CN113754419A - 一种硅基可低温烧结的低介高品质因数微波介质陶瓷的制备及应用 - Google Patents
一种硅基可低温烧结的低介高品质因数微波介质陶瓷的制备及应用 Download PDFInfo
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Abstract
本发明公开了一种硅基可低温烧结的低介高品质因数微波介质陶瓷的制备及应用。（1）将Li2CO3、SrCO3和SiO2按Li2SrSiO4的组成称量配料；（2）球磨混合6小时，球磨介质为酒精，烘干后预烧；（3）将预烧后粉末与SiTiO3粉末按(1‑x)Li2SrSiO4‑xSrTiO3进行称量，其中x为体积百分比（0≤x≤0.06），再次球磨后添加聚乙烯醇溶液并造粒，再压制成型，最后在大气气氛中烧结。本发明制备的硅基低介高品质因数微波介质陶瓷，介电常数为7.4~8.2，品质因数高达63,200~100,700GHz，谐振频率温度系数近零，能应用于各种陶瓷基板、介质谐振器与滤波器等微波元器件的制造。
Description
技术领域
本发明涉及介电陶瓷材料，特别是涉及在微波频率使用的陶瓷基板、谐振器、滤波器等微波元器件，以及陶瓷电容器或温度补偿电容器的介电陶瓷材料的制备及应用。
背景技术
微波介质陶瓷是指应用于微波频段(300Mz～300Hz)电路中作为介质并完成微波波导、屏蔽和谐振等一种或多种功能的材料，已成为现代移动通讯技术的关键基础材料。衡量微波介质材料性能的三个重要指标是介电常数εr、品质因数Q×f和谐振频率温度系数τf。其中，介电常数与器件的尺寸成反比，决定了元器件的尺寸；高品质因数有利于提高信号强度和谐振频率分辨率；尽可能近零(±10ppm/℃)的谐振频率温度系数以保证器件良好的热稳定性。
近来基于5G的无线通信系统、物联网、智能运输系统和智能驾驶等应用市场的迅猛发展，微波介质元器件趋向高频、小型、轻量、薄型与高性能的发展。当通讯频率上升到毫米波频段(>30GHz)，低εr不仅能降低材料与电极之间的交互耦合损耗，而且可以减少信号传输过程中的延迟以满足高频高速的要求，高品质因数(Q×f>90000GHz)有利于提高元件的选频特性并减少工作过程中的发热量，因此超低介电常数(εr<10)和高品质因数(Q×f>90,000GHz)微波介质陶瓷的研究与开发越来越受到重视。
现有低εr与高Q×f值的材料体系主要是Al2O3系、尖晶石MgAl2O4和ZnAl2O4系、MgTiO3系、硅酸盐M2SiO4(M＝Mg、Zn)、Li2TiO3系、K2NiF4型SrRAlO4(R＝Sm、Nd、La)等[1-4]，其中硅酸盐陶瓷如Mg2SiO4、Zn2SiO4等因具有低εr与高Q×f，以及密度低、价格便宜等优点而受到关注。
以上这些材料体系的烧结温度一般高于1300℃，不能直接与Ag和Cu等低熔点金属共烧形成多层陶瓷电容器。近年来，随着低温共烧陶瓷技术(Low Temperature Co-firedCeramics，LTCC)的发展和微波多层器件发展的要求，国内外的研究人员对一些低烧体系材料进行了广泛的探索和研究，主要是采用微晶玻璃或玻璃-陶瓷复合材料体系，因低熔点玻璃相具有相对较高的介质损耗，玻璃相的存在大大提高了材料的介质损耗。因此研制无玻璃相的本征低烧结温度的微波介质陶瓷材料是当前研究的重点。
在探索与开发新型可低烧微波介电陶瓷材料的过程中，固有烧结温度低的Li基化合物、Bi基化合物、钒酸盐、钼酸盐、钨酸盐体系化合物和碲酸盐体系化合物等材料体系得到了广泛关注与研究。但是由于微波介电陶瓷的三个性能指标之间是相互制约的关系，满足三个性能要求且可低温烧结的单相微波介质陶瓷非常少。目前对微波介质陶瓷的研究大部分是通过大量实验而得出的经验总结，却没有完整的理论来阐述微观结构与介电性能的关系，这在很大程度上限制了低温共烧技术及微波多层器件的发展。探索与开发既能低温烧结同时具有超低介电常数与较高品质因数的微波介电陶瓷是本领域技术人员一直渴望解决但始终难以获得成功的难题。
我们通过研究及总结发现，向正硅酸盐和正锗酸盐中引入一定比例的Li，能有效降低其烧结温度，如Li2ZnSiO4、Li2MgSiO4、Li2CaSiO4和Li2ZnGeO4、Li2MgGeO4，比其对应的正硅酸盐和正锗酸盐烧结温度降低了200～450℃，但是仍高于银电极的熔点(961℃)。只有用2mol的Li离子取代Sr2SiO4中1mol的Sr离子制备Li2SrSiO4陶瓷，其烧结温度才降低至880℃，且具有超低介电常数和高品质因数。通过复杂化学键理论分析发现，其Si-O键中较弱的共价性(18％)是其烧结温度低的关键。并通过向Li2SrSiO4中添加0.06体积比的SrTiO3，将Li2SrSiO4陶瓷较大的τf调节至近零。
发明内容
本发明的目的是提供一种硅基可低温烧结的低介高品质因数微波介质陶瓷的制备及应用。
本发明涉及的硅基低介高品质因数微波介质陶瓷的化学组成为：(1-x)Li2SrSiO4-xSrTiO3，其中：x为体积百分比(0≤x≤0.06)。
所述硅基低介高品质因数微波介质陶瓷的制备方法步骤为：
(1)将99.9％分析纯的原料粉末Li2CO3、SrCO3和SiO2按Li2SrSiO4的组成称量配料；
(2)将步骤(1)原料湿式球磨混合6小时，球磨介质为酒精，烘干后在600～720℃大气气氛中预烧3～5小时；
(3)将步骤(2)获得的预烧粉末与99.9％分析纯的SiTiO3粉末按(1-x)Li2SrSiO4-xSrTiO3进行称量，其中x为体积百分比(0≤x≤0.06)，再次球磨后添加质量百分比浓度为5％的聚乙烯醇溶液并造粒，聚乙烯醇溶液剂量占粉末总质量的2～4％；再压制成型，最后在800～900℃大气气氛中烧结2～6小时，得硅基低介高品质因数微波介质陶瓷(1-x)Li2SrSiO4-xSrTiO3。
本发明制备的硅基低介高品质因数微波介质陶瓷(1-x)Li2SrSiO4-xSrTiO3的致密化温度较低为880℃，其介电常数较低为7.4～8.2，品质因数高达63,200～100,700GHz，谐振频率温度系数近零，可广泛用于各种陶瓷基板、谐振器和滤波器等微波元器件的制造，满足低温共烧技术及微波多层器件的技术需要，且合成原料低廉，在工业上有着极大的应用价值。
具体实施方式
实施例1：
(1)将99.9％分析纯的原料粉末Li2CO3、SrCO3和SiO2按Li2SrSiO4的组成称量配料；
(2)将步骤(1)原料湿式球磨混合6小时，球磨介质为酒精，烘干后在700℃大气气氛中预烧4小时；
(3)将步骤(2)获得的预烧粉末再次球磨后添加质量百分比浓度为5％的聚乙烯醇溶液并造粒，聚乙烯醇溶液剂量占粉末总质量的2％；再压制成型，最后在880℃大气气氛中烧结4小时，得硅基低介高品质因数微波介质陶瓷Li2SrSiO4。
实施例2：
(1)将99.9％分析纯的原料粉末Li2CO3、SrCO3和SiO2按Li2SrSiO4的组成称量配料；
(2)将步骤(1)原料湿式球磨混合6小时，球磨介质为酒精，烘干后在700℃大气气氛中预烧4小时；
(3)将步骤(2)获得的预烧粉末与99.9％分析纯的SiTiO3粉末按0.96Li2SrSiO4-0.04SrTiO3进行称量，再次球磨后添加质量百分比浓度为5％的聚乙烯醇溶液并造粒，聚乙烯醇溶液剂量占粉末总质量的3％；再压制成型，最后在880℃大气气氛中烧结4小时，得硅基低介高品质因数微波介质陶瓷0.96Li2SrSiO4-0.04SrTiO3。
实施例3：
(1)将99.9％分析纯的原料粉末Li2CO3、SrCO3和SiO2按Li2SrSiO4的组成称量配料；
(2)将步骤(1)原料湿式球磨混合6小时，球磨介质为酒精，烘干后在700℃大气气氛中预烧4小时；
(3)将步骤(2)获得的预烧粉末与99.9％分析纯的SiTiO3粉末按0.94Li2SrSiO4-0.06SrTiO3进行称量，再次球磨后添加质量百分比浓度为5％的聚乙烯醇溶液并造粒，聚乙烯醇溶液剂量占粉末总质量的4％；再压制成型，最后在880℃大气气氛中烧结4小时，得硅基低介高品质因数微波介质陶瓷0.94Li2SrSiO4-0.06SrTiO3。
本陶瓷可广泛用于各种陶瓷基板、介质谐振起器、滤波器等微波元器件的制造，可满足移动通信、卫星通信等系统的技术需要。
表1示出各实施例的成分含量及其微波介电性能，用圆柱介质谐振器法进行微波介电性能的评价。
表1：各实施例的成分含量及其微波介电性能
Claims (2)
1.一种硅基可低温烧结的低介高品质因数微波介质陶瓷的制备及应用，其特征在于所述硅基低介高品质因数微波介质陶瓷的组成通式为：(1-x)Li2SrSiO4-xSrTiO3，其中x为体积百分比，0≤x≤0.06；
所述硅基低介高品质因数微波介质陶瓷的制备方法步骤为：
（1）将99.9%分析纯的原料粉末Li2CO3、SrCO3和SiO2按Li2SrSiO4的组成称量配料；
（2）将步骤（1）原料湿式球磨混合6小时，球磨介质为酒精，烘干后在600~720℃大气气氛中预烧3~5小时；
（3）将步骤（2）获得的预烧粉末与99.9%分析纯的SiTiO3粉末按(1-x)Li2SrSiO4-xSrTiO3进行称量，其中x为体积百分比，0≤x≤0.06，再次球磨后添加质量百分比浓度为5%的聚乙烯醇溶液并造粒，聚乙烯醇溶液剂量占粉末总质量的2~4%；再压制成型，最后在800~900℃大气气氛中烧结2~6小时，得硅基低介高品质因数微波介质陶瓷(1-x)Li2SrSiO4-xSrTiO3。
2.根据权利要求1所述的硅基可低温烧结的低介高品质因数微波介质陶瓷的应用，其特征在于所述硅基低介高品质因数微波介质陶瓷能应用于各种陶瓷基板、介质谐振器与滤波器微波元器件的制造。
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