CN107117967B - 一种低温烧结复合微波介质陶瓷材料及其制备方法 - Google Patents
一种低温烧结复合微波介质陶瓷材料及其制备方法 Download PDFInfo
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Abstract
本发明属于电子陶瓷及其制造领域,涉及一种低温烧结复合微波介质陶瓷材料及其制备方法。本发明提供的材料,由质量百分比97%~99.5%的(Zn1‑xCox)0.5Ti0.5(Nb1‑yTay)O4基料和质量百分比0.5%~3%的降烧剂组成,x=0.05~0.95,y=0.05~0.95;主晶相ZnTiNb2O8相,次晶相Zn0.17Nb0.33Ti0.5O2相。本发明在Zn0.5Ti0.5NbO4基础上进行离子掺杂Co2O3和Ta2O5,并在离子掺杂后的体系上掺杂0.5~3wt.%降烧剂,低于900℃烧结温度下烧结致密,在保证微波介电性能优异的前提下,且能够调节体系较正的τf值,介电常数20~34,损耗≤10‑4,频率温度系数稳定‑10ppm/℃≤τf≤+10ppm/℃,制备工艺简单,易于工业化生产。
Description
技术领域
本发明属于电子陶瓷及其制造领域,涉及一种低温烧结复合微波介质陶瓷材料及其制备方法。
背景技术
微波介质陶瓷随着移动通信产业的快速发展,对其需求日益增加,作为现代通信系统的基础材料,微波介质陶瓷材料被广泛应用于介质谐振器、滤波器、介质波导回路、微波电容、双工器、天线等微波元器件,适用于卫星通信及移动通讯基站。
低温共烧陶瓷LTCC(Low Temperature Co-fired Ceramics)技术能够将多个不同类型、不同性能的无源元件集成在一个封装内,是无源集成的主流技术。但LTCC技术要求陶瓷材料能够与Ag、Cu等金属共烧,而一般陶瓷的烧结温度高于1000℃无法实现,因此降低陶瓷材料的烧结温度是应用于LTCC的门槛。
在微波介质陶瓷材料的制备过程中,评判体系性能主要在于以下三点:(1)适宜的介电常数;(2)低的损耗tanδ和高的品质因数Q×f值;(3)稳定近零的谐振频率温度系数。
通常情况下,降烧剂具有负的τf值,在陶瓷-玻璃的混合体系中,根据混合对数规则,为了得到近零的谐振频率温度系数,采取基料为τf为正值的配比。而(Zn1-xCox)0.5Ti0.5(Nb1-yTay)O4(x=0.05~0.95,y=0.05~0.95)陶瓷在1150℃~1200℃烧结下具有较好的微波介电性能及较正的谐振频率温度系数:1175℃,εr=45.15、Q×f=16774GHz、τf=90.17ppm/℃(x=0.3,y=0.4)。
但其烧结温度仍尚高(1150℃~1200℃),不能直接与Ag、Cu等低熔点金属共烧,因此需要引入低熔点的烧结助剂。常用的办法有:(1)低熔点氧化物;(2)低熔点玻璃料烧结助剂;(3)改善工艺条件。相对比而言,低熔点氧化物或低熔点玻璃烧结助剂的工艺相对简单(在基料烧结后按质量比加入),易于批量生产。
发明内容
针对上述存在问题或不足,本发明提供了一种低温烧结复合微波介质陶瓷材料及其制备方法。
本发明提供的材料,由质量百分比97%~99.5%的(Zn1-xCox)0.5Ti0.5(Nb1-yTay)O4(x=0.05~0.95,y=0.05~0.95)基料和质量百分比0.5%~3%的降烧剂组成。
基料原料组分是ZnO、Co2O3、TiO2、Nb2O5和Ta2O5按照化学通式(Zn1-xCox)0.5Ti0.5(Nb1-yTay)O4配比,x=0.05~0.95,y=0.05~0.95;
降烧剂原料组分的重量百分比为:32.42%≤Li2CO3≤40.04%,42.54%≤H3BO3≤54.26%,2.56%≤SiO2≤6.33%,0%<ZnO≤2.54%,0%<Al2O3≤18.25%;以及微量的添加物0%<MnCO3≤0.4%和0%<CuO≤1.2%,两者重量比为1:3。
主晶相为ZnTiNb2O8相,次晶相为Zn0.17Nb0.33Ti0.5O2相,烧结温度≤900℃,体系致密,具有中等介电常数(20~34),损耗≤10-4,频率温度系数稳定(-10ppm/℃≤τf≤+10ppm/℃),制备工艺简单,易于工业化生产。
其制备方法如下:
步骤1:将ZnO、Co2O3、TiO2、Nb2O5和Ta2O5的原始粉料按照(Zn1-xCox)0.5Ti0.5(Nb1- yTay)O4(x=0.05~0.95,y=0.05~0.95)化学通式进行配料;
步骤2:将步骤1所得配料装入球磨罐,以锆球及去离子水作为研磨介质,按照配料:锆球:去离子水质量比1:3~7:1~3行星球磨4~7小时,然后在80~100℃烘干,以40~60目筛网过筛,最后在800~1200℃大气气氛中预烧2~4小时合成主晶相ZnTiNb2O8相;
步骤3:按32.42%≤Li2CO3≤40.04%,42.54%≤H3BO3≤54.26%,2.56%≤SiO2≤6.33%,0%<ZnO≤2.54%,0%<Al2O3≤18.25%,0%<MnCO3≤0.4%,0%<CuO≤1.2%,MnCO3:CuO重量比1:3配料,然后装入球磨罐中,球磨4~7小时,待烘干过筛后,再于500℃~800℃下预烧2~6小时,最后在1100℃~1500℃保温1~5小时熔融玻璃渣,将制备的玻璃渣再破碎球磨成粉制得降烧剂;
步骤4:在步骤2制得的预烧粉料中加入占预烧粉料质量百分比的0.5%~3%的降烧剂,以粉体:锆球:去离子水质量比1:3~7:1~3,行星球磨3~6小时,再取出烘干后,以丙烯酸溶液作为粘结剂造粒,压制成型,最后在850℃~900℃大气气氛中烧结2~6小时,制成微波介质陶瓷材料。
综上所述,本发明在Zn0.5Ti0.5NbO4基础上进行离子掺杂Co2O3和Ta2O5,并在离子掺杂后的体系上掺杂0.5~3wt.%降烧剂,低于900℃烧结温度下烧结致密,在保证微波介电性能优异的前提下,且能够调节体系较正的τf值。
附图说明
图1为实施例x=0.3,y=0.4时掺杂1wt.%降烧剂的收缩曲线图;
图2(a)为实施例x=0.3,y=0.4时掺杂1wt.%降烧剂,850℃~900℃下烧结的XRD图谱;图2(b)为实施例x=0.3,y=0.4时掺杂0.5~3wt.%降烧剂,在900℃下烧结后的XRD图谱;
图3为x=0.3,y=0.4掺杂1wt.%降烧剂在850℃~900℃下烧结后的SEM图,其中(a)对应实施例2,(b)对应实施例6,(c)对应实施例10。
具体实施方式
下面结合附图和实施例对本发明做进一步的详细说明。
(Zn1-xCox)0.5Ti0.5(Nb1-yTay)O4,x=0.3,y=0.4。
步骤1、将各组成原料按表中参数配料,按照粉料:锆球:去离子水质量比1:5:2行星球磨6小时,然后100℃烘干,以60目筛网过筛,最后在1000℃大气气氛中预烧3小时。
步骤2、将降烧剂原料按表中参数配料,球磨7小时,烘干过筛后,在800℃下预烧3小时,然后1200℃保温3小时熔融玻璃渣,将玻璃渣破碎球磨成粉制得降烧剂。
步骤3、将制得的降烧剂粉料按照预烧料的质量百分比0.5~3wt.%加入预烧料中,并进行二次球磨,按照粉料:锆球:去离子水质量比1:5:1行星球磨4小时,然后在100℃烘箱中烘干,烘干后用丙烯酸造粒,并压制成型,最后在850℃~900℃大气气氛中烧结4小时,制成微波介质陶瓷材料。
图1展示了该复合陶瓷体系掺杂1wt.%降烧剂的收缩曲线,从曲线中可以看出,未掺杂降烧剂时,样品开始收缩的温度大概位于800℃附近,并且当温度达到1100℃时,收缩率不足6%,而当掺杂1wt.%降烧剂时,体系开始收缩的温度提前200℃,并且在1100℃时体系的收缩率最大可达到23%,明显大于为掺杂降烧剂时的体系收缩率,进一步说明降烧剂的加入使得陶瓷材料在较低温度下实现致密化,能够有效的促进烧结过程。
图2(a)为x=0.3,y=0.4掺杂1wt.%降烧剂后在850℃~900℃下烧结后的XRD图谱;图2(b)为x=0.3,y=0.4掺杂0.5~3wt.%降烧剂后在900℃下烧结后的XRD图谱。
从图2(a)可以看出,在不同烧结温度下,该样品呈现出两种物相,其中主晶相为ZnTiNb2O8(JCPDS#48-0323),次晶相为Zn0.17Nb0.33Ti0.5O2(JCPDS#39-0291)。从图2(b)中看出,掺杂不同量降烧剂后,该样品仍然只有两种物相ZnTiNb2O8(JCPDS#48-0323),Zn0.17Nb0.33Ti0.5O2(JCPDS#39-0291)。
以实施例2、6、10为例,探讨不同烧结温度(850℃-900℃)下样品的晶粒生长情况,从SEM图(图3)可以看出,在三个温度下样品的晶粒尺寸小。在850℃时,晶粒尺寸大小约为0.6μm,并且尺寸分布均匀,在875℃时,出现异常大的晶粒,同时表面可以看到出现气孔,在900℃时,表面观察不到气孔,样品致密,并且异常大晶粒数量增多。
各实施例的成分和微波介电性能如下表格
从上表格数据可以看出,降烧剂的加入,使得该体系在低于900℃烧结温度下烧结致密。并且掺杂1wt.%降烧剂的体系的谐振频率温度系数均在±10ppm/℃范围内,微波介电性能优异(以实施例2,6,10为例),说明本发明降烧剂的加入,低于900℃烧结温度下烧结致密,并能够调节体系较正的τf值。
综上所述,本发明在Zn0.5Ti0.5NbO4基础上进行离子掺杂Co2O3和Ta2O5,并在离子掺杂后的体系上掺杂0.5~3wt.%降烧剂,低于900℃烧结温度下烧结致密,在保证微波介电性能优异的前提下,且能够调节体系较正的τf值。
Claims (2)
1.一种低温烧结复合微波介质陶瓷材料,其特征在于:
由质量百分比97%~99.5%的(Zn1-xCox)0.5Ti0.5(Nb1-yTay)O4基料和质量百分比0.5%~3%的降烧剂组成,x=0.05~0.95,y=0.05~0.95;
基料原料组分是ZnO、Co2O3、TiO2、Nb2O5和Ta2O5按化学通式(Zn1-xCox)0.5Ti0.5(Nb1-yTay)O4配比,x=0.05~0.95,y=0.05~0.95;
降烧剂原料组分的重量百分比为:32.42%≤Li2CO3≤40.04%,42.54%≤H3BO3≤54.26%,2.56%≤SiO2≤6.33%,0%<ZnO≤2.54%,0%<Al2O3≤18.25%,0%<MnCO3≤0.4%和0%<CuO≤1.2%,MnCO3:CuO的重量比为1:3;
其主晶相为ZnTiNb2O8相,次晶相为Zn0.17Nb0.33Ti0.5O2相,烧结温度≤900℃,体系致密,介电常数20~34,损耗≤10-4,频率温度系数-10ppm/℃≤τf≤+10ppm/℃。
2.如权利要求1所述低温烧结复合微波介质陶瓷材料,其制备方法如下:
步骤1、将ZnO、Co2O3、TiO2、Nb2O5和Ta2O5的原始粉料按照(Zn1-xCox)0.5Ti0.5(Nb1-yTay)O4化学通式进行配料,x=0.05~0.95,y=0.05~0.95;
步骤2、将步骤1所得配料装入球磨罐,以锆球及去离子水作为研磨介质,按照配料:锆球:去离子水质量比1:3~7:1~3行星球磨4~7小时,然后在80~100℃烘干,以40~60目筛网过筛,最后在800~1200℃大气气氛中预烧2~4小时合成主晶相ZnTiNb2O8相;
步骤3、按32.42%≤Li2CO3≤40.04%,42.54%≤H3BO3≤54.26%,2.56%≤SiO2≤6.33%,0%<ZnO≤2.54%,0%<Al2O3≤18.25%,0%<MnCO3≤0.4%,0%<CuO≤1.2%,MnCO3:CuO重量比1:3配料,然后装入球磨罐中,球磨4~7小时,待烘干过筛后,再于500℃~800℃下预烧2~6小时,最后在1100℃~1500℃保温1~5小时熔融玻璃渣,将制备的玻璃渣再破碎球磨成粉制得降烧剂;
步骤4、在步骤2制得的预烧粉料中加入占预烧粉料质量百分比的0.5%~3%的降烧剂,以粉体:锆球:去离子水质量比1:3~7:1~3,行星球磨3~6小时,再取出烘干后,以丙烯酸溶液作为粘结剂造粒,压制成型,最后在850℃~900℃大气气氛中烧结2~6小时,制成微波介质陶瓷材料。
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