CN112142465A - 稀土离子改性的5g基站用滤波器陶瓷及其制备方法 - Google Patents

稀土离子改性的5g基站用滤波器陶瓷及其制备方法 Download PDF

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CN112142465A
CN112142465A CN202011022154.2A CN202011022154A CN112142465A CN 112142465 A CN112142465 A CN 112142465A CN 202011022154 A CN202011022154 A CN 202011022154A CN 112142465 A CN112142465 A CN 112142465A
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李春宏
钟云
康晓丽
崔旭东
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Abstract

本发明涉及一种稀土离子改性的5G基站用滤波器陶瓷的制备方法，其化学式组成为0.6CaTiO3‑0.4ZnTaNb2O6，通过添加稀土氧化物和氧化锂组合的多元烧结助剂xRe2O3+yLi2O，1<x<2wt％,1<y<3wt％,Re为Y、Eu、Dy、La、Pr中的一种或两种；使陶瓷基质改性，获得更高的Q×f：80000～90000GHz，稳定的介电常数εr：21～23，趋近于零的τf：‑2～0ppm/℃，使其适用于5G基站用滤波器陶瓷。

Description

稀土离子改性的5G基站用滤波器陶瓷及其制备方法
技术领域
本发明涉及一种稀土离子改性的5G基站用滤波器陶瓷及其制备方法，属于微波介质陶瓷领域。
背景技术
随着5G时代的快速发展，滤波器作为射频器件重要的组成部分，承担了帮助基站选频的重任。滤波器的主要功能是对发送和接受的信号进行滤波，可以剔除不要频段的信号，从而保证接受和发送信号的准确度。因此滤波器陶瓷需要合适的介电常数，高的品质因数使滤波器的插损更低，趋近于0的谐振频率温度系数使滤波器获得更高的稳定性。
面对5G滤波器陶瓷要求的高品质因数、低温漂，作为新型低温烧结微波介质陶瓷，不仅要有适用于5G基站用的介电常数，更高的Q×f值，低的介电损耗与小的谐振频率温度系数。目前多数的研究是往陶瓷基体材料中添加一定量的金属氧化物或者玻璃类助剂，但是这些微波介质陶瓷的介电性能变差，温度频率谐振系数也变大。王丹等人在电子元件与材料2014年第6期发表《氧化钛添加对ZnNb2O6陶瓷谐振频率温度系数的影响》添加1.5wt％TiO2作烧结助剂在1150℃获得最佳性能，εr＝46.2，Q×f＝48000GHz，τf：-8ppm/℃，但是其品质因数还不够高，温漂也较大。
发明内容
针对上述技术问题，本发明提供一种稀土离子改性的5G基站用滤波器陶瓷的制备方法，优点在于通过稀土离子和氧化锂的掺杂，使得陶瓷获得更优异的介电性能。
具体技术方案为：
本发明提供的稀土离子改性的5G基站用滤波器陶瓷，由主晶相和烧结助剂烧结而成；主晶相化学式：0.6CaTiO3-0.4Zn0.4Ta0.6Nb2O6；
烧结助剂组成：xRe2O3+yLi2O，1<x<2wt％,1<y<3wt％，Re为Y、Eu、Dy、La中的一种或两种。
该稀土离子改性的5G基站用滤波器陶瓷的制备方法，包括以下步骤：
(1)将原料按所述化学式0.6CaTiO3-0.4Zn0.4Ta0.6Nb2O6计量比精确称量；
(2)将精确称量好的原料放入卧式球磨机中以350r/min球磨6～8小时，其中原料粉体、氧化锆球、去离子水重量比为1：3.5：1.5；
(3)将混合均匀的原料在预烧得到主晶相0.6CaTiO3-0.4Zn0.4Ta0.6Nb2O6；
(4)将步骤(3)得到的块状主晶相用气流粉碎机破碎，按比例加入烧结助剂xRe2O3+yLi2O和去离子水继续球磨6h；其中1<x<2wt％,1<y<3wt％，Re为Y、Eu、Dy、La中的一种或两种；
(5)步骤(4)的混合物在空气气氛下60℃烘干4h，然后将混合物过40目筛得到均匀细腻的粉体；
(6)加入粘结剂造粒，压制成厚度为6mm、直径为13mm的小圆片；
(7)将步骤(6)所得小圆片在高温烧结炉中烧结，得到滤波器陶瓷。
进一步的，步骤(1)所述的原料为CaO、TiO2、Ta2O5、ZnO、NbO2。
步骤(3)预烧的条件为：在高温烧结炉空气气氛下，以8℃/min升温到800℃预烧2.5h。
步骤(6)所述的粘结剂为聚乙烯醇，加入量为总物料的5wt％。
步骤(7)中的烧结条件为：以3℃/min升到500℃，空气气氛中预烧2h排胶，再以5℃/min升温到1150～1250℃保温3小时，以5℃/min降温600℃，随炉冷却。
采用上述方法所得到的微波介电陶瓷，介电常数(εr)为21～23，Q*f值(Q为品质因素)80000～90000GHz，以及较小的谐振频率系数:τf：-2～0ppm/℃。该制备方工艺简单、烧结温度较低，并且可以使陶瓷致密化烧结，同时拥有优异的介电性能，能够适应5G滤波器的要求，是一种新型的5G滤波器陶瓷。
具体实施方式
结合实施例说明本发明的具体技术方案。
实施例1
步骤一：精确称量CaO、TiO2、Ta2O5、ZnO、NbO2分别为，33.6g、47.9g、106g、13g、100g；
步骤二：将精确称量好的原料放入卧式球磨机中以350r/min球磨6小时，其中氧化锆球、去离子水重量分别为，1050g、450g。
步骤三：将混合均匀的原料在高温烧结炉空气气氛下以8℃/min升温到800℃预烧2.5h得到主晶相0.6CaTiO3-0.4Zn0.4Ta0.6Nb2O6。
步骤四：将上一步得到的块状主晶相用气流粉碎机破碎，按比例加入烧结助剂3.6gLa2O3，3.6gLi2O和去离子水460g继续球磨6h；
步骤五：在空气气氛下60℃烘干4h，然后将粉体过40目筛得到均匀细腻的粉体；
步骤六：加入5wt％聚乙烯醇(PVA)粘结剂造粒，压制成厚度为6mm、直径为13mm的小圆片；
步骤七：将步骤6所得小圆片在高温烧结炉中以3℃/min升到500℃，空气气氛中预烧2h排胶，再以5℃/min升温到1150℃保温3小时，以5℃/min降温600℃，随炉冷却，得到滤波器陶瓷，性能如表1。
实施例2
步骤一：精确称量CaO、TiO2、Ta2O5、ZnO、NbO2分别为33.3g、47.6g、106.2g、13.3g、100.1g；
步骤二：将精确称量好的原料放入卧式球磨机中以350r/min球磨6小时，其中氧化锆球、去离子水重量分别为，1050g、450g。
步骤三：将混合均匀的原料在高温烧结炉空气气氛下以8℃/min升温到800℃预烧2.5h得到主晶相0.6CaTiO3-0.4Zn0.4Ta0.6Nb2O6。
步骤四：将上一步得到的块状主晶相用气流粉碎机破碎，按比例加入烧结助剂1.8gLa2O3,1.8gY2O3，3.6gLi2O和去离子水460g继续球磨6h；
步骤五：在空气气氛下60℃烘干4h，然后将粉体过40目筛得到均匀细腻的粉体；
步骤六：加入5wt％聚乙烯醇(PVA)粘结剂造粒，压制成厚度为6mm、直径为13mm的小圆片；
步骤七：将步骤6所得小圆片在高温烧结炉中以3℃/min升到500℃，空气气氛中预烧2h排胶，再以5℃/min升温到1200℃保温3小时，以5℃/min降温600℃，随炉冷却，得到滤波器陶瓷，性能如表1。
实施例3
步骤一：精确称量CaO、TiO2、Ta2O5、ZnO、NbO2分别为33.3g、47.9g、106.2g、13.1g、100g；
步骤二：将精确称量好的原料放入卧式球磨机中以350r/min球磨6小时，其中氧化锆球、去离子水重量分别为，1050g、450g。
步骤三：将混合均匀的原料在高温烧结炉空气气氛下以8℃/min升温到800℃预烧2.5h得到主晶相0.6CaTiO3-0.4Zn0.4Ta0.6Nb2O6。
步骤四：将上一步得到的块状主晶相用气流粉碎机破碎，按比例加入烧结助剂4.57gLa2O3，1.52gEu2O3，6.04gLi2O和去离子水460g继续球磨6h；
步骤五：在空气气氛下60℃烘干4h，然后将粉体过40目筛得到均匀细腻的粉体；
步骤六：加入5wt％聚乙烯醇(PVA)粘结剂造粒，压制成厚度为6mm、直径为13mm的小圆片；
步骤七：将步骤6所得小圆片在高温烧结炉中以3℃/min升到500℃，空气气氛中预烧2h排胶，再以5℃/min升温到1200℃保温3小时，以5℃/min降温600℃，随炉冷却，得到滤波器陶瓷，性能如表1。
实施例4
步骤一：精确称量CaO、TiO2、Ta2O5、ZnO、NbO2分别为33.2g、47.6g、106.4g、13.2g、100g；
步骤二：将精确称量好的原料放入卧式球磨机中以350r/min球磨6小时，其中氧化锆球、去离子水重量分别为，1060g、460g。
步骤三：将混合均匀的原料在高温烧结炉空气气氛下以8℃/min升温到800℃预烧2.5h得到主晶相0.6CaTiO3-0.4Zn0.4Ta0.6Nb2O6。
步骤四：将上一步得到的块状主晶相用气流粉碎机破碎，按比例加入烧结助剂2.40gY2O3，2.43gEu2O3，6.06gLi2O和去离子水460g继续球磨6h；
步骤五：在空气气氛下60℃烘干4h，然后将粉体过40目筛得到均匀细腻的粉体；
步骤六：加入5wt％聚乙烯醇(PVA)粘结剂造粒，压制成厚度为6mm、直径为13mm的小圆片；
步骤七：将步骤6所得小圆片在高温烧结炉中以3℃/min升到500℃，空气气氛中预烧2h排胶，再以5℃/min升温到1200℃保温3小时，以5℃/min降温600℃，随炉冷却，得到滤波器陶瓷，性能如表1。
实施例5
步骤一：精确称量CaO、TiO2、Ta2O5、ZnO、NbO2分别为33.3g、47.5g、106.3g、13.2g、100g；
步骤二：将精确称量好的原料放入卧式球磨机中以350r/min球磨6小时，其中氧化锆球、去离子水重量分别为，1060g、460g。
步骤三：将混合均匀的原料在高温烧结炉空气气氛下以8℃/min升温到800℃预烧2.5h得到主晶相0.6CaTiO3-0.4Zn0.4Ta0.6Nb2O6。
步骤四：将上一步得到的块状主晶相用气流粉碎机破碎，按比例加入烧结助剂6.32gY2O3，6.04gLi2O和去离子水470g继续球磨6h；
步骤五：在空气气氛下60℃烘干4h，然后将粉体过40目筛得到均匀细腻的粉体；
步骤六：加入5wt％聚乙烯醇(PVA)粘结剂造粒，压制成厚度为6mm、直径为13mm的小圆片；
步骤七：将步骤6所得小圆片在高温烧结炉中以3℃/min升到500℃，空气气氛中预烧2h排胶，再以5℃/min升温到1250℃保温3小时，以5℃/min降温600℃，随炉冷却，得到滤波器陶瓷，性能如表1。
表1：滤波器陶瓷性能
Figure BDA0002701010860000051
通过稀土氧化物和氧化锂共掺0.6CaTiO3-0.4Zn0.4Ta0.6Nb2O6，能够大大提高品质因数，平均在82000GHz以上，谐振频率温度系数最高在-1.65ppm/℃，当掺杂1.5wt％La2O3+0.5wt％Eu2O3+2wt％Li2O获得最优性能，介电常数εr：22.32，Q×f：85012GHz，，趋τf：-0.96ppm/℃。

Claims (6)

1.稀土离子改性的5G基站用滤波器陶瓷，其特征在于，由主晶相和烧结助剂烧结而成；主晶相化学式：0.6CaTiO3-0.4Zn0.4Ta0.6Nb2O6；
烧结助剂组成：xRe2O3+yLi2O，1<x<2wt％,1<y<3wt％，Re为Y、Eu、Dy、La中的一种或两种。
2.稀土离子改性的5G基站用滤波器陶瓷的制备方法，其特征在于，包括以下步骤：
(1)将原料按所述化学式0.6CaTiO3-0.4Zn0.4Ta0.6Nb2O6计量比精确称量；
(2)将精确称量好的原料放入卧式球磨机中以350r/min球磨6～8小时，其中原料粉体、氧化锆球、去离子水重量比为1：3.5：1.5；
(3)将混合均匀的原料在预烧得到主晶相0.6CaTiO3-0.4Zn0.4Ta0.6Nb2O6；
(4)将步骤(3)得到的块状主晶相用气流粉碎机破碎，按比例加入烧结助剂xRe2O3+yLi2O和去离子水继续球磨6h；其中1<x<2wt％,1<y<3wt％，Re为Y、Eu、Dy、La中的一种或两种；
(5)步骤(4)的混合物在空气气氛下60℃烘干4h，然后将混合物过40目筛得到均匀细腻的粉体；
(6)加入粘结剂造粒，压制成厚度为6mm、直径为13mm的小圆片；
(7)将步骤(6)所得小圆片在高温烧结炉中烧结，得到滤波器陶瓷。
3.根据权利要求2所述的稀土离子改性的5G基站用滤波器陶瓷的制备方法，其特征在于，步骤(1)所述的原料为CaO、TiO2、Ta2O5、ZnO、NbO2。
4.根据权利要求2所述的稀土离子改性的5G基站用滤波器陶瓷的制备方法，其特征在于，步骤(3)预烧的条件为：在高温烧结炉空气气氛下，以8℃/min升温到800℃预烧2.5h。
5.根据权利要求2所述的稀土离子改性的5G基站用滤波器陶瓷的制备方法，其特征在于，步骤(6)所述的粘结剂为聚乙烯醇，加入量为总物料的5wt％。
6.根据权利要求2所述的稀土离子改性的5G基站用滤波器陶瓷的制备方法，其特征在于，步骤(7)中的烧结条件为：以3℃/min升到500℃，空气气氛中预烧2h排胶，再以5℃/min升温到1150～1250℃保温3小时，以5℃/min降温600℃，随炉冷却。
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