CN114874005B - 温度稳定型钛酸镁基微波介质复合陶瓷及其制备方法 - Google Patents

温度稳定型钛酸镁基微波介质复合陶瓷及其制备方法 Download PDF

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CN114874005B
CN114874005B CN202210655936.2A CN202210655936A CN114874005B CN 114874005 B CN114874005 B CN 114874005B CN 202210655936 A CN202210655936 A CN 202210655936A CN 114874005 B CN114874005 B CN 114874005B
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马建立
刘晓佳
杨忠意
付志粉
朱何平
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Abstract

本发明公开了温度稳定型钛酸镁基微波介质复合陶瓷及其制备方法，制备的方法步骤如下：S1：Mg2TiO4预烧粉的制备：将MgO和TiO2按Mg2TiO4的化学计量比与无水乙醇混合球磨，经干燥、预烧后制得Mg2TiO4预烧粉；S2：LiF‑CaF2‑B2O3烧结助剂粉的制备：将LiF、CaF2和B2O3按1:1‑3:1‑3的比例混合研磨制得LiF‑CaF2‑B2O3烧结助剂粉；S3：钛酸镁基微波介质复合陶瓷的制备：将S1的Mg2TiO4预烧粉与S2的LiF‑CaF2‑B2O3烧结助剂粉与无水乙醇混合，经干燥、造粒、过筛、压片、烧结，制得钛酸镁基微波介质复合陶瓷。本发明克服了钛酸镁基微波介质复合陶瓷烧结温度高、谐振频率温度系数偏大的缺点，保证材料温度稳定性的同时降低了烧结温度，满足了当前高频通信设备对较好的工作环境温度稳定性和Q值较高的低介电常数材料的要求。

Description

温度稳定型钛酸镁基微波介质复合陶瓷及其制备方法
技术领域
本发明涉及复合陶瓷技术领域，尤其涉及温度稳定型钛酸镁基微波介质复合陶瓷及其制备方法。
背景技术
对于Mg2TiO4微波介质陶瓷材料来说，其温度稳定性为负值，为了提高该材料的稳定性，现有的常用温度稳定性为正值的材料如CaTiO3来微波介质陶瓷材料的温度稳定性；但是由于CaTiO3本身损耗较大且烧结温度较高(1350℃)，在调控其温度稳定性的同时极大增大了损耗，严重损害了其品质因数，且无法改善Mg2TiO4微波介质陶瓷材料(烧结温度1450-1500℃)的烧结性能。因此，亟需开发一种新的钛酸镁基微波介质复合陶瓷的制备工艺以在提高温度稳定性的同时改善其烧结性能。
发明内容
基于背景技术存在的技术问题，本发明提出了温度稳定型钛酸镁基微波介质复合陶瓷及其制备方法，克服了钛酸镁基微波介质复合陶瓷烧结温度高、谐振频率温度系数偏大的缺点，保证材料温度稳定性的同时降低了烧结温度，满足了当前高频通信设备对较好的工作环境温度稳定性和Q值较高的低介电常数材料的要求。
本发明提出的温度稳定型钛酸镁基微波介质复合陶瓷的制备方法，方法步骤如下：
S1：Mg2TiO4预烧粉的制备；
S2：LiF-CaF2-B2O3烧结助剂粉的制备
将LiF、CaF2和B2O3混合研磨制得LiF-CaF2-B2O3烧结助剂粉；
S3：钛酸镁基微波介质复合陶瓷的制备
将S1的Mg2TiO4预烧粉与S2的LiF-CaF2-B2O3烧结助剂粉与无水乙醇混合，经干燥、造粒、过筛、压片、烧结，制得钛酸镁基微波介质复合陶瓷。
优选地，所述S1中Mg2TiO4预烧粉制备的方法步骤如下：将MgO和TiO2按Mg2TiO4的化学计量比与无水乙醇混合球磨，经干燥、预烧后制得Mg2TiO4预烧粉。
优选地，干燥的温度80-100℃、时间10-12h；预烧的温度1000-1100℃、时间4-6h。
优选地，所述LiF、CaF2和B2O3的摩尔比为1:1-3:1-3。
优选地，所述S3中Mg2TiO4预烧粉与LiF-CaF2-B2O3烧结助剂粉的质量比为(100-x):x，其中6≤x≤9。
优选地，所述S3中烧结温度1150-1200℃、时间4-8h。
本发明提出的上述方法制备的温度稳定型钛酸镁基微波介质复合陶瓷。
优选地，包括含如下重量百分比计的物相组成：
Mg2TiO4 84.9-94.8％；
CaTiO3 5.2-8.6％；
其余为Mg3B2O6。
优选地，所述复合陶瓷的介电损耗为0.000214～0.000295，品质因数为23950～34110GHz，介电常数为15.2～15.4，谐振频率温度系数为-4.4～2.82ppm/℃。
本发明提出的上述温度稳定型钛酸镁基微波介质复合陶瓷在微波器件中的应用。
作用机理
本发明通过在Mg2TiO4陶瓷中加入低烧结温度的复合烧结助剂LiF-CaF2-B2O3，并控制其配比和调控后期烧结工艺过程，促进其中的CaF2和B2O3分别和基体材料中小部分Mg2TiO4发生化学反应，得到了CaTiO3和Mg3B2O6，也就得到了陶瓷中主要的组成成分：Mg2TiO4，CaTiO3和Mg3B2O6，正是通过这一反应，在降低Mg2TiO4陶瓷的烧结温度的同时，显著地提高了Mg2TiO4陶瓷材料的温度稳定性，获得了一种具有良好微波介电性能的新材料。
本发明的有益技术效果：
(1)本发明温度稳定型钛酸镁基微波介质复合陶瓷微波性能良好(介电损耗为0.000214～0.000295，品质因数为23950GHz～34110GHz，介电常数为15.2～15.4，谐振频率温度系数为-4.4～2.82ppm/℃，烧结温度为1150～1200℃)，克服了陶瓷材料烧结温度高、谐振频率温度系数偏大的缺点，保证材料温度稳定性的同时降低了烧结温度，满足了当前高频通信设备对较好的工作环境温度稳定性和Q值较高的低介电常数材料的要求。
(2)本发明温度稳定型钛酸镁基微波介质复合陶瓷材料制备方法简单，所用原料来源丰富、成本低廉，适合大规模生产，可广泛应用于LTCC系统、GPS天线、WIFI滤波器、多层介质谐振器等微波器件的制造。
附图说明
图1为本发明提出的实施例1-7制备的温度稳定型钛酸镁基微波介质复合陶瓷的X射线粉末衍射图。
具体实施方式
实施例1
(1)制备Mg2TiO4预烧粉
按照Mg2TiO4的化学计量比称取19.091g纯度为99.99％的MgO、18.949g纯度为99.8％的TiO2，与无水乙醇混合球磨，8小时，90℃干燥12h后在1100℃条件下预烧4h，制备成Mg2TiO4预烧粉。
(2)制备LiF-CaF2-B2O3烧结助剂粉
称取0.075g纯度为99.99％的LiF、0.451g纯度为99.99％的CaF2和0.403g纯度为99.9％的B2O3，放入研钵中研磨0.5～1小时，制备成LiF-CaF2-B2O3烧结助剂粉。
(3)制备钛酸镁基微波介质复合陶瓷
称取30g Mg2TiO4预烧粉和2.432g LiF-CaF2-B2O3烧结助剂粉，与无水乙醇混合，经干燥、造粒、过筛、压片(直径11.5mm、厚度6mm)、烧结(温度1175℃、时间6小时)，制得钛酸镁基微波介质复合陶瓷。
实施例2
本实施例的步骤(3)中，将生坯1175℃烧结4小时，其余条件与实施例1相同。
实施例3
本实施例的步骤(3)中，将生坯1175℃烧结8小时，其余条件与实施例1相同。
实施例4
本实施例的步骤(3)中，将生坯1150℃烧结6小时，其余条件与实施例1相同。
实施例5
本实施例的步骤(3)中，将生坯1200℃烧结6小时，其余条件与实施例1相同。
实施例6
本实施例的步骤(3)中，称取30g Mg2TiO4预烧粉和1.915g LiF-CaF2-B2O3烧结助剂粉，其余条件与实施例1相同。
实施例7
本实施例的步骤(3)中，称取30g Mg2TiO4预烧粉和2.967g LiF-CaF2-B2O3烧结助剂粉，其余条件与实施例1相同。
对比例1
(1)按照Mg2TiO4的化学计量比称取19.091g纯度为99.99％的MgO、18.949g纯度为99.8％的TiO2，与无水乙醇混合球磨，8小时，90℃干燥12h后在1100℃条件下预烧4h，制备成Mg2TiO4预烧粉。
(2)称取30g Mg2TiO4预烧粉和2.432g纯度为99.9％的B2O3，与无水乙醇混合，经干燥、造粒、过筛、压片(直径11.5mm、厚度6mm)、烧结(温度1175℃、时间6小时)，制备钛酸镁基微波介质陶瓷。
对比例2
(1)按照Mg2TiO4的化学计量比称取19.091g纯度为99.99％的MgO、18.949g纯度为99.8％的TiO2，与无水乙醇混合球磨，8小时，90℃干燥12h后在1100℃条件下预烧4h，制备成Mg2TiO4预烧粉。
(2)称取30g Mg2TiO4预烧粉和2.432g纯度为99.99％的CaF2，与无水乙醇混合，经干燥、造粒、过筛、压片(直径11.5mm、厚度6mm)、烧结(温度1175℃、时间6小时)，制备钛酸镁基微波介质陶瓷。
采用Smartlab型X射线衍射仪对上述实施例得到的钛酸镁基微波介质复合陶瓷进行表征，结果见图1。由图1可知，所制备的陶瓷材料由四方结构Mg2TiO4相，正交结构的CaTiO3相和正交结构的Mg3B2O6相所组成，各物质的各物相的质量百分含量见表1。
表1微波介质陶瓷材料的物相组成
Figure BDA0003687677940000041
Figure BDA0003687677940000051
将实施例1-7制备的温度稳定型钛酸镁基微波介质复合陶瓷以及对比例1-2制备的钛酸镁基陶瓷研磨抛光后加工成直径为11.5mm、高5.5～6.5mm的圆柱，采用闭腔谐振法，用ZVB20矢量网络分析仪(由德国罗德&施瓦茨公司生产)配合高低温箱，对陶瓷材料进行微波介电性能测试，测试结果与现有文献报道的添加3wt％LiF的(Mg0.95Zn0.05)2(Ti0.8Sn0.2)O4(Effects of LiF addition on sintering behavior and microwave dielectricproperties of(Mg0.95Zn0.05)2(Ti0.8Sn0.2)O4 ceramics.Ceramics International,2012,38(3):2239-2242)陶瓷材料的微波介电性能进行对比，结果见表2。
表2不同材料的微波介电性能对比
Figure BDA0003687677940000052
由表2可知，本发明的温度稳定型钛酸镁基微波介质复合陶瓷微波性能良好(介电损耗为0.000214～0.000295，品质因数为23950GHz～34110GHz，介电常数为15.2～15.4，谐振频率温度系数为-4.4～2.82ppm/℃，烧结温度为1150～1200℃)，克服了陶瓷材料烧结温度高、谐振频率温度系数偏大的缺点，保证材料温度稳定性的同时降低了烧结温度，满足了当前高频通信设备对较好的工作环境温度稳定性和Q值较高的低介电常数材料的要求。
以上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、改进等，均应包含在本发明的保护范围之内。

Claims (7)

1.温度稳定型钛酸镁基微波介质复合陶瓷的制备方法，其特征在于，方法步骤如下：
S1：Mg2TiO4预烧粉的制备；
S2：LiF-CaF2-B2O3烧结助剂粉的制备
将LiF、CaF2和B2O3混合研磨制得LiF-CaF2-B2O3烧结助剂粉；
S3：钛酸镁基微波介质复合陶瓷的制备
将S1的Mg2TiO4预烧粉与S2的LiF-CaF2-B2O3烧结助剂粉与无水乙醇混合，经干燥、造粒、过筛、压片、烧结，制得钛酸镁基微波介质复合陶瓷；
所述LiF、CaF2和B2O3的摩尔比为1:1-3:1-3；
所述S3中Mg2TiO4预烧粉与LiF-CaF2-B2O3烧结助剂粉的质量比为(100-x):x，其中6≤x≤9；
所述S3中烧结温度1150-1200℃、时间4-8h。
2.根据权利要求1所述的温度稳定型钛酸镁基微波介质复合陶瓷的制备方法，其特征在于，所述S1中Mg2TiO4预烧粉制备的方法步骤如下：将MgO和TiO2按Mg2TiO4的化学计量比与无水乙醇混合球磨，经干燥、预烧后制得Mg2TiO4预烧粉。
3.根据权利要求2所述的温度稳定型钛酸镁基微波介质复合陶瓷的制备方法，其特征在于，干燥的温度80-100℃、时间10-12h；预烧的温度1000-1100℃、时间4-6h。
4.如权利要求1-3任一项所述方法制备的温度稳定型钛酸镁基微波介质复合陶瓷。
5.根据权利要求4所述的温度稳定型钛酸镁基微波介质复合陶瓷，其特征在于，包括含如下重量百分比计的物相组成：
Mg2TiO484.9-94.8％；
CaTiO35.2-8.6％；
其余为Mg3B2O6。
6.根据权利要求4所述的温度稳定型钛酸镁基微波介质复合陶瓷，其特征在于，所述复合陶瓷的介电损耗为0.000214～0.000295，品质因数为23950～34110GHz，介电常数为15.2～15.4，谐振频率温度系数为-4.4～2.82ppm/℃。
7.如权利要求4-6任一项所述的温度稳定型钛酸镁基微波介质复合陶瓷在微波器件中的应用。
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