CN115925415B - 一种离子改性的微波介质陶瓷、其制备方法及微波元器件 - Google Patents

一种离子改性的微波介质陶瓷、其制备方法及微波元器件 Download PDF

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CN115925415B
CN115925415B CN202211317183.0A CN202211317183A CN115925415B CN 115925415 B CN115925415 B CN 115925415B CN 202211317183 A CN202211317183 A CN 202211317183A CN 115925415 B CN115925415 B CN 115925415B
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microwave dielectric
dielectric ceramic
ceramic
ball milling
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CN115925415A (zh
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邢孟江
杨鸿宇
刘永红
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Yunnan Infine Neo Material Co ltd
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Abstract

本发明涉及电子陶瓷及其制造技术领域的一种离子改性的微波介质陶瓷，所述微波介质陶瓷的化学通式为Zn0.15Nb0.3[Ti1‑x (W1/3Zr1/2) x ]0.55O2，其中x=0.01~0.03；所述微波介质陶瓷由包括以下重量份数的组分制成：12.58~12.67份ZnO，41.11‑41.39份TiO2，43.93~45.14份Nb2O5，0.44~1.31份WO3，以及0.35~1.05份ZrO2，本发明的产品即制备方法可应用于不同需求的电子元器件、通信设备、微波元器件中，拓展了Zn0.15Nb0.3Ti0.55O2系陶瓷在电子陶瓷制造领域的实用价值。

Description

一种离子改性的微波介质陶瓷、其制备方法及微波元器件
技术领域
本发明涉及电子陶瓷及其制造技术领域，尤其涉及一种离子改性的微波介质陶瓷、其制备方法及微波元器件。
背景技术
在移动通信时代数据流量***式增长的背景下，第五代移动通信技术（5G）的工作频率朝向毫米波波段发展，进而使通信***拥有更高的数据速率和更大的带宽，此外高频下可以使用的频谱资源也更丰富。微波介质陶瓷由于具有小型化、易于集成化、高稳定性、***损耗低和低功耗化等优点，被广泛应用于5G***的多种电子元器件中，如介质谐振器、滤波器、基片、天线、双工器和波导等，具有广阔的市场应用前景。
微波介质陶瓷的性能主要包括：（1）适当的介电常数εr值；（2）高的品质因数Q值（一般用Q×f代表在一定谐振频率下的品质因数值）；（3）可协调的谐振频率温度系数τf值。
金红石型Zn0.15Nb0.3Ti0.55O2陶瓷体系在1075oC烧结温度下表现出十分优异的微波介电性能：εr~93.1，Q×f~11815GHz，τf~346.0ppm/oC，但与此同时注意到其τf值较大，因此如何在保证高Q×f值的同时降低其τf值是一个十分重要的研究方向。
通常情况下，调节陶瓷材料的微波介电性能主要基于两相复合原理以及混合对数规则，通过在陶瓷基料中引入一种具有相反τf值的材料体系改善陶瓷的综合微波介电表现；但局限性较高，不仅需要保证引入的改性剂具有相当的εr值或者较高的Q×f值，同时引入剂亦不能与主晶相发生化学反应，否则无法实现准确调节微波介电性能的目的。因此，针对金红石型Zn0.15Nb0.3Ti0.55O2陶瓷，需要寻找一种能更有效地调节其微波介电性能的方法，以满足陶瓷材料在射频通信行业的应用需求。
发明内容
本发明的特征和优点在下文的描述中部分地陈述，或者可从该描述显而易见，或者可通过实践本发明而学习。
为克服现有技术的问题，本发明提供一种离子改性的微波介质陶瓷，所述微波介质陶瓷的化学通式为Zn0.15Nb0.3[Ti1-x (W1/3Zr1/2) x ]0.55O2，其中x=0.01~0.03；所述微波介质陶瓷由包括以下重量份数的组分制成：12.58~12.67份ZnO，41.11-41.39份TiO2，43.93~45.14份Nb2O5，0.44~1.31份WO3，以及0.35~1.05份ZrO2。
优选的，所述微波介质陶瓷的烧结温度为1050~1150oC。
优选的，所述微波介质陶瓷由包括以下重量份数的组分制成：12.67份ZnO，41.39份TiO2，45.14份Nb2O5，0.441份WO3，0.352份ZrO2。
优选的，在1100oC烧结温度下，微波介质陶瓷的介电常数为90.8，Q×f值高达14381GHz，τf低至243.8ppm/oC。
本发明还提供了一种离子改性的微波介质陶瓷的制备方法，用于制备如上所述的离子改性的金红石Zn0.15Nb0.3Ti0.55O2系微波介质陶瓷，所述制备方法包括以下步骤：
配料：将ZnO、TiO2、Nb2O5、WO3、ZrO2的粉料按照化学通式Zn0.15Nb0.3[Ti1-x (W1/ 3Zr1/2) x ]0.55O2进行配料，得到原料粉；
第一次球磨：将配好的原料粉装入球磨罐，选择锆球和去离子水做为研磨介质，并按照原料粉：锆球：去离子水的质量比为1:4~6:2~4的配比进行4~6小时的第一次行星球磨，待球磨结束后，将混合浆料置于烘箱中烘干，随后以80~100目的筛网过筛，将过筛后的粉体于900~1000℃的大气气氛中预烧3~5小时，得到预烧料；
第二次球磨：按照预烧料粉：锆球：去离子水的质量比为1:5~7:3~5的配比，进行第二次行星球磨6~8小时，待球磨后的物料烘干后，添加聚乙烯醇溶液作为粘结剂，造粒，得到陶瓷生料；
压制成型：将制得的陶瓷生料压制成型，随后以2~4oC/min的升温速率在600~650℃温度下排胶2~4小时，紧接着再以2~4oC/min的升温速率升温至1050~1150oC，再保温4~6小时，即制得离子改性的金红石Zn0.15Nb0.3[Ti1-x (W1/3Zr1/2) x ]0.55O2系微波介质陶瓷。
优选的，本发明还提供了一种微波元器件，其采用如上所述的离子改性的金红石Zn0.15Nb0.3Ti0.55O2系微波介质陶瓷制成。
本发明的有益效果：本发明不仅保持了微波介质陶瓷的较高的Q×f值特性，同时在一定程度上降低了τf值，提高了谐振频率的温度稳定性，可制备出具有高Q×f值、成本低廉且具有良好工艺稳定性的微波介质陶瓷材料。本发明的产品的制备方法可应用于不同需求的电子元器件、通信设备、微波元器件中，拓展了Zn0.15Nb0.3Ti0.55O2系陶瓷在电子陶瓷制造领域的实用价值。
附图说明
下面通过参考附图并结合实例具体地描述本发明，本发明的优点和实现方式将会更加明显，其中附图所示内容仅用于对本发明的解释说明，而不构成对本发明的任何意义上的限制，在附图中：
图1 为本发明具体实施例中实施例1的XRD图谱；
图2 为本发明具体实施例中实施例1的SEM图谱。
具体实施方式
下面结合附图和实施例对本发明的实施方式作进一步详细描述。以下实施例用于说明本发明，但不能用来限制本发明的范围。
本发明提供一种离子改性的微波介质陶瓷，所述微波介质陶瓷的化学通式为Zn0.15Nb0.3[Ti1-x (W1/3Zr1/2) x ]0.55O2，其中x=0.01~0.03；所述微波介质陶瓷由包括以下重量份数的组分制成：12.58~12.67份ZnO，41.11-41.39份TiO2，43.93~45.14份Nb2O5，0.44~1.31份WO3，以及0.35~1.05份ZrO2。
进一步地，所述微波介质陶瓷的烧结温度为1050~1150oC。
进一步地，作为本发明的优选实施例，所述微波介质陶瓷由包括以下重量份数的组分制成：12.67份ZnO，41.39份TiO2，45.14份Nb2O5，0.441份WO3，0.352份ZrO2。在1100oC烧结温度下，微波介质陶瓷的介电常数为90.8，Q×f值高达14381GHz，τf低至243.8ppm/oC。
本发明还提供了一种离子改性的微波介质陶瓷的制备方法，用于制备上述的离子改性的金红石Zn0.15Nb0.3Ti0.55O2系微波介质陶瓷，所述制备方法包括以下步骤：
配料：将ZnO、TiO2、Nb2O5、WO3、ZrO2的粉料按照化学通式Zn0.15Nb0.3[Ti1-x (W1/ 3Zr1/2) x ]0.55O2进行配料，得到原料粉；
第一次球磨：将配好的原料粉装入球磨罐，选择锆球和去离子水做为研磨介质，并按照原料粉：锆球：去离子水的质量比为1:4~6:2~4的配比进行4~6小时的第一次行星球磨，待球磨结束后，将混合浆料置于烘箱中烘干，随后以80~100目的筛网过筛，将过筛后的粉体于900~1000℃的大气气氛中预烧3~5小时，得到预烧料；
第二次球磨：按照预烧料粉：锆球：去离子水的质量比为1:5~7:3~5的配比，再次进行行星球磨6~8小时，待球磨后的物料烘干后，添加聚乙烯醇溶液作为粘结剂，造粒，得到陶瓷生料；
压制成型：将制得的陶瓷生料压制成型，随后以2~4oC/min的升温速率在600~650℃温度下排胶2~4小时，紧接着再以2~4oC/min的升温速率升温至1050~1150oC，再保温4~6小时，即制得离子改性的金红石Zn0.15Nb0.3[Ti1-x (W1/3Zr1/2) x ]0.55O2系微波介质陶瓷。
为更好的阐述本发明的技术效果，按照上述步骤制作了3份实施例样品。实施例1-3中原料的各组分含量及烧结温度，如表1所示：
表1 实施例1-3中原料的各组分含量及烧结温度
实施例1-3中原料的各组分含量采用的是本申请所提供的微波介质陶瓷中原料的最优配比，并将上述实施例1-3的原料按照本发明提供的制备方法制得了离子改性的金红石Zn0.15Nb0.3Ti0.55O2系微波介质陶瓷。将得到的微波介质陶瓷进行检测，得到了各实施例样品的性能参数及图谱，实施例1-3样品的各项性能参数如表2所示：
表2 实施例1-3样品的各项性能参数
图1为实施例1的XRD衍射图谱，经检索，陶瓷的物相组成为纯金红石Zn0.15Nb0.3Ti0.55O2相，与标准卡片JCPDS79-1186相匹配，除此之外并无多余物相的衍射峰出现，说明(W1/3Zr1/2)4+复合离子成功进入Ti格位并形成固溶体，且制备过程中所添加的掺杂剂并未使物相组成发生改变。图2为实施例2的SEM图谱，从图可知，在1100oC的烧结温度下，试样的晶粒尺寸已经生长充分，表面结构微气孔数量少且气孔率低，说明(W1/3Zr1/2)4+复合离子取代促进了Zn0.15Nb0.3Ti0.55O2陶瓷的烧结致密性。
从表1、表2所展示的数据可以看出，在实施例1-3中，试样的介电常数与品质因数Q×f值与离子改性前的数值相比出现了降低的趋势，τf值则介于243~267ppm/℃，也低于常规的金红石Zn0.15Nb0.3Ti0.55O2系微波介质陶瓷。特别地，在实施例1中，当复合离子的掺杂量为0.01mol时，陶瓷体系的晶体结构未发生改变，为金红石固溶体结构，此时试样的外部烧结致密性高，说明此时材料的微波介电性能更多受制于晶体结构因素，介电常数由纯相的93.1小幅降低至90.8，但此时的Q×f值出现较大幅度的增加趋势，从纯相的11815GHz增加至14381GHz，更重要的是，陶瓷材料的τf值亦得到了一定程度的降低，从346.0ppm/℃降低至243.8ppm/℃。因此(W1/3Zr1/2)4+复合离子的掺入不仅保持了金红石Zn0.15Nb0.3Ti0.55O2陶瓷的高Q×f值的特性，同时亦一定程度的提高了谐振频率的温度稳定性，拓展了Zn0.15Nb0.3Ti0.55O2系陶瓷在电子陶瓷制造领域的实用价值。
本发明的离子改性的金红石Zn0.15Nb0.3[Ti1-x (W1/3Zr1/2) x ]0.55O2系微波介质陶瓷可应用于微波元器件，电子元器件以及通信设备中。
以上参照附图说明了本发明的优选实施例，本领域技术人员不脱离本发明的范围和实质，可以有多种变型方案实现本发明。举例而言，作为一个实施例的部分示出或描述的特征可用于另一实施例以得到又一实施例。以上仅为本发明较佳可行的实施例而已，并非因此局限本发明的权利范围，凡运用本发明说明书及附图内容所作的等效变化，均包含于本发明的权利范围之内。

Claims (6)

1.一种离子改性的微波介质陶瓷，其特征在于，所述微波介质陶瓷的化学通式为Zn0.15Nb0.3[Ti1-x(W1/3Zr1/2)x]0.55O2，其中x＝0.01～0.03；所述微波介质陶瓷由包括以下重量份数的组分制成：12.58～12.67份ZnO，41.11-41.39份TiO2，43.93～45.14份Nb2O5，0.44～1.31份WO3，以及0.35～1.05份ZrO2。
2.根据权利要求1所述的一种离子改性的微波介质陶瓷，其特征在于，所述微波介质陶瓷的烧结温度为1050～1150℃。
3.根据权利要求2所述的一种离子改性的微波介质陶瓷，其特征在于，所述微波介质陶瓷由包括以下重量份数的组分制成：12.67份ZnO，41.39份TiO2，45.14份Nb2O5，0.441份WO3，0.352份ZrO2。
4.根据权利要求3所述的一种离子改性的微波介质陶瓷，其特征在于，在1100℃烧结温度下，微波介质陶瓷的介电常数为90.8，Q×f值高达14381GHz，τf低至243.8ppm/℃。
5.一种离子改性的微波介质陶瓷的制备方法，其特征在于，用于制备如权利要求1～4任一项所述的离子改性的微波介质陶瓷，所述制备方法包括以下步骤：
配料：将ZnO、TiO2、Nb2O5、WO3、ZrO2的粉料按照化学通式Zn0.15Nb0.3[Ti1-x(W1/3Zr1/2)x]0.55O2进行配料，得到原料粉；
第一次球磨：将配好的原料粉装入球磨罐，选择锆球和去离子水做为研磨介质，并按照原料粉：锆球：去离子水的质量比为1:4～6:2～4的配比进行4～6小时的第一次行星球磨，待球磨结束后，将混合浆料置于烘箱中烘干，随后以80～100目的筛网过筛，将过筛后的粉体于900～1000℃的大气气氛中预烧3～5小时，得到预烧料；
第二次球磨：按照预烧料粉：锆球：去离子水的质量比为1:5～7:3～5的配比，进行第二次行星球磨6～8小时，待球磨后的物料烘干后，添加聚乙烯醇溶液作为粘结剂，造粒，得到陶瓷生料；
压制成型：将制得的陶瓷生料压制成型，随后以2～4℃/min的升温速率在600～650℃温度下排胶2～4小时，紧接着再以2～4℃/min的升温速率升温至1050～1150℃，再保温4～6小时，即制得离子改性的金红石Zn0.15Nb0.3[Ti1-x(W1/3Zr1/2)x]0.55O2系微波介质陶瓷。
6.一种微波元器件，其特征在于，其采用如权利要求1-4任一项所述的离子改性的微波介质陶瓷制成。
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