CN113896530A - 一种温度稳定的改性NiO-Ta2O5基微波介质陶瓷材料及其制备方法 - Google Patents
一种温度稳定的改性NiO-Ta2O5基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,涉及一种温度稳定的改性NiO‑Ta2O5基微波介质陶瓷材料及其制备方法。利用离子掺杂改性形成固溶体结构是调节微波介电性能,尤其是调节温度稳定性的重要措施。本发明基于固溶体的形成规则,考虑在NiTa2O6陶瓷中引入Ni2+与Ta5+离子在相同配位环境下(配位数CN=6)具有相近离子半径的阳离子掺杂,包括了设计Ni2+离子被Cu2+离子取代,(Ni1/3Ta2/3)4+复合离子被复合离子[(Al1/ 2Nb1/2)ySn1‑y]4+取代的方式,从而获得NiTa2O6固溶体结构的陶瓷材料,并通过调节各掺杂离子的摩尔含量,最终制备出了一种具有优异温度稳定性且低损耗的微波介质陶瓷材料,微波介电性能优越。
Description
技术领域
本发明属于电子陶瓷及其制造领域,涉及一种温度稳定的改性NiO-Ta2O5基微波介质陶瓷材料及其制备方法。
背景技术
5G移动通讯技术的快速发展对高频通讯的电子元器件,如谐振器、滤波器、介质天线等的介电性能提出了严苛的要求。微波介质陶瓷是指应用于微波频段(300MHz~300GHz)电路中作为介质材料并发挥一定功能性的陶瓷材料,由于其尺寸可控、微波介电性能优异,应用广泛,近年来得到了愈来愈多的关注。
在现有微波介质陶瓷材料中,NiTa2O6陶瓷是一种具有四方结构的体系。经研究学者报道,该体系在1400~1600℃烧结温度下的微波介电性能为:εr=25~27,Q×f=31200GHz,τf=26~35ppm/℃,可以发现该材料的谐振频率温度系数较大,实际应用价值较低。一般τf值介于±10ppm/℃视为温度稳定性佳,且该数值越趋向于0ppm/℃则说明温度稳定性越好。
尽管现今已经出现部分关于ATa2O6陶瓷的报道,然而大部分体系如ATa2O6(A=Co、Ni)的τf值过大(如A=Co体系的τf值~25ppm/℃);亦有利用TiO2与ATa2O6(A=Ni/Co/Zn)复合的探索,同样表现出了较大的τf值(如NiTiTa2O8的τf值为75ppm/℃)。寻找一种具有低损耗且温度稳定的改性NiTa2O6陶瓷体系成为该研究领域亟需攻克的难点。
发明内容
针对上述存在的问题或不足,为解决现有NiTa2O6陶瓷存在的温度稳定性欠佳的问题,本发明提供了一种改性NiO-Ta2O5基微波介质陶瓷材料的制备方法,在保持低介质损耗的同时,提升了该类微波介质陶瓷材料的温度稳定性,使其能够广泛应用于电子通信领域。
本发明提供的一种温度稳定的改性NiO-Ta2O5基微波介质陶瓷材料,其化学通式为[(Ni1-xCux)1/3Ta2/3]1-z[(Al1/2Nb1/2)ySn1-y]zO2,其中0.02≤x≤0.08,0.05≤y≤0.2,0.02≤z≤0.06,经由固相法制备获得;且在0.02≤x≤0.08,0.05≤y≤0.2,0.02≤z≤0.06范围内材料具有单一的NiTa2O6固溶体相组成,晶体结构为NiTa2O6固溶体;
该微波介质陶瓷材料的烧结温度为1325~1400℃,介电常数εr介于19~23,品质因数Q×f值介于30000~52000GHz,谐振频率温度系数τf介于-5~+5ppm/℃。
作为优选,当x=0.05,y=0.15且z=0.02时,在1375℃烧结温度下材料的介电常数为20.91,介质损耗为2.14×10-4,品质因数Q×f值为50028GHz,谐振频率温度系数为-1.7ppm/℃。
本发明提供的一种温度稳定的改性NiO-Ta2O5基微波介质陶瓷材料的制备方法,其包括以下步骤:
步骤1:将NiO、CuO、Al2O3、Nb2O5、SnO2和Ta2O5的原始粉料按照化学通式[(Ni1- xCux)1/3Ta2/3]1-z[(Al1/2Nb1/2)ySn1-y]zO2进行配料,其中0.02≤x≤0.08,0.05≤y≤0.2,0.02≤z≤0.06;
步骤2:将步骤1配好的粉体装入球磨罐,研磨介质为锆球和去离子水,按照粉料:锆球:去离子水质量比为1:6~8:4~6进行球磨,行星球磨6~8小时,取出后在80~120℃烘箱中烘干,以40~60目筛网过筛,后在1000~1100℃大气气氛中预烧3~5小时;
步骤3:将步骤2预烧后的粉体,再次按照粉体:锆球:去离子水质量比为1:5~7:1~3进行球磨,行星球磨混合3~6小时,取出烘干后得到二次球磨烘干料;并在得到的二次球磨烘干料中加入聚乙烯醇溶液进行造粒;
步骤4:将步骤3制得陶瓷生料压制成型,在600~650℃排胶后在1325℃~1400℃大气气氛中烧结4~6小时后,即可制得[(Ni1-xCux)1/3Ta2/3]1-z[(Al1/2Nb1/2)ySn1-y]zO2微波介质陶瓷材料。
结合行业现有技术的报道,利用离子掺杂改性形成固溶体结构是调节微波介电性能,尤其是调节温度稳定性的重要措施。本发明基于固溶体的形成规则,考虑在NiTa2O6陶瓷中引入Ni2+与Ta5+离子在相同配位环境下(配位数CN=6)具有相近离子半径的阳离子掺杂,包括了设计Ni2+离子被Cu2+离子取代,(Ni1/3Ta2/3)4+复合离子被复合离子[(Al1/2Nb1/2)ySn1-y]4+取代的方式,从而获得NiTa2O6固溶体结构的陶瓷材料,并通过调节各掺杂离子的摩尔含量,最终制备出了一种具有优异温度稳定性且低损耗的微波介质陶瓷材料,微波介电性能优越。
附图说明
图1对应实施例样7、8、与9的XRD衍射图谱;
图2对应实施例样7的SEM形貌图。
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。
步骤1、将NiO、CuO、Al2O3、Nb2O5、SnO2和Ta2O5的原始粉料按照化学通式[(Ni1- xCux)1/3Ta2/3]1-z[(Al1/2Nb1/2)ySn1-y]zO2(x=0.05;y=0.15;z=0.02,0.04,0.06),采用摩尔比进行配料;
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1:6:4行星球磨6小时,然后在100℃烘干,以60目筛网过筛,最后在1100℃大气气氛中预烧3小时。
步骤3、将预烧后的粉料、放入球磨罐中进行二次球磨,以粉体:锆球:去离子水质量比1:6:3,行星球磨4小时,再取出烘干后得到二次球磨烘干料;然后向二次球磨烘干料中加入质量分数为5%的聚乙烯醇溶液进行造粒。
步骤4、将步骤3造粒好的粉体放入φ12的模具中,在20MPa压力下干压成型(尺寸为12mm×6mm的圆柱块体),然后将圆柱块体在650℃下保温2小时以除去粘结剂,然后升至1325℃~1400℃下保温4小时,最终制得[(Ni1-xCux)1/3Ta2/3]1-z[(Al1/2Nb1/2)ySn1-y]zO2微波介质陶瓷材料。
按照上述步骤制作了12份实施例样。图1为实施例样7、8、与9的XRD衍射图谱。在三个不同实施例下陶瓷试样的物相组成经过检索,与NiTa2O6的标准卡片JCPDS card No.32-0702对应,各掺杂离子均固溶至阳离子格位且并未发现第二相衍射峰的存在,则说明[(Ni1-xCux)1/3Ta2/3]1-z[(Al1/2Nb1/2)ySn1-y]zO2陶瓷属于NiTa2O6结构的固溶体。
图2为实施例7的SEM形貌图,可以看出陶瓷试样的晶粒生长充分,晶界清晰可见,说明并未出现过烧现象,但此时仍存在部分微气孔。
各实施例样品的具体成分及微波介电性能如下:
表1为各实施例样品成分
表2为各实施例样品微波介电性能
结合表1、表2提供的数据可以看出在x=0.05,y=0.15且z=0.02,0.04,0.06范围内,烧结温度介于1325~1400℃间陶瓷试样的谐振频率温度系数τf值全部介于±5ppm/℃,均十分优异。尤其是在z=0.02且烧结温度为1375℃时,即(实施例7)[(Ni1-xCux)1/3Ta2/3]1-z[(Al1/2Nb1/2)ySn1-y]zO2陶瓷的微波介电性能最佳:εr=20.91,tanδ=2.14×10-4,Q×f=50028GHz,τf=-1.7ppm/℃,可以广泛应用于高频通讯的电子元器件中。
Claims (3)
1.一种温度稳定的改性NiO-Ta2O5基微波介质陶瓷材料,其特征在于,该温度稳定的改性NiO-Ta2O5基微波介质陶瓷材料的化学通式为[(Ni1-xCux)1/3Ta2/3]1-z[(Al1/2Nb1/2)ySn1-y]zO2,其中0.02≤x≤0.08,0.05≤y≤0.2,0.02≤z≤0.06,经由固相法制备获得;且在0.02≤x≤0.08,0.05≤y≤0.2,0.02≤z≤0.06范围内材料具有单一的NiTa2O6固溶体相组成,晶体结构为NiTa2O6固溶体;
该微波介质陶瓷材料的烧结温度为1325~1400℃,介电常数εr介于19~23,品质因数Q×f值介于30000~52000GHz,谐振频率温度系数τf介于-5~+5ppm/℃。
2.根据权利要求1所述的一种温度稳定的改性NiO-Ta2O5基微波介质陶瓷材料,其特征在于:当x=0.05,y=0.15且z=0.02时,在1375℃烧结温度下材料的介电常数为20.91,介质损耗为2.14×10-4,品质因数Q×f值为50028GHz,谐振频率温度系数为-1.7ppm/℃。
3.一种温度稳定的改性NiO-Ta2O5基微波介质陶瓷材料的制备方法,其特征在于:包括以下步骤:
步骤1:将NiO、CuO、Al2O3、Nb2O5、SnO2和Ta2O5的原始粉料按照化学通式[(Ni1-xCux)1/ 3Ta2/3]1-z[(Al1/2Nb1/2)ySn1-y]zO2进行配料,其中0.02≤x≤0.08,0.05≤y≤0.2,0.02≤z≤0.06;
步骤2:将步骤1配好的粉体装入球磨罐,研磨介质为锆球和去离子水,按照粉料:锆球:去离子水质量比为1:6~8:4~6进行球磨,行星球磨6~8小时,取出后在80~120℃烘箱中烘干,以40~60目筛网过筛,后在1000~1100℃大气气氛中预烧3~5小时;
步骤3:将步骤2预烧后的粉体,再次按照粉体:锆球:去离子水质量比为1:5~7:1~3进行球磨,行星球磨混合3~6小时,取出烘干后得到二次球磨烘干料;并在得到的二次球磨烘干料中加入聚乙烯醇溶液进行造粒;
步骤4:将步骤3制得陶瓷生料压制成型,在600~650℃排胶后在1325℃~1400℃大气气氛中烧结4~6小时后,即可制得[(Ni1-xCux)1/3Ta2/3]1-z[(Al1/2Nb1/2)ySn1-y]zO2微波介质陶瓷材料。
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