MgO-Al2O3-3TiO2样品,将制得的3MgO-Al2O3-3TiO2样品粉碎,分别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,放入烘炉内在120~140℃下烘干,制得3MgO-Al2O3-3TiO2粉体;
(2)以纯度≥99%的CaCO3和TiO2为主要原料,按CaTiO3进行称料,然后混合制得混合料;按照无水乙醇与混合料质量比为1:1的比例向混合料中加入无水乙醇,采用湿磨法混合4小时,磨细后在120~140℃下烘干,以60目的筛网过筛,过筛后压制成块状,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CaTiO3样品,将制得的CaTiO3样品粉碎,分别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,放入烘炉内在120~140℃下烘干,制得CaTiO3粉体;
(3)以步骤(1)制得的3MgO-Al2O3-3TiO2粉体和步骤(2)制得的CaTiO3粉体为原料,按(1-x)(3MgO-Al2O3-3TiO2)-xCaTiO3进行称料,其中x为摩尔分数,且0.1≤x≤0.3,然后混合制得混合料;按照无水乙醇与混合料质量比为1:1的比例向混合料中加入无水乙醇,采用湿磨法混合4小时,磨细后在120~140℃下烘干,制得混合粉体;
(4)将步骤(3)制得的混合粉体造粒后压制成直径为12mm、厚度为6mm的小圆柱,于500~600℃下排胶4小时,随炉冷却后得到瓷料,再将瓷料在1275~1350℃下烧结4小时即制得近零谐振频率温度系数的微波介质材料。
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CN111943675A (zh) * 2020-08-24 2020-11-17 贵阳顺络迅达电子有限公司 一种基于反应烧结的铝钛酸钕钙微波介质材料制备方法

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