CN113480303B - 一种铝酸盐基低介微波介质陶瓷及其制备方法 - Google Patents

一种铝酸盐基低介微波介质陶瓷及其制备方法 Download PDF

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CN113480303B
CN113480303B CN202110850519.9A CN202110850519A CN113480303B CN 113480303 B CN113480303 B CN 113480303B CN 202110850519 A CN202110850519 A CN 202110850519A CN 113480303 B CN113480303 B CN 113480303B
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宋小强
雷文
吕文中
付明
王晓川
梁飞
汪小红
范桂芬
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Wenzhou Institute Of Advanced Manufacturing Technology Huazhong University Of Science And Technology
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Abstract

本发明公开了一种铝酸盐基低介电常数微波介质陶瓷及其制备方法，其中微波介质陶瓷的主晶相具有石榴石型晶体结构，具体化学组成为(2+x)CaO‑0.5Ln2O3‑(2‑y)ZrO2‑(x+y)MO2‑1.5Al2O3，Ln为Y、La、Lu、Gd或其它镧系元素，M为Hf、Sn或Ti，0≤x≤0.5，0≤y≤2.0。微波介质陶瓷的介电常数为10.81～13.52，品质因数为72441GHz～121930GHz，谐振频率温度系数为+0.50ppm/℃～‑35.48ppm/℃。在制备过程中陶瓷材料预烧条件为1300℃保温5小时，烧结条件为1500℃～1600℃保温10小时。本发明中制备得到的微波介质陶瓷具有低介电常数、高品质因数、谐振频率温度系数可调控至近零的特点，适合用于制备介质基板、介质谐振器、介质天线等微波通讯器件。

Description

一种铝酸盐基低介微波介质陶瓷及其制备方法
技术领域
本发明属于微波介质陶瓷技术领域，更具体地，涉及一种铝酸盐基低介微波介质陶瓷及其制备方法。
背景技术
微波介质陶瓷是制备高频电容、介质基板、介质波导滤波器、介质天线等无源器件的基础材料，因而广泛应用于各种无线通讯***中。随着5G通讯逐渐进入商用阶段，通信设备的集成度与工作频率不断提高，信号时延、信号串扰、***发热等问题日益凸显。低介电常数、低介电损耗微波介质陶瓷能有效提高微波信号的传输速率，降低信号能量损失，符合5G等微波毫米波通讯的需求，因此逐渐成为学术界与工业界关注的焦点，开发新型低介微波介质陶瓷正当其时。
发明内容
针对现有技术中存在的不足之处，本发明提供了一种铝酸盐基低介微波介质陶瓷及其制备方法，由此缓解微波通讯技术中存在的高信号时延、高能量损耗、高***发热等问题。
为实现上述目的，本发明提供了一种铝酸盐基低介微波介质陶瓷及其制备方法，陶瓷主晶相的化学式为(2+x)CaO-0.5Ln 2O3-(2-y)ZrO2-(x+y)MO2-1.5Al2O3，其中Ln为Y、La、Lu、Gd或其它镧系元素，M为Hf、Sn或Ti，0≤x≤0.5，0≤y≤2.0。
进一步地，微波介质陶瓷的介电常数为10.81~13.52。
进一步地，微波介质陶瓷的品质因数为72441GHz ~121930GHz。
进一步地，微波介质陶瓷的谐振频率温度系数为+0.50ppm/℃~-35.48ppm/℃。
本发明提供了一种铝酸盐基低介微波介质陶瓷的制备方法，包括：
（1）将CaCO3、Ln 2O3、ZrO2、MO2、及Al2O3按化学式(2+x)CaO-0.5Ln 2O3-(2-y)ZrO2-(x+y)MO2-1.5Al2O3进行配料，得到混合原料，其中，Ln为Y、La、Lu、Gd或其它镧系元素，M为Hf、Sn或Ti，0≤x≤0.5，0≤y≤2.0，对混合原料依次进行球磨、干燥、过筛，得到颗粒均匀的粉料；
（2）将粉料在1300℃下预烧5小时，得到预烧粉料，对预烧粉料依次进行球磨、干燥、过筛，得到预烧陶瓷粉体，利用粘结剂对预烧陶瓷粉体进行造粒后加压成型，得到陶瓷坯体，将陶瓷坯体在1500℃~1600℃下烧结10小时，得到微波介质陶瓷。
进一步地，球磨的具体实现方式为：
将混合原料和无水乙醇加入装有锆球的聚酯球磨罐中，在行星式球磨机中球磨16小时。
进一步地，干燥的具体实现方式为：
将球磨后的混合原料置于90℃的鼓风干燥箱中干燥24 h。
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）本发明制备得到的铝酸盐基低介微波介质陶瓷的介电常数为10.81~13.52，可提高微波信号的在介质中的传输速率，缓解信号时延问题。
（2）本发明制备的铝酸盐基低介微波介质陶瓷不仅具有低介电常数，还具有高的品质因数，同时谐振频率温度系数可调控至近零。由此可见本发明制备得到的微波介质陶瓷性能良好，可以用于介质波导滤波器、介质谐振器及介质天线等微波通讯器件中。
（3）本发明制备步骤中依次进行球磨、干燥、过筛，是为了使原料混合均匀，同时细化粉料颗粒，在适中温度烧结后制备得到的微波介质陶瓷质量较好。
附图说明
图1是本发明实施例提供的一种铝酸盐基低介微波介质陶瓷的制备方法的流程图。
图2是本发明实施例提供的铝酸盐基低介微波介质陶样品X射线衍射图谱。
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，以下结合附图及实施例，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。
如图1所示，一种铝酸盐基低介微波介质陶瓷的制备方法，包括：
（1）将纯度为99.5%以上的CaCO3、Ln 2O3、ZrO2、MO2、及Al2O3按化学式(2+x)CaO-0.5Ln 2O3-(2-y)ZrO2-(x+y)MO2-1.5Al2O3进行配料，得到混合原料，其中，Ln为Y、La、Lu、Gd或其它镧系元素，M为Hf、Sn或Ti，0≤x≤0.5，0≤y≤2.0，对混合原料依次进行球磨、干燥、过筛，得到颗粒均匀的粉料；
（2）将（1）中混合均匀的原材料在1300℃下预烧5小时，得到预烧粉料，对预烧粉料依次进行球磨、干燥、过筛，得到预烧陶瓷粉体，利用粘结剂对预烧陶瓷粉体进行造粒后加压成型，得到陶瓷坯体，将陶瓷坯体在1500℃~1600℃下烧结10h，得到微波介质陶瓷。
本发明实施例优选的，球磨、干燥、过筛的具体实现方式为：
按照1：1.6的质量比将混合原料与无水乙醇分别加入装有锆球的聚酯球磨罐中，在行星式球磨机中球磨16小时。将球磨后的混合原料置于90℃的鼓风干燥箱中干燥24小时。将干燥后的混合原料过40目筛。
本发明实施例优选的，粘结剂为质量分数5%的PVA水溶液，粘结剂添加量为粉料质量的8wt%，加压成型时压力为150MPa，陶瓷坯体的直径为12mm，陶瓷坯体的高度6mm。
表1为本发明实施例1-11制备时的配方以及制备得到的铝酸盐基低介微波介质陶瓷的性能参数。
表1 实施例1-11的微波介电性能
Figure DEST_PATH_IMAGE002
为测试实施例1-11制备的微波介质陶瓷的微波介电性能，首先将实施例1-11制备的微波介质陶瓷在600目金刚石磨盘上打磨，然后在去离子水中超声清洗，最后放置于90℃的鼓风干燥箱中干燥24小时。采用平行板谐振腔法分析样品介电性能，测试频率在9GHz ~12GHz。通过测量平行板谐振器的谐振频率随温度的变化率得到样品的谐振频率温度系数，测量温度范围为30℃~80℃。可以看出，本发明实施例制备得到的微波介质陶瓷的介电常数为10.81~13.52，品质因数为72441GHz ~121930GHz，谐振频率温度系数为+0.50ppm/℃~-35.48ppm/℃。
在 Ln=Y，M=Ti的情况下，当x=0.19, y=0.3时，本发明实施例7制备得到的微波介质陶瓷满足低介电常数、高品质因数、谐振频率温度系数近零的使用要求，可用于制备高频电容、介质波导滤波器、介质谐振器及介质天线等电子元器件。
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 (2)

1.一种铝酸盐基低介微波介质陶瓷，其特征在于：陶瓷主晶相的化学式为(2+x)CaO-0.5Ln 2O3-(2-y)ZrO2-(x+y)MO2-1.5Al2O3，其中Ln为Y、La、Lu、或Gd元素，M为Hf、Sn或Ti，0≤x≤0.5，0≤y≤2.0；所述陶瓷的介电常数为10.81~13.52，品质因数为72441GHz~121930GHz，谐振频率温度系数为+0.50ppm/℃~-35.48ppm/℃。
2.如权利要求1所述的一种铝酸盐基低介微波介质陶瓷的制备方法，制备步骤如下：
(1) 将CaCO3、Ln 2O3、ZrO2、MO2及Al2O3按权利要求1中的化学式进行配料称量，然后将称量后的原料依次倒入球磨罐中得到混合原料；
(2) 在球磨罐中加入粉料质量1.6倍的无水乙醇，在行星式球磨机上按照360r/min的转速球磨16小时，然后将球磨后的浆料在90℃烘箱中放置24小时，待粉料完全干燥后过40目尼龙筛；
(3) 将过筛后的粉料倒入刚玉坩埚中，然后在高温炉中1300℃预烧5小时，得到预烧后的粉料；
(4) 将预烧后的粉料按照上述步骤再次进行球磨、干燥、过筛，然后加入8wt%的粘结剂对粉料进行造粒，最后施加150MPa 压力加压成型，得到陶瓷坯体；
(5) 将陶瓷坯体在1500℃~1600℃下烧结10小时，得到微波介质陶瓷。
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