CN112174665B - 5g基站用介电常数精准可控的滤波器陶瓷及其制备方法 - Google Patents
5g基站用介电常数精准可控的滤波器陶瓷及其制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 39
- 239000013078 crystal Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 5
- 229910009116 xCuO Inorganic materials 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 18
- 235000012431 wafers Nutrition 0.000 claims description 18
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- 230000001276 controlling effect Effects 0.000 abstract 1
- 229910000431 copper oxide Inorganic materials 0.000 abstract 1
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Abstract
本发明涉及一种5G基站用介电常数精准可控的滤波器陶瓷及其制备方法，由主晶相和烧结助剂烧结而成；主晶相化学式和烧结助剂的组成：0.75Mg0.3Ba0.7TiO3‑0.25LaAlO3+xCuO+yZnO，其中0＜x≤1wt％，1≤y≤3wt％。本发明通过调控氧化锌、氧化铜的配比，实现5G基站用滤波器陶瓷烧结温度降低到1300～1350℃、品质因素Q×f＝40000～50000GHz的同时，陶瓷的介电常数在40～45范围内精准可调控、εr误差范围小于±0.2，适用于5G基站用陶瓷滤波器对于介电常数序列化、精准化的需求。
Description
技术领域
本发明涉及一种5G基站用介电常数精准可控的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时代的来临，5G基站向着小型化、轻量化和高集成化发展。因此，对5G基站用陶瓷滤波器提出了更高的要求。国家大力支持5G网络商业化，发改办高技[2020]530号出台了关于加快5G网络规模部署和商业应用，推进重点区域5G基站和配套网络建设的文件。国内5G基站滤波器需求超10亿只，且未来5年市场规模将达370亿元，那么就需要更多高品质、高性能的滤波器陶瓷来满足市场的需要。
面对滤波器在2.40～2.70GHz和3.4～3.6GHz的不同频段，对滤波器陶瓷的介电常数提出跟高要求，希望每个波段对应一个确切的滤波器陶瓷的介电常数(误差在±0.1)。那么对于同种基质的滤波器陶瓷，在规定范围内的中介电常数(40～45)的精确控制的研究迫在眉睫。杨秀玲等在《MgTiO3-CaTiO3基微波介质陶瓷材料介电性能的研究》通过掺杂Cu、Co、V、Cu-Al等离子得到介电常数为20、21、22、25等序列的陶瓷，误差为±0.3。面对5G基站用的滤波器陶瓷，该误差范围太大，造成滤波器性能不稳定。
发明内容
本发明提供一种5G基站用范围内可控介电常数滤波器陶瓷的制备方法，其特点在于可以通过双元助剂量的搭配在低误差±0.1范围内制备介电常数为40、41、42、43、44、45等序列的滤波器陶瓷，Q×f：40000～50000GHz，τf：-3～4ppm/℃。
具体技术方案为：
5G基站用介电常数精准可控的滤波器陶瓷，由主晶相和烧结助剂烧结而成；主晶相化学式和烧结助剂的组成：0.75Mg0.3Ba0.7TiO3-0.25LaAlO3+xCuO+yZnO，其中0＜x≤1wt％，1≤y≤3wt％。
该5G基站用介电常数精准可控的滤波器陶瓷的制备方法，包括以下步骤：
(1)将原料按化学式0.75Mg0.3Ba0.7TiO3-0.25LaAlO3进行配料；
(2)将配好的原料放入卧式球磨机中，其中原料粉体、氧化锆球、去离子水重量比为1：4：1.5，以400r/min球磨5-8小时，过40目筛；
(3)将混合均匀的原料预烧得到主晶相0.75Mg0.3Ba0.7TiO3-0.25LaAlO3；
(4)将步骤(3)得到的主晶相用气流粉碎机破碎，按比例加入烧结助剂xCuO+yZnO和去离子水继续球磨6h，然后在空气气氛下80℃烘干5h；其中，0＜x≤1wt％，1≤y≤3wt％；
(5)加入粘结剂造粒，压制成小圆片；
(6)将步骤(5)所得小圆片在高温烧结炉预烧，即可得到滤波器陶瓷。
其中，步骤(1)中所述的原料为MgO、TiO2、BaO、La2O3、Al2O3。
步骤(3)所述预烧的条件为：将混合均匀的原料用高温烧结炉在空气气氛下800℃预烧3h，升温速率为5℃/min。
步骤(5)中所述的粘结剂为聚乙烯醇，加入量为总物料的3～5wt％，在7MPa下压制成直径18mm、高3～5mm的小圆片。
步骤(6)烧结的条件为：以5℃/min升到600℃，空气气氛中预烧2h排胶，再10℃/min升温到1300℃保温2小时，随炉冷却。
采用上述方法所得到的微波介电陶瓷，先通过预烧形成主晶0.75Mg0.3Ba0.7TiO3-0.25LaAlO3，主晶相介电常数在38～44，相通过在0＜x≤1wt％，1≤y≤3wt％范围内调控CuO：ZnO的比值，在误差±0.1范围内，精确得到40、41、42、43、44、45序列的介电常数，除此之外，还能得到较高的Q×f：40000～50000GHz，趋近零的温漂。能够满足5G滤波器对于不同频段要求的在40～45中的确切的介电常数值。
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：MgO、TiO2、BaO、La2O3、Al2O3分别称取：12.12g、107.11g、80.02g、162.96g、101.96g；
步骤二：将配好的料放入卧式球磨机中，其中粉体、氧化锆球、去离子水重量比为1：4：1.5，以400r/min球磨5-8小时；
步骤三：将混合均匀的原料用高温烧结炉在空气气氛以5℃/min升温到800℃预烧3h得到主晶相0.75Mg0.3Ba0.7TiO3-0.25LaAlO3；
步骤四：将上一步得到的主晶相用气流粉碎机破碎，按比例加入烧结助剂10.341gCuO、85.449gZnO和去离子水990g继续球磨6h，然后在空气气氛下80℃烘干5h；
步骤五：加入3wt％聚乙烯醇粘结剂造粒，在8Mpa压力下，压制成直径为18mm，高度为4mm小圆片；
步骤六：将步骤五所得小圆片在高温烧结炉中以5℃/min升到600℃，空气气氛中预烧2h排胶，再10℃/min升温到1300℃保温2小时，随炉冷却，即可得到所述的5G基站用介电常数可控的滤波器陶瓷，介电性能如表1。
实施例2
步骤一：MgO、TiO2、BaO、La2O3、Al2O3分别称取：12.11g、107.12g、80.04g、162.95g、101.94g；
步骤二：将配好的料放入卧式球磨机中，其中粉体、氧化锆球、去离子水重量比为1：4：1.5，以400r/min球磨5-8小时；
步骤三：将混合均匀的原料用高温烧结炉在空气气氛以5℃/min升温到800℃预烧3h得到主晶相0.75Mg0.3Ba0.7TiO3-0.25LaAlO3。
步骤四：将上一步得到的主晶相用气流粉碎机破碎，按比例加入烧结助剂22.274gCuO、108.235gZnO和去离子水1020g继续球磨6h，然后在空气气氛下80℃烘干5h；
步骤五：加入3wt％聚乙烯醇粘结剂造粒，在8Mpa压力下，压制成直径为18mm，高度为4mm小圆片；
步骤六：将步骤五所得小圆片在高温烧结炉中以5℃/min升到600℃，空气气氛中预烧2h排胶，再10℃/min升温到1300℃保温2小时，随炉冷却，即可得到所述的5G基站用介电常数可控的滤波器陶瓷，介电性能如表1。
实施例3
步骤一：MgO、TiO2、BaO、La2O3、Al2O3分别称取：12.11g、107.15g、80.04g、162.93g、101.91g；
步骤二：将配好的料放入卧式球磨机中，其中粉体、氧化锆球、去离子水重量比为1：4：1.5，以400r/min球磨5-8小时；
步骤三：将混合均匀的原料用高温烧结炉在空气气氛以5℃/min升温到800℃预烧3h得到主晶相0.75Mg0.3Ba0.7TiO3-0.25LaAlO3。
步骤四：将上一步得到的主晶相用气流粉碎机破碎，按比例加入烧结助剂32.615gCuO、115.559gZnO和去离子水1100g继续球磨6h，然后在空气气氛下80℃烘干5h；
步骤五：加入3wt％聚乙烯醇粘结剂造粒，在8Mpa压力下，压制成直径为18mm，高度为4mm小圆片；
步骤六：将步骤五所得小圆片在高温烧结炉中以5℃/min升到600℃，空气气氛中预烧2h排胶，再10℃/min升温到1300℃保温2小时，随炉冷却，即可得到所述的5G基站用介电常数可控的滤波器陶瓷，介电性能如表1。
实施例4
步骤一：MgO、TiO2、BaO、La2O3、Al2O3分别称取：12.15g、107.13g、80.01g、162.92g、101.91g；
步骤二：将配好的料放入卧式球磨机中，其中粉体、氧化锆球、去离子水重量比为1：4：1.5，以400r/min球磨5-8小时；
步骤三：将混合均匀的原料用高温烧结炉在空气气氛以5℃/min升温到800℃预烧3h得到主晶相0.75Mg0.3Ba0.7TiO3-0.25LaAlO3。
步骤四：将上一步得到的主晶相用气流粉碎机破碎，按比例加入烧结助剂40.570gCuO、120.442gZnO和去离子水1120g继续球磨6h，然后在空气气氛下80℃烘干5h；
步骤五：加入3wt％聚乙烯醇粘结剂造粒，在8Mpa压力下，压制成直径为18mm，高度为4mm小圆片；
步骤六：将步骤五所得小圆片在高温烧结炉中以5℃/min升到600℃，空气气氛中预烧2h排胶，再10℃/min升温到1300℃保温2小时，随炉冷却，即可得到所述的5G基站用介电常数可控的滤波器陶瓷，介电性能如表1。
实施例5
步骤一：MgO、TiO2、BaO、La2O3、Al2O3分别称取：12.12g、107.10g、80.02g、162.96g、101.95g；
步骤二：将配好的料放入卧式球磨机中，其中粉体、氧化锆球、去离子水重量比为1：4：1.5，以400r/min球磨5-8小时；
步骤三：将混合均匀的原料用高温烧结炉在空气气氛以5℃/min升温到800℃预烧3h得到主晶相0.75Mg0.3Ba0.7TiO3-0.25LaAlO3。
步骤四：将上一步得到的主晶相用气流粉碎机破碎，按比例加入烧结助剂43.752gCuO、140.787ZnO和去离子水1150g继续球磨6h，然后在空气气氛下80℃烘干5h；
步骤五：加入3wt％聚乙烯醇粘结剂造粒，在8Mpa压力下，压制成直径为18mm，高度为4mm小圆片；
步骤六：将步骤五所得小圆片在高温烧结炉中以5℃/min升到600℃，空气气氛中预烧2h排胶，再10℃/min升温到1300℃保温2小时，随炉冷却，即可得到所述的5G基站用介电常数可控的滤波器陶瓷，介电性能如表1。
实施例6
步骤一：MgO、TiO2、BaO、La2O3、Al2O3分别称取：12.14g、107.12g、80.03g、162.92g、101.96g；
步骤二：将配好的料放入卧式球磨机中，其中粉体、氧化锆球、去离子水重量比为1：4：1.5，以400r/min球磨5-8小时；
步骤三：将混合均匀的原料用高温烧结炉在空气气氛以5℃/min升温到800℃预烧3h得到主晶相0.75Mg0.3Ba0.7TiO3-0.25LaAlO3。
步骤四：将上一步得到的主晶相用气流粉碎机破碎，按比例加入烧结助剂62.049gCuO、116.373gZnO和去离子水1000g继续球磨6h，然后在空气气氛下80℃烘干5h；
步骤五：加入3wt％聚乙烯醇粘结剂造粒，在8Mpa压力下，压制成直径为18mm，高度为4mm小圆片；
步骤六：将步骤五所得小圆片在高温烧结炉中以5℃/min升到600℃，空气气氛中预烧2h排胶，再10℃/min升温到1300℃保温2小时，随炉冷却，即可得到所述的5G基站用介电常数可控的滤波器陶瓷，介电性能如表1。
表1：滤波器陶瓷性能
如表1所示，随着CuO、ZnO掺杂量的改变，介电常数可以实现序列化(40、41、42、43、44)、且偏差范围始终控制在±0.1。当x＝0.41，y＝1.42时，得到0.75Mg0.3Ba0.7TiO3-0.25LaAlO3陶瓷性能最好，介电常数εr为42.0，τf为1.43ppm/℃，Q×f为44563GHz。
Claims (6)
1.5G基站用介电常数精准可控的滤波器陶瓷，其特征在于，由主晶相和烧结助剂烧结而成；主晶相化学式和烧结助剂的组成：0.75Mg0.3Ba0.7TiO3-0.25LaAlO3+xCuO+yZnO，其中0＜x≤1wt%，1≤y≤3wt%。
2. 5G基站用介电常数精准可控的滤波器陶瓷的制备方法，其特征在于，包括以下步骤：
（1）将原料按化学式0.75Mg0.3Ba0.7TiO3-0.25LaAlO3进行配料；
（2）将配好的原料放入卧式球磨机中，其中原料粉体、氧化锆球、去离子水重量比为1：4：1.5，以400r/min球磨5-8小时，过40目筛；
（3）将混合均匀的原料预烧得到主晶相0.75Mg0.3Ba0.7TiO3-0.25LaAlO3；
（4）将步骤（3）得到的主晶相用气流粉碎机破碎，按比例加入烧结助剂xCuO+yZnO和去离子水继续球磨6h，然后在空气气氛下80℃烘干5h；其中，0＜x≤1wt%，1≤y≤3wt%；
（5）加入粘结剂造粒，压制成小圆片；
（6）将步骤（5）所得小圆片在高温烧结炉中烧结，即可得到滤波器陶瓷。
3.根据权利要求2所述的5G基站用介电常数精准可控的滤波器陶瓷的制备方法，其特征在于：步骤（1）中所述的原料为MgO、TiO2、BaO、La2O3、Al2O3。
4.根据权利要求2所述的5G基站用介电常数精准可控的滤波器陶瓷的制备方法，其特征在于：步骤（3）所述预烧的条件为：将混合均匀的原料用高温烧结炉在空气气氛下800℃预烧3h，升温速率为5℃/min。
5.根据权利要求2所述的5G基站用介电常数精准可控的滤波器陶瓷的制备方法，其特征在于：步骤（5）中所述的粘结剂为聚乙烯醇，加入量为总物料的3~5wt%，在7MPa下压制成直径18mm、高3~5mm的小圆片。
6.根据权利要求2所述的5G基站用介电常数精准可控的滤波器陶瓷的制备方法，其特征在于：步骤（6）烧结的条件为：以5℃/min升到600℃，空气气氛中预烧2h排胶，再10℃/min升温到1300℃保温2小时，随炉冷却。
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