CN114634352A - 一种硅锗基低介微波介质陶瓷及其制备方法 - Google Patents
一种硅锗基低介微波介质陶瓷及其制备方法 Download PDFInfo
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Abstract
本发明属于低介微波介质陶瓷技术领域,更具体地,涉及一种硅锗基低介微波介质陶瓷及其制备方法。将化学通式为xBaO‑MO2‑3NO2(M=SnyZrzHfk;N=Si1‑lGel;y+z+k=1;0<x≤1.0;0≤y≤1.0;0≤z≤1.0;0≤k≤1.0;0≤l≤1.0)的化合物用于制备微波介质陶瓷材料。该陶瓷具有低介电常数(εr=6.6~9.5)、优异的品质因数(Q×f=7977~36100GHz)和较宽的烧结温度(1200℃~1450℃),同时该微波介质陶瓷具有负的谐振频率温度系数(‑37.8ppm/℃≤τf≤‑22.8ppm/℃)。该微波介质陶瓷的较低的烧结温度、低的介电常数和优异的品质因数可使这种低介微波介质材料作为介质基板、介质谐振器以及介质滤波器等元器件的原材料使用。
Description
技术领域
本发明属于微波介质陶瓷技术领域,更具体地,涉及一种硅锗基低介微波介质陶瓷及其制备方法。
背景技术
微波介质陶瓷是指应用于微波频段(300MHz~3000GHz)电路中作为介质的陶瓷材料。随着通信设备运行频率不断的提高,信号延迟现象会变得更加明显,系统损耗和发热量也会随之增大,系统稳定性会逐渐变差。而低介电常数能减小材料与电极之间的交互耦合损耗,并且能提高电信号的传输速率,优异的品质因数能减小系统损耗且会提高材料的选频特性。而低介微波介质陶瓷主要集中在硅酸盐、锗酸盐、磷酸盐、钒酸盐和钨钼酸盐体系,由于硅酸盐和锗酸盐中含有大量的硅氧四面体和锗氧四面体,该四面体中的Si-O键和Ge-O键表现出强烈的共价特性,因而具有较高四面体含量的硅酸盐和锗酸盐可能具有较低介电常数的同时拥有较高的品质因数。考虑到环境友好和不易潮解等因数,具有大量四面体三节环结构的硅锗基低介电常数微波介质陶瓷将是未来介质基板、介质谐振器以及介质滤波器等元器件的主要候选原材料之一。
在万物互联的大背景下,信号传输的高速率、低时延以及高稳定性成为了急需解决的问题。对于应用于通信系统中的介质谐振器、滤波器等基础无源器件,其尺寸与通信电磁波的半波长成整数倍,通信频率的升高势必会要求器件进行小型化,而目前发达的生产技术已经可以实现超小尺寸元器件的大规模生产,反倒是在降低时延上面临一定困难,而降低时延最有效的方式就是降低器件材料的介电常数,介电常数的平方根与时延成正比。对于即将到来的6G以及毫米波通讯,介电常数小于10的微波介质陶瓷将成为制备介质基板、介质谐振器、机制滤波器等元器件必不可少的原材料,而高性能、高稳定性的低介微波介质陶瓷生产技术几乎被日本、韩国、美国等国家和地区垄断,针对目前日益增长的低介微波介质陶瓷需求,自主研发出一系列介电常数小于10且品质因数较高的低介微波介质陶瓷体系尤为重要。
发明内容
针对现有技术的以上缺陷或改进需求,本发明提供了一种化合物在制备微波介质陶瓷中的应用,拓宽了低介电常数的微波介质陶瓷材料的选择范围。
为实现上述目的,按照本发明的一个方面,提供了一种化合物在制备微波介质陶瓷中的应用,该化合物的化学式为xBaO-MO2-3NO2,其中M=SnyZrzHfk;N=Si1-lGel;y+z+k=1;0<x≤1.0;0≤y≤1.0;0≤z≤1.0;0≤k≤1.0;0≤l≤1.0。
优选地,采用所述化合物制备得到的微波介质陶瓷的介电常数6.6至9.5之间,品质因数Q×f为7977~36100GHz,谐振频率温度系数τf的范围为:-37.8ppm/℃≤τf≤-22.8ppm/℃。
优选地,按照如下方法制备得到所述微波介质陶瓷:
步骤(1):按照化学表达式为xBaO-MO2-3NO2(M=SnyZrzHfk;N=Si1-lGel;y+z+k=1;0<x≤1.0;0≤y≤1.0;0≤z≤1.0;0≤k≤1.0;0≤l≤1.0)的化学计量比称取BaCO3、SnO2、ZrO2、HfO2、SiO2和GeO2,称量后湿法球磨处理,球磨后烘干,然后进行预烧,得到预烧陶瓷粉体;
步骤(2):将步骤(1)得到的预烧陶瓷粉体,进行二次湿法球磨处理,烘干后加入粘合剂造粒,压片后进行烧结,获得所述微波介质陶瓷。
优选地,步骤(1)所述湿法球磨处理,湿法球磨分散剂为200wt%的去离子水,球磨介质为锆球,球磨工艺为以360r/min的速度球磨5~10小时。
优选地,步骤(1)所述预烧的温度为900℃~1050℃,预烧时间为5~10小时。
优选地,步骤(2)所述粘结剂为PVA或石蜡,粘合剂加入的质量分数为5%~10%。
优选地,步骤(2)所述烧结的温度为1200℃~1450℃,烧结时间为5~10小时。
总体而言,通过本发明所构思的以上技术方案与现有技术相比,能够取得下列有益效果:
(1)本发明将化学通式为xBaO-MO2-3NO2(M=SnyZrzHfk;N=Si1-lGel;y+z+k=1;0<x≤1.0;0≤y≤1.0;0≤z≤1.0;0≤k≤1.0;0≤l≤1.0)的化合物用于制备微波介质陶瓷材料,该新型微波介质陶瓷具有低于10的介电常数和优异的品质因数,且相成分为单相、多次实验微波介电性能稳定的优点。
(2)本发明提供了一种不含易变价元素、主晶相不易潮解且烧结温度较低的介质元器件用微波介质陶瓷。
附图说明
图1为本发明硅锗基低介微波介质陶瓷的制备流程图;
图2和图3为本发明硅锗基低介微波介质陶瓷的XRD图谱;
图4和图5为本发明硅锗基低介微波介质陶瓷的SEM和EDS图;
图6为本发明硅锗基低介微波介质陶瓷的晶体结构示意图;
图7为本发明硅锗基低介微波介质陶瓷的远红外光谱图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明,并不用于限定本发明。此外,下面所描述的本发明各个实施方式中所涉及到的技术特征只要彼此之间未构成冲突就可以相互组合。
本发明提供了一种化合物在制备微波介质陶瓷中的应用,该化合物的化学式为xBaO-MO2-3NO2,其中M=SnyZrzHfk;N=Si1-lGel;y+z+k=1;0<x≤1.0;0≤y≤1.0;0≤z≤1.0;0≤k≤1.0;0≤l≤1.0。
将该化合物用于制备微波介质陶瓷时,所述微波介质陶瓷具有低介电常数和优异的品质因数(Q×f=7977~36100GHz),其介电常数小于10且大小可调,可调控的范围在6.6至9.5之间,所述的微波介质陶瓷具有低介电常数的同时还具有负的谐振频率温度系数(-37.8ppm/℃≤τf≤-22.8ppm/℃)。
按照如下方法制备得到所述微波介质陶瓷:
步骤(1):按照化学表达式为xBaO-MO2-3NO2(M=SnyZrzHfk;N=Si1-lGel;y+z+k=1;0<x≤1.0;0≤y≤1.0;0≤z≤1.0;0≤k≤1.0;0≤l≤1.0)的化学计量比称取BaCO3、SnO2、ZrO2、HfO2、SiO2和GeO2,称量后湿法球磨处理,球磨后烘干,然后进行预烧,得到预烧陶瓷粉体;
步骤(2):将步骤(1)得到的预烧陶瓷粉体,进行二次湿法球磨处理,烘干后加入粘合剂造粒,压片后进行烧结,获得所述微波介质陶瓷。
作为一种具体实施方式,步骤(1)所述湿法球磨处理,湿法球磨分散剂为200wt%的去离子水,球磨介质为锆球,球磨工艺为以360r/min的速度球磨5~10小时。
作为一种具体实施方式,步骤(1)所述预烧的温度为900℃~1050℃,预烧时间为5~10小时,预烧的目的是得到陶瓷粉体的预烧相。
作为一种具体实施方式,步骤(2)所述粘结剂为PVA或石蜡,粘合剂加入的质量分数为5%~10%。
作为一种具体实施方式,步骤(2)所述烧结的温度为1200℃~1450℃,烧结时间为5~10小时。
本发明所制备的新型微波介质陶瓷具有低介电常数的同时还具有优异的综合微波介电性能。其中低介电常数的特性有利于提高电信号在介质材料中传输的速率,优异的综合微波介电性能减少了系统工作的损耗并改善了稳定性,且该新型微波介质陶瓷不含易变价元素、主晶相不易潮解、烧结温度较低,可作为微波电路中介质元器件的原材料来使用。
以下为实施例:
实施例1~14
一种微波介质陶瓷,其制备方法按照如下步骤进行:
(1)将纯度为99.9%的BaCO3、SnO2、ZrO2、HfO2、SiO2和GeO2分别按照化学计量比配比混合后,以锆球为球磨介质、去离子水为分散剂,利用球磨机将粉末混合搅拌5小时,转速为360r/min;将获得的浆料烘干后在1000℃下预烧5小时,得到预烧陶瓷粉体;
(2)将步骤(1)得到的预烧陶瓷粉体再次进行湿法球磨处理,分散剂采用去离子水,烘干后在干燥的粉末中加入8wt%的聚乙烯醇(PVA)粘接剂造粒,在150MPa压力下将其压制成厚度与直径比为0.4~0.6的圆柱形生坯试样;压片后在1200℃~1450℃的空气中烧结5小时,获得如表1所述的微波介质陶瓷。
表1实施例1~14、烧结温度、相对密度及微波介电性能
从实施例1~14可以看出,该新型的硅锗基微波介质陶瓷材料具有低介电常数和优异的品质因数,其介电常数在6.6至9.5之间,品质因数在Q×f在7977~36100GHz之间,且相成分为单相、不含易变价元素、不易潮解、烧结温度较低,是一种能用来制备介质元器件的候选材料。
本领域的技术人员容易理解,以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (6)
1.一种硅锗基低介微波介质陶瓷,其特征在于:包括陶瓷本体,所述陶瓷本体由化合物制备而成,该化合物的化学式为xBaO-MO2-3NO2,其中M=SnyZrzHfk;N=Si1-lGel;y+z+k=1;0<x≤1.0;0≤y≤1.0;0≤z≤1.0;0≤k≤1.0;0≤l≤1.0。
2.根据权利要求1所述的一种硅锗基低介微波介质陶瓷,其特征在于:该陶瓷主晶相的晶体结构中具有硅锗四面体三节环层和氧八面体层,采用所述化合物制备得到的微波介质陶瓷的介电常数在6.6至9.5之间,品质因数Q×f为7977~36100GHz,谐振频率温度系数τf的范围为:-37.8ppm/℃≤τf≤-22.8ppm/℃。
3.一种根据权利要求1所述的硅锗基低介微波介质陶瓷的制备方法,其特征在于,按照如下方法制备得到所述微波介质陶瓷:
步骤(1):按照化学表达式为xBaO-MO2-3NO2(M=SnyZrzHfk;N=Si1-lGel;y+z+k=1;0<x≤1.0;0≤y≤1.0;0≤z≤1.0;0≤k≤1.0;0≤l≤1.0)的化学计量比称取BaCO3、SnO2、ZrO2、HfO2、SiO2和GeO2,称量后湿法球磨处理,球磨后烘干,然后进行预烧,得到预烧陶瓷粉体;
步骤(2):将步骤(1)得到的预烧陶瓷粉体,进行二次湿法球磨处理,烘干后加入粘合剂造粒,压片后进行烧结,获得所述微波介质陶瓷。
4.根据权利要求3所述一种硅锗基低介微波介质陶瓷的制备方法,其特征在于:步骤(1)、(2)所述的湿法球磨处理,球磨分散剂为200wt%的去离子水,球磨介质为锆球,球磨工艺为以360r/min的速度球磨5~10小时。
5.根据权利要求3所述一种硅锗低介微波介质陶瓷的制备方法,其特征在于:步骤(1)所述预烧的温度为900℃~1050℃,预烧时间为5~10小时;步骤(2)所述烧结的温度为1200℃~1450℃,烧结时间为5~10小时。
6.根据权利要求3所述一种硅锗低介微波介质陶瓷的制备方法,其特征在于:步骤(2)所述粘合剂含量为5~10wt%。
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