CN117585994A - 现代通信用超低介电常数微波介质材料及其制备方法 - Google Patents
现代通信用超低介电常数微波介质材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种现代通信用超低介电常数微波介质材料及其制备方法，属于微波介质材料制备工艺技术领域。发明通过调整主要组分和微量添加剂的比例，改善微波介质材料的电性能，在本发明的制备工艺条件下，可以得到εr接近6、Τf≈±10ppm/℃、品质因数符合要求的超低微波介质材料，为更高频率微波器件的开发提供一个全新的材料基础，满足6～9GHz及以上更高频段的通信要求。
Description
技术领域
本发明涉及微波介质材料制备工艺技术领域，具体为现代通信用超低介电常数微波介质材料及其制备方法。
背景技术
众所周知，半导体等电子元器件的发展，材料和工艺是基础，微波介质陶瓷(MWDC)材料，是指应用于微波频段电路中作为介质材料并完成一种或多种功能的功能陶瓷材料，以其优异的微波介电性能在微波电路***中发挥着介质隔离、介质传导以及介质谐振等重要功能。在现代通讯中被广泛用于谐振器、滤波器、双工器、介质基板等微波元器件的生产中。例如，介质谐振器、介质滤波器、介质双工(多工)器、卫星授时天线等均是现代通信的重要元器件。基于优异的微波电性能，微波介质陶瓷元器件被广泛应用于移动通信、卫星通讯、卫星导航与定位、航空航天、汽车电子、物联网等领域。
随着第五代无线通信，即5G的发展，以及即将到来的6G发展时代，对现代通讯技术中的关键基础材料——微波介质陶瓷材料的要求越来越高，在要求品质因数Q尽可能高、频率温度系数τf尽可能小的同时，也要求介电常数εr向着更高和超低两个方向发展，以满足不同频段的通信要求。
εr＝5.8左右的超低介电常数的微波介质材料在国际上还未面世或应用。本发明是在这种背景下开发成功的，以满足6～9GHz及以上更高频段的通信要求。
发明内容
本发明提供了现代通信用超低介电常数微波介质材料及其制备方法，是一种Mg-Al-Ba-Si***的复合型微波介质材料及其制备方法。
本发明是通过以下技术方案实现的：
现代通信用超低介电常数微波介质材料，按重量百分比wt％包括如下组分：
其余为改性添加剂。
所述微量添加剂包括矾的化合物、铈的化合物、锰的化合物等。
所述微量添加剂为五氧化二钒。
现代通信用超低介电常数微波介质材料的制备方法，包括如下步骤：
步骤a、根据上述组分配方，准确称量各种原料并倒入树脂球磨罐内，加入去离子水和ZrO2磨球，二者比重为：原料/去离子水＝1/3；
步骤b、然后将树脂球磨罐放到行星球磨机上球磨，以300r/min转速连续球磨6小时，出料后将浆料放入烘箱中，在80～120℃下烘干；
步骤c、烘干后的物料在1000～1250℃下预烧2小时，再将煅烧后的料粉倒入树脂球磨罐中，加入去离子水，二者比重为料粉：水＝1：2，进行二次球磨，以300r/min转速连续球磨6小时，出料后烘干；
步骤d、将烘干后的物料粉碎后过60目筛，得到粒度均匀的粉体；
步骤e、在粉体中加入14～17％粉体质量的浓度为10wt％的聚乙烯醇粘合剂，进行造粒，在研钵中研磨均匀后，取60目～120目粒度的料粉，在130Mpa左右压力下干压成型；
步骤f、成型后在450-500℃保温2小时进行充分排胶，然后以3℃/min的升温速率，在1150～1300℃下烧结4小时，最终制得介电常数在5-6.5左右的新型超低微波介质材料。
与现有技术相比，本发明的有益效果是：
本发明通过调整主要组分和微量添加剂的比例，改善微波介质材料的电性能，在本发明的制备工艺条件下，可以得到εr接近6、τf≈±10ppm/℃、品质因数符合要求的超低微波介质材料，为更高频率微波器件的开发提供一个全新的材料基础，满足6～9GHz及以上更高频段的通信要求。
附图说明
图1为本发明中材料的介电常数与SiO2含量的关系图；
图2为本发明中材料的温漂系数与SiO2含量的关系图。
具体实施方式
下面结合附图对本发明进一步说明：
现代通信用超低介电常数微波介质材料，按重量百分比wt％包括如下组分：
其余为改性添加剂。
所述微量添加剂包括矾的化合物、铈的化合物、锰的化合物等。
所述微量添加剂为五氧化二钒。
现代通信用超低介电常数微波介质材料的制备方法，包括如下步骤：
步骤a、根据上述组分配方，准确称量各种原料并倒入树脂球磨罐内，加入去离子水和ZrO2磨球，二者比重为：原料/去离子水＝1/3；
步骤b、然后将树脂球磨罐放到行星球磨机上球磨，以300r/min转速连续球磨6小时，出料后将浆料放入烘箱中，在80～120℃下烘干；
步骤c、烘干后的物料在1000～1250℃下预烧2小时，再将煅烧后的料粉倒入树脂球磨罐中，加入去离子水，二者比重为料粉：水＝1：2，进行二次球磨，以300r/min转速连续球磨6小时，出料后烘干；
步骤d、将烘干后的物料粉碎后过60目筛，得到粒度均匀的粉体；
步骤e、在粉体中加入14～17％粉体质量的浓度为10wt％的聚乙烯醇粘合剂，进行造粒，在研钵中研磨均匀后，取60目～120目粒度的料粉，在130Mpa左右压力下干压成型；
步骤f、成型后在450-500℃保温2小时进行充分排胶，然后以3℃/min的升温速率，在1150～1300℃下烧结4小时，最终制得介电常数在5-6.5左右的新型超低微波介质材料。
实施例
表1
按照表1中的组分配方，分别制得5个样品，制备方法如下：准确称量各种原料并倒入树脂球磨罐内，加入去离子水和ZrO2磨球，二者比重为：料：水＝1：3，然后放到行星球磨机上球磨，300r/min转速连续球磨6小时，出料后将浆料放入烘箱中，在80～120℃下烘干，然后在1000～1250℃下预烧2小时，再将煅烧后的料粉倒入树脂球磨罐中，加入去离子水，二者比重为料：水＝1：2，进行二次球磨，300r/min转速连续球磨6小时，出料后烘干，粉碎后过60目筛，得到粒度均匀的粉体；在粉体中加入14～17％粉体质量的浓度为10wt％的聚乙烯醇粘合剂，进行造粒，在研钵中研磨均匀后，取60目～120目粒度的料粉，在130Mpa左右压力下干压成型；成型后在500℃左右保温2小时以排胶，然后以3℃/min的升温速率，在1150～1300℃下烧结4小时。出炉后，按照测试要求研磨到规定尺寸，并将材料制成DR6×6谐振器，用安捷伦E5071C矢量网络分析仪测试。
测试结果如表2所示：
表2
Τf的测试范围为-45℃～85℃。
如说明书附图图1所示，随着主要组分SiO2的改变，所得微波材料的介电常数εr会发生变化。
如说明书附图图2所示，随着主要组分SiO2的改变，温漂系数τf发生变化，微量添加剂对改善τf的效果很明显。
在本发明的制备工艺条件下，可以得到εr接近6、τf≈±10ppm/℃、品质因数符合要求的超低微波介质材料，为更高频率微波器件的开发提供一个全新的材料基础，满足6～9GHz及以上更高频段的通信要求。
在本发明中，除非另有明确的规定和限定，术语“安装”、“设置”、“连接”、“固定”、“旋接”等术语应做广义理解，例如，可以是固定连接，也可以是可拆卸连接，或成一体；可以是机械连接，也可以是电连接；可以是直接相连，也可以通过中间媒介间接相连，可以是两个元件内部的连通或两个元件的相互作用关系，除非另有明确的限定，对于本领域的普通技术人员而言，可以根据具体情况理解上述术语在本发明中的具体含义。
综上所述，仅为本发明的较佳实施例而已，并非用来限定本发明实施的范围，凡依本发明权利要求范围所述的形状、构造、特征及精神所为的均等变化与修饰，均应包括于本发明的权利要求范围内。
Claims (4)
1.现代通信用超低介电常数微波介质材料，其特征在于：按重量百分比wt％包括如下组分：
其余为改性添加剂。
2.根据权利要求1所述的现代通信用超低介电常数微波介质材料，其特征在于：所述微量添加剂包括矾的化合物、铈的化合物、锰的化合物等。
3.根据权利要求1所述的现代通信用超低介电常数微波介质材料，其特征在于：所述微量添加剂为五氧化二钒。
4.根据权利要求1所述的现代通信用超低介电常数微波介质材料的制备方法，其特征在于：包括如下步骤：
步骤a、根据上述组分配方，准确称量各种原料并倒入树脂球磨罐内，加入去离子水和ZrO2磨球，二者比重为：原料/去离子水＝1/3；
步骤b、然后将树脂球磨罐放到行星球磨机上球磨，以300r/min转速连续球磨6小时，出料后将浆料放入烘箱中，在80～120℃下烘干；
步骤c、烘干后的物料在1000～1250℃下预烧2小时，再将煅烧后的料粉倒入树脂球磨罐中，加入去离子水，二者比重为料粉：水＝1：2，进行二次球磨，以300r/min转速连续球磨6小时，出料后烘干；
步骤d、将烘干后的物料粉碎后过60目筛，得到粒度均匀的粉体；
步骤e、在粉体中加入14～17％粉体质量的浓度为10wt％的聚乙烯醇粘合剂，进行造粒，在研钵中研磨均匀后，取60目～120目粒度的料粉，在130Mpa左右压力下干压成型；
步骤f、成型后在450-500℃保温2小时进行充分排胶，然后以3℃/min的升温速率，在1150～1300℃下烧结4小时，最终制得介电常数在5-6.5左右的新型超低微波介质材料。
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