CN111848132A - 易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料及其制备方法 - Google Patents

易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料及其制备方法 Download PDF

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CN111848132A
CN111848132A CN202010748520.6A CN202010748520A CN111848132A CN 111848132 A CN111848132 A CN 111848132A CN 202010748520 A CN202010748520 A CN 202010748520A CN 111848132 A CN111848132 A CN 111848132A
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zirconia balls
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刘成
张洪阳
杨青慧
金立川
李元勋
张怀武
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University of Electronic Science and Technology of China
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Abstract

本发明公开一种易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料及其制备方法，化学式为Li3(Mg1‑xZnx)2SbO6，其中0.02≤x≤0.08。制备方法：第一步，将Sb2O3、Li2CO3按照化学配比混合球磨后烘干，预烧后获得Li3SbO4相；第二步，将MgO、ZnO和Li3SbO4粉体按照Li3(Mg1‑xZnx)2SbO6的化学配比进行混合球磨后烘干，然后加入粘合剂后造粒过筛并压制成圆柱状坯体，于空气中在1325℃下常压烧结成瓷，介电常数为7.2～8.5，品质因数为51844～97719GHz，谐振频率温度系数为‑14～‑1ppm/℃。该微波介质陶瓷体系在5G通信微波器件领域具有广阔的应用前景。

Description

易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料及其制备方法
技术领域
本发明属于电子信息功能陶瓷材料与电子器件技术领域，具体涉及到用于微波介质基板与集成器件等领域。
背景技术
随着无线通信集成化、小型化、高频化特别是5G通信技术的发展，人们对广泛应用于天线、谐振器、基板、滤波器等部件的各种材料提出了新的要求。目前广泛采用的微波介质陶瓷材料虽然能够满足以上各类电子元器件对性能的要求，但随着移动通信技术的进一步升级以及各类移动通信设备的更新换代和普及，需要研发出一类具有低介电常数(减小介质与电极之间的交互耦合损耗，并提高信号传输速率)、低损耗(提高器件工作频率的可选择性)、近零的谐振温度系数(提高器件的频率温度稳定特性)且易于制备的新型微波介质陶瓷材料体系。国内外相关公司及研究机构针对新型微波介质材料的探索已成为目前电子信息功能陶瓷领域的研发热点之一。因此，开发出一种信号响应速度快、损耗小、工作环境温度适应性强、能够广泛应用于移动通讯、雷达及卫星通信等领域，且满足5G通信需求的微波介质陶瓷材料是实现上述技术的关键。本发明所提供的一种易烧结高Q值微波介质陶瓷材料具有品质因数较高、介电常数较低、温度稳定性好的特点，有助于进一步丰富此类产品的需求。
发明内容
本发明所要解决的技术问题是，针对纯相Li3Mg2SbO6微波介质陶瓷难于烧结的特点，开发一种易烧结的高Q值Li3Mg2SbO6基微波介质陶瓷材料，满足日益增长的无线通信元器件需求。该体系具有易于制备、介电常数小、品质因数高、温度稳定性优异等特点，为微波介质元器件向高频化、集成化发展提供了一种有效解决方案。
为实现上述发明目的，本发明技术方案如下：
一种易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料，该陶瓷材料的化学式为Li3(Mg1-xZnx)2SbO6，其中0.02≤x≤0.08，制备方法采用固相反应法进行两步烧结：
(1)将Sb2O3、Li2CO3按照Li3SbO4化学配比混合球磨后烘干，预烧后获得Li3SbO4微波介质相；
(2)以MgO、ZnO和上述制备的Li3SbO4微波介质相，按照分子式Li3(Mg1-xZnx)2SbO6配制，0.02≤x≤0.08，进行混合球磨后烘干，然后加入粘合剂后造粒过筛并压制成圆柱状坯体，于空气中常压下烧结成瓷。
作为优选方式，该微波介质陶瓷介电常数为7.2～8.5，品质因数为51844～97719GHz，谐振频率温度系数为-14～-1ppm/℃。
作为优选方式，步骤(1)进一步为：
(1.1)以纯度为99％的Li2CO3、Sb2O3为原料，按照Li3SbO4化学配比得到Li3SbO4粉体；
(1.2)将上述粉体混合均匀，以纯水为分散剂、氧化锆球为球磨介质，其中氧化锆球的直径为3～15mm，按照原料：纯水：氧化锆球的重量比为1:2:1.5，采用湿磨法混合8小时，出料后在120℃下烘干，过80目筛后以2℃/min的升温速率由室温升温至900℃保温4小时制得Li3SbO4微波介质相。
作为优选方式，步骤(2)进一步为：
(2.1)以纯度为99％的MgO、ZnO与上述步骤制备得到Li3SbO4微波介质相为原料，按照分子式Li3(Mg1-xZnx)2SbO6配制得到粉体，0.02≤x≤0.08；
(2.2)将上述步骤配制得到的粉体混合均匀，以纯水为分散剂、氧化锆球为球磨介质，其中氧化锆球的直径为3～15mm，按照原料：纯水：氧化锆球的重量比为1:2:1.5，采用湿磨法混合8小时，出料后在120℃下烘干，出料后烘干过80目筛，然后按照重量比加入6～10wt％的有机粘合剂进行造粒，过120目筛后压制成直径10～12mm、高5～6mm的圆柱状素坯，之后将素坯放入马弗炉内，在空气中于1325℃下烧结5小时即制得烧结微波介质陶瓷；
(2.3)将烧结好的Li3(Mg1-xZnx)2SbO6陶瓷两表面抛光制成成品待测。
为实现上述发明目的，本发明还提供一种易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料的制备方法，包括如下步骤：
(1.1)以纯度为99％的Li2CO3、Sb2O3为原料，按照Li3SbO4化学配比得到Li3SbO4粉体；
(1.2)将上述粉体混合均匀，以纯水为分散剂、氧化锆球为球磨介质，其中氧化锆球的直径为3～15mm，按照原料：纯水：氧化锆球的重量比为1:2:1.5，采用湿磨法混合8小时，出料后在120℃下烘干，过80目筛后以2℃/min的升温速率由室温升温至900℃保温4小时制得Li3SbO4微波介质相。
(2.1)以纯度为99％的MgO、ZnO与上述步骤制备得到Li3SbO4微波介质相为原料，按照分子式Li3(Mg1-xZnx)2SbO6配制得到粉体，0.02≤x≤0.08；
(2.2)将上述步骤配制得到的粉体混合均匀，以纯水为分散剂、氧化锆球为球磨介质，其中氧化锆球的直径为3～15mm，按照原料：纯水：氧化锆球的重量比为1:2:1.5，采用湿磨法混合8小时，出料后在120℃下烘干，出料后烘干过80目筛，然后按照重量比加入6～10wt％的有机粘合剂进行造粒，过120目筛后压制成直径10～12mm、高5～6mm的圆柱状素坯，之后将素坯放入马弗炉内，在空气中于1325℃下烧结5小时即制得烧结微波介质陶瓷；
(2.3)将烧结好的Li3(Mg1-xZnx)2SbO6陶瓷两表面抛光制成成品待测。
本发明中所涉及的微波介电性能测试采用Hakki and Coleman提出的介质谐振腔法测试圆柱体谐振频率下的介电常数与微波介电性能[Ref:B.W.Hakki,P.D.Coleman,"Dielectric Resonator Method of Measuring Inductive Capacities in theMillimeter Range",IEEE Trans.Microw.Theory Technol.,Mtt-8,402(1970)]。
本发明的有益效果为：本发明提供的易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料能够很好的满足当前移动通信技术领域对使用环境日趋严苛的要求，不仅易于制备，还具有高品质因数以及稳定的温度特性。该微波介质陶瓷体系适合用作微波谐振器、滤波器、天线及相关电子线路基板材料。
附图说明
图1是本发明实施例1～4在1325℃下烧结制得的陶瓷材料XRD图谱；
图2是本发明实施例1～4在1325℃下烧结制得的陶瓷材料表面SEM照片(图(a)～图(d)分别对应实施例1～4)；
图3是本发明实施例1～4在1325℃下烧结制得的陶瓷材料微波介电性能附图(含介电常数、品质因数、谐振频率温度系数)。
具体实施方式
以下通过特定的具体实例说明本发明的实施方式，本领域技术人员可由本说明书所揭露的内容轻易地了解本发明的其他优点与功效。本发明还可以通过另外不同的具体实施方式加以实施或应用，本说明书中的各项细节也可以基于不同观点与应用，在没有背离本发明的精神下进行各种修饰或改变。
实施例1
本实施例提供一种易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料，该陶瓷材料的化学式为Li3(Mg0.98Zn0.02)2SbO6(Li3(Mg1-xZnx)2SbO6，x＝0.02)。
制备方法包括如下步骤：
(1.1)以纯度为99％的Li2CO3、Sb2O3为原料，按照Li3SbO4化学配比得到Li3SbO4粉体；
(1.2)将上述粉体混合均匀，以纯水为分散剂、氧化锆球为球磨介质，其中氧化锆球的直径为3～15mm，按照原料：纯水：氧化锆球的重量比为1:2:1.5，采用湿磨法混合8小时，出料后在120℃下烘干，过80目筛后以2℃/min的升温速率由室温升温至900℃保温4小时制得Li3SbO4微波介质相。
(2.1)以纯度为99％的MgO、ZnO与上述步骤制备得到Li3SbO4微波介质相为原料，按照分子式Li3(Mg0.98Zn0.02)2SbO6配制得到粉体；
(2.2)将上述步骤配制得到的粉体混合均匀，以纯水为分散剂、氧化锆球为球磨介质，其中氧化锆球的直径为3～15mm，按照原料：纯水：氧化锆球的重量比为1:2:1.5，采用湿磨法混合8小时，出料后在120℃下烘干，出料后烘干过80目筛，然后按照重量比加入6～10wt％的有机粘合剂进行造粒，过120目筛后压制成直径10～12mm、高5～6mm的圆柱状素坯，之后将素坯放入马弗炉内，在空气中于1325℃下烧结5小时即制得烧结微波介质陶瓷；
(2.3)将烧结好的Li3(Mg0.98Zn0.02)2SbO6陶瓷两表面抛光制成成品待测；
(2.4)利用阿基米德排水法获得材料的实测表观密度；
(2.5)利用Miniflex X射线衍射仪获得材料的物相结构信息；
(2.6)利用JEOL JSM-6490SEM获得材料的表观形貌。
本实施例中所涉及的微波介电性能测试采用Hakki and Coleman提出的介质谐振腔法测试圆柱体谐振频率下的介电常数与微波介电性能，采用美国Agilent N5230A网络分析仪测试得到；
1325℃下烧结的Li3(Mg0.98Zn0.02)2SbO6陶瓷其微波介电性能测试结果如下：谐振频率13.512GHz，介电常数8.5，品质因数82400GHz，谐振频率温度系数-14ppm/℃，结果见附图3。
实施例2
本实施例提供一种易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料，该陶瓷材料的化学式为Li3(Mg0.96Zn0.04)2SbO6(Li3(Mg1-xZnx)2SbO6，x＝0.04)。
制备方法包括如下步骤：
(1.1)以纯度为99％的Li2CO3、Sb2O3为原料，按照Li3SbO4化学配比得到Li3SbO4粉体；
(1.2)将上述粉体混合均匀，以纯水为分散剂、氧化锆球为球磨介质，其中氧化锆球的直径为3～15mm，按照原料：纯水：氧化锆球的重量比为1:2:1.5，采用湿磨法混合8小时，出料后在120℃下烘干，过80目筛后以2℃/min的升温速率由室温升温至900℃保温4小时制得Li3SbO4微波介质相。
(2.1)以纯度为99％的MgO、ZnO与上述步骤制备得到Li3SbO4微波介质相为原料，按照分子式Li3(Mg0.96Zn0.04)2SbO6配制得到粉体；
(2.2)将上述步骤配制得到的粉体混合均匀，以纯水为分散剂、氧化锆球为球磨介质，其中氧化锆球的直径为3～15mm，按照原料：纯水：氧化锆球的重量比为1:2:1.5，采用湿磨法混合8小时，出料后在120℃下烘干，出料后烘干过80目筛，然后按照重量比加入6～10wt％的有机粘合剂进行造粒，过120目筛后压制成直径10～12mm、高5～6mm的圆柱状素坯，之后将素坯放入马弗炉内，在空气中于1325℃下烧结5小时即制得烧结微波介质陶瓷；
(2.3)将烧结好的Li3(Mg0.96Zn0.04)2SbO6的陶瓷两表面抛光制成成品待测；
(2.4)利用阿基米德排水法获得材料的实测表观密度；
(2.5)利用Miniflex X射线衍射仪获得材料的物相结构信息；
(2.6)利用JEOL JSM-6490SEM获得材料的表观形貌。
本实施例中所涉及的微波介电性能测试采用Hakki and Coleman提出的介质谐振腔法测试圆柱体谐振频率下的介电常数与微波介电性能，采用美国Agilent N5230A网络分析仪测试得到；
1325℃下烧结的Li3(Mg0.96Zn0.04)2SbO6陶瓷其微波介电性能测试结果如下：谐振频率13.705GHz，介电常数8.2，品质因数97719GHz，谐振频率温度系数-7ppm/℃，结果见附图3。
实施例3
本实施例提供一种易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料，该陶瓷材料的化学式为Li3(Mg0.94Zn0.06)2SbO6(Li3(Mg1-xZnx)2SbO6，x＝0.06)。
制备方法包括如下步骤：
(1.1)以纯度为99％的Li2CO3、Sb2O3为原料，按照Li3SbO4化学配比得到Li3SbO4粉体；
(1.2)将上述粉体混合均匀，以纯水为分散剂、氧化锆球为球磨介质，其中氧化锆球的直径为3～15mm，按照原料：纯水：氧化锆球的重量比为1:2:1.5，采用湿磨法混合8小时，出料后在120℃下烘干，过80目筛后以2℃/min的升温速率由室温升温至900℃保温4小时制得Li3SbO4微波介质相。
(2.1)以纯度为99％的MgO、ZnO与上述步骤制备得到Li3SbO4微波介质相为原料，按照分子式Li3(Mg0.98Zn0.06)2SbO6配制得到粉体；
(2.2)将上述步骤配制得到的粉体混合均匀，以纯水为分散剂、氧化锆球为球磨介质，其中氧化锆球的直径为3～15mm，按照原料：纯水：氧化锆球的重量比为1:2:1.5，采用湿磨法混合8小时，出料后在120℃下烘干，出料后烘干过80目筛，然后按照重量比加入6～10wt％的有机粘合剂PVA进行造粒，过120目筛后压制成直径10～12mm、高5～6mm的圆柱状素坯，之后将素坯放入马弗炉内，在空气中于1325℃下烧结5小时即制得烧结微波介质陶瓷；
(2.3)将烧结好的Li3(Mg0.94Zn0.06)2SbO6陶瓷两表面抛光制成成品待测；
(2.4)利用阿基米德排水法获得材料的实测表观密度；
(2.5)利用Miniflex X射线衍射仪获得材料的物相结构信息；
(2.6)利用JEOL JSM-6490SEM获得材料的表观形貌。
本实施例中所涉及的微波介电性能测试采用Hakki and Coleman提出的介质谐振腔法测试圆柱体谐振频率下的介电常数与微波介电性能，采用美国Agilent N5230A网络分析仪测试得到；
1325℃下烧结的Li3(Mg0.94Zn0.06)2SbO6陶瓷其微波介电性能测试结果如下：谐振频率13.495GHz，介电常数7.7，品质因数53095GHz，谐振频率温度系数-4ppm/℃，结果见附图3。
实施例4
本实施例提供一种易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料，该陶瓷材料的化学式为Li3(Mg0.92Zn0.08)2SbO6(Li3(Mg1-xZnx)2SbO6，x＝0.08)。
制备方法包括如下步骤：
(1.1)以纯度为99％的Li2CO3、Sb2O3为原料，按照Li3SbO4化学配比得到Li3SbO4粉体；
(1.2)将上述粉体混合均匀，以纯水为分散剂、氧化锆球为球磨介质，其中氧化锆球的直径为3～15mm，按照原料：纯水：氧化锆球的重量比为1:2:1.5，采用湿磨法混合8小时，出料后在120℃下烘干，过80目筛后以2℃/min的升温速率由室温升温至900℃保温4小时制得Li3SbO4微波介质相。
(2.1)以纯度为99％的MgO、ZnO与上述步骤制备得到Li3SbO4微波介质相为原料，按照分子式Li3(Mg0.92Zn0.08)2SbO6配制得到粉体；
(2.2)将上述步骤配制得到的粉体混合均匀，以纯水为分散剂、氧化锆球为球磨介质，其中氧化锆球的直径为3～15mm，按照原料：纯水：氧化锆球的重量比为1:2:1.5，采用湿磨法混合8小时，出料后在120℃下烘干，出料后烘干过80目筛，然后按照重量比加入6～10wt％的有机粘合剂PVA进行造粒，过120目筛后压制成直径10～12mm、高5～6mm的圆柱状素坯，之后将素坯放入马弗炉内，在空气中于1325℃下烧结5小时即制得烧结微波介质陶瓷；
(2.3)将烧结好的Li3(Mg0.92Zn0.08)2SbO6陶瓷两表面抛光制成成品待测；
(2.4)利用阿基米德排水法获得材料的实测表观密度；
(2.5)利用Miniflex X射线衍射仪获得材料的物相结构信息；
(2.6)利用JEOL JSM-6490SEM获得材料的表观形貌。
本实施例中所涉及的微波介电性能测试采用Hakki and Coleman提出的介质谐振腔法测试圆柱体谐振频率下的介电常数与微波介电性能，采用美国Agilent N5230A网络分析仪测试得到；
1325℃下烧结的Li3(Mg0.92Zn0.08)2SbO6陶瓷其微波介电性能测试结果如下：谐振频率13.850GHz，介电常数7.2，品质因数51844GHz，谐振频率温度系数-1ppm/℃，结果见附图3。
上述的4个具体实施例中，实施例2中制备的Li3(Mg0.96Zn0.04)2SbO6陶瓷品质因数最大，为97719GHz，表明其信号传输时的能量损耗最低；介电常数为8.2；谐振频率温度系数为-7ppm/℃。实施例4中制备的Li3(Mg0.92Zn0.08)2SbO6陶瓷谐振频率温度系数最接近于零，为-1ppm/℃，表明其温度稳定性最好；介电常数为7.2；品质因数为51844GHz。在制备的4个实施例中，实施例2因其较高的品质因数Q，综合性能最优。
本发明包括但不限于以上实施例，凡符合本发明要求的实施方案均属于本发明的保护范围。
综上，本发明提供了一种易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料及其制备方法。通过Zn对Li3Mg2SbO6陶瓷的改性，获得了具有品质因数高、介电常数小、温度稳定性较优异的一种高Q值微波介质陶瓷材料，为5G通信微波介质元器件的高频化应用提供了一种有效解决方案。
上述实施例仅例示性说明本发明的原理及其功效，而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下，对上述实施例进行修饰或改变。因此，凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变，仍应由本发明的权利要求所涵盖。

Claims (5)

1.一种易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料，其特征在于该陶瓷材料的化学式为Li3(Mg1-xZnx)2SbO6，其中0.02≤x≤0.08，制备方法采用固相反应法进行两步烧结：
(1)将Sb2O3、Li2CO3按照Li3SbO4化学配比混合球磨后烘干，预烧后获得Li3SbO4微波介质相；
(2)以MgO、ZnO和上述制备的Li3SbO4微波介质相，按照分子式Li3(Mg1-xZnx)2SbO6配制，其中0.02≤x≤0.08，进行混合球磨后烘干，然后加入粘合剂后造粒过筛并压制成圆柱状坯体，于空气中常压下烧结成瓷。
2.根据权利要求1所述的易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料，其特征在于：该微波介质陶瓷介电常数为7.2～8.5，品质因数为51844～97719GHz，谐振频率温度系数为-14～-1ppm/℃。
3.根据权利要求1所述的易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料，其特征在于步骤(1)进一步为：
(1.1)以纯度为99％的Li2CO3、Sb2O3为原料，按照Li3SbO4化学配比得到Li3SbO4粉体；
(1.2)将上述粉体混合均匀，以纯水为分散剂、氧化锆球为球磨介质，其中氧化锆球的直径为3～15mm，按照原料：纯水：氧化锆球的重量比为1:2:1.5，采用湿磨法混合8小时，出料后在120℃下烘干，过80目筛后以2℃/min的升温速率由室温升温至900℃保温4小时制得Li3SbO4微波介质相。
4.根据权利要求1所述的易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料，其特征在于步骤(2)进一步为：
(2.1)以纯度为99％的MgO、ZnO与上述步骤制备得到Li3SbO4微波介质相为原料，按照分子式Li3(Mg1-xZnx)2SbO6配制得到粉体，0.02≤x≤0.08；
(2.2)将上述步骤配制得到的粉体混合均匀，以纯水为分散剂、氧化锆球为球磨介质，其中氧化锆球的直径为3～15mm，按照原料：纯水：氧化锆球的重量比为1:2:1.5，采用湿磨法混合8小时，出料后在120℃下烘干，出料后烘干过80目筛，然后按照重量比加入6～10wt％的有机粘合剂进行造粒，过120目筛后压制成直径10～12mm、高5～6mm的圆柱状素坯，之后将素坯放入马弗炉内，在空气中于1325℃下烧结5小时即制得烧结微波介质陶瓷；
(2.3)将烧结好的Li3(Mg1-xZnx)2SbO6陶瓷两表面抛光制成成品待测。
5.一种易烧结高Q值Li3Mg2SbO6基微波介质陶瓷材料的制备方法，其特征在于包括如下步骤：
(1.1)以纯度为99％的Li2CO3、Sb2O3为原料，按照Li3SbO4化学配比得到Li3SbO4粉体；
(1.2)将上述粉体混合均匀，以纯水为分散剂、氧化锆球为球磨介质，其中氧化锆球的直径为3～15mm，按照原料：纯水：氧化锆球的重量比为1:2:1.5，采用湿磨法混合8小时，出料后在120℃下烘干，过80目筛后以2℃/min的升温速率由室温升温至900℃保温4小时制得Li3SbO4微波介质相；
(2.1)以纯度为99％的MgO、ZnO与上述步骤制备得到Li3SbO4微波介质相为原料，按照分子式Li3(Mg1-xZnx)2SbO6配制得到粉体，0.02≤x≤0.08；
(2.2)将上述步骤配制得到的粉体混合均匀，以纯水为分散剂、氧化锆球为球磨介质，其中氧化锆球的直径为3～15mm，按照原料：纯水：氧化锆球的重量比为1:2:1.5，采用湿磨法混合8小时，出料后在120℃下烘干，出料后烘干过80目筛，然后按照重量比加入6～10wt％的有机粘合剂进行造粒，过120目筛后压制成直径10～12mm、高5～6mm的圆柱状素坯，之后将素坯放入马弗炉内，在空气中于1325℃下烧结5小时即制得烧结微波介质陶瓷；
(2.3)将烧结好的Li3(Mg1-xZnx)2SbO6陶瓷两表面抛光制成成品待测。
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