CN113354413A - 一种层状中高介电常数低损耗微波介质陶瓷及其制备方法 - Google Patents

一种层状中高介电常数低损耗微波介质陶瓷及其制备方法 Download PDF

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CN113354413A
CN113354413A CN202110759080.9A CN202110759080A CN113354413A CN 113354413 A CN113354413 A CN 113354413A CN 202110759080 A CN202110759080 A CN 202110759080A CN 113354413 A CN113354413 A CN 113354413A
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dielectric ceramic
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岳振星
郭蔚嘉
马志宇
骆宇
陈雨谷
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Tsinghua University
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Abstract

本发明公开了属于电子功能材料与器件技术领域的一种层状中高介电常数低损耗微波介质陶瓷及其制备方法。该陶瓷材料由A基片和B基片层状粘合而成，其中A基片由质量百分比为16％～17％的BaO、6.5％～45％的Sm2O3、8.5％～37％的Nd2O3、36％～40％的TiO2和0.0％～3.0％的Al2O3构成，B基片由质量百分比为21％～22％的CaO、29％～30％的Sm2O3、30％～50％的TiO2和0.0％～18％的Al2O3构成；这种微波介质陶瓷材料的介电常数为60～80，Q×f值为13000～22000GHz，谐振频率温度系数为‑5～+5ppm/℃。本发明制备的层状结构微波介质陶瓷材料的综合性能优于现有的中高介电常数微波介质陶瓷材料，制备方法避免了两种基片材料在高温下可能发生的化学反应，在介质谐振器、滤波器等微波器件制作领域有良好的应用前景。

Description

一种层状中高介电常数低损耗微波介质陶瓷及其制备方法
技术领域
本发明涉及电子功能材料与器件技术领域，尤其涉及一种层状中高介电常数低损耗微波介质陶瓷及其制备方法。
背景技术
微波通常指频率为300MHz～300GHz的电磁波，相对于普通的无线电波，其频率高、信息容量大，具有更快的数据传输速度，并且为移动通信提供了大量的可用带宽。但高频率下介质材料的损耗更大，移动通信向高频发展对材料和器件都提出了更高的要求。微波介质陶瓷具有较大的相对介电常数、较低的损耗和较好的温度稳定性，被认为是一种在移动通信领域具有广阔应用前景的材料。介质谐振器的小型化要求介质具有更高的介电常数，因此具有中高介电常数(>55)的微波介质陶瓷得到了研究者的广泛关注。
Ba6-3xLn8+2xTi18O54作为目前应用最为广泛的高介电常数微波介质陶瓷体系，其介电损耗已难以满足目前移动通信的需要。Ca1-xLn2x/3TiO3具有高介电常数(>100)和高Q×f值(>10000GHz)，但其谐振频率温度系数非常大(>100ppm/℃)，同样限制了其进一步应用。因此，需要开发新的材料体系和制备方法以获得性能更优的微波介质陶瓷体系。
发明内容
本发明的目的是提出一种层状中高介电常数低损耗微波介质陶瓷及其制备方法。
一种层状中高介电常数低损耗微波介质陶瓷，其特征在于，该陶瓷由A基片和B基片层状粘合而成；所述A基片由质量百分比为16％～17％的BaO、6.5％～45％的Sm2O3、8.5％～37％的Nd2O3、36％～40％的TiO2和0.0％～3.0％的Al2O3构成；所述B基片由质量百分比为21％～22％的CaO、29％～30％的Sm2O3、30％～50％的TiO2和0.0％～18％的Al2O3构成；所述微波介质陶瓷的介电常数为60～80，Q×f值为13000～22000GHz，谐振频率温度系数为-5～+5ppm/℃。
一种层状中高介电常数低损耗微波介质陶瓷的制备方法，其特征在于，包括以下步骤：
步骤1：按质量百分比称取A基片的原料粉体，加入无水乙醇行星球磨混合，干燥后过60目筛并进行预烧；将预烧后的粉体再次行星球磨，干燥后再过60目筛，加入聚乙烯醇水溶液，造粒并干压成圆柱状；对生坯进行排胶处理和烧结，得到A基片；
步骤2：按质量百分比称取B基片的原料粉体，加入无水乙醇行星球磨混合，干燥后过60目筛并进行预烧；将预烧后的粉体再次行星球磨，干燥后再过60目筛，加入聚乙烯醇水溶液，造粒并干压成圆柱状；对生坯进行排胶处理和烧结，得到B基片；
步骤3：将烧结后的A基片与B基片的两底面打磨、抛光，采用堆叠方式同轴粘合。
所述步骤1中A基片预烧的温度范围为1100～1200℃，预烧时间为2～4小时；干压的压力范围为100～200兆帕且施加压力方式为轴向施压；排胶处理的温度为600℃，排胶时间为2～4小时；烧结的温度范围为1300～1450℃，烧结时间为2～8小时。
所述步骤2中B基片预烧的温度范围为1100～1300℃，预烧时间为2～4小时；干压的压力范围为100～200兆帕且施加压力方式为轴向施压；排胶处理的温度为600℃，排胶时间为2～4小时；烧结的温度范围为1300～1550℃，烧结时间为2～8小时。
所述步骤3中的堆叠方式为A基片在上、B基片在中、A基片在下，或B基片在上、A基片在中、B基片在下，或A基片在上、B基片在下。
本发明的有益效果在于：
本发明制备的层状结构微波介质陶瓷材料的介电常数为60～80，Q×f值为13000～22000GHz，谐振频率温度系数为-5～+5ppm/℃，综合性能优于现有的中高介电常数微波介质陶瓷材料；本发明采用的层状粘合的制备方法避免了两种基片材料在高温下可能发生的化学反应，制备工艺简单，在介质谐振器、滤波器等微波器件制作领域有良好的应用前景。
具体实施方式
本发明提出一种层状中高介电常数低损耗微波介质陶瓷及其制备方法，下面结合具体实施例对本发明做进一步说明。
实施例1
(1)按照质量分数16.7％BaO、44.2％Sm2O3、38.8％TiO2、0.3％Al2O3的配比，称量碳酸钡、氧化钐、二氧化钛(金红石相)、氧化铝，加入无水乙醇行星球磨混合，干燥后过60目筛，在1150℃下预烧4小时；将预烧后的粉体再次行星球磨，干燥后过60目筛，加入聚乙烯醇(PVA)水溶液，造粒并干压成型；对生坯在600℃进行4小时的排胶处理，而后在1350℃烧结4小时，得到A基片。
(2)按照质量分数21.1％CaO、29.2％Sm2O3、47.6％TiO2、2.1％Al2O3的配比，称量碳酸钙、氧化钐、二氧化钛(金红石相)、氧化铝，加入无水乙醇行星球磨混合，干燥后过60目筛，在1100℃下预烧3小时；将预烧后的粉体再次行星球磨，干燥后过60目筛，加入聚乙烯醇(PVA)水溶液，造粒并干压成型；对生坯在600℃进行4小时的排胶处理，而后在1300℃烧结4小时，得到B基片。
(3)将两种基片按照A基片在上、B基片在中、A基片在下的堆叠方式同轴粘合，自上到下每层的厚度占比为47.4％、5.2％、47.4％，得到微波介质陶瓷。
实施例2
(1)按照实施例1(1)(2)步骤分别得到A基片和B基片。
(2)将两种基片按照B基片在上、A基片在中、B基片在下的堆叠方式同轴粘合，自上到下每层的厚度占比为20.5％、59.0％、20.5％，得到微波介质陶瓷。
实施例3
(1)按照实施例1(1)(2)步骤分别得到A基片和B基片。
(2)将两种基片按照A基片在上、B基片在下的堆叠方式同轴粘合，自上到下每层的厚度占比为73.8％、26.2％，得到微波介质陶瓷。
实施例4
(1)按照质量分数16.7％BaO、44.4％Sm2O3、37.4％TiO2、1.5％Al2O3的配比，称量碳酸钡、氧化钐、二氧化钛(金红石相)、氧化铝，加入无水乙醇行星球磨混合，干燥后过60目筛，在1150℃下预烧4小时；将预烧后的粉体再次行星球磨，干燥后过60目筛，加入聚乙烯醇(PVA)水溶液，造粒并干压成型；对生坯在600℃进行4小时的排胶处理，而后在1350℃烧结4小时，得到A基片。
(2)按照质量分数21.3％CaO、29.4％Sm2O3、42.9％TiO2、6.4％Al2O3的配比，称量碳酸钙、氧化钐、二氧化钛(金红石相)、氧化铝，加入无水乙醇行星球磨混合，干燥后过60目筛，在1100℃下预烧3小时；将预烧后的粉体再次行星球磨，干燥后过60目筛，加入聚乙烯醇(PVA)水溶液，造粒并干压成型；对生坯在600℃进行4小时的排胶处理，而后在1425℃烧结4小时，得到B基片。
(3)将两种基片按照A基片在上、B基片在中、A基片在下的堆叠方式同轴粘合，自上到下每层的厚度占比为42.2％、15.6％、42.2％，得到微波介质陶瓷。
实施例5
(1)按照实施例4(1)(2)步骤分别得到A基片和B基片。
(2)将两种基片按照B基片在上、A基片在中、B基片在下的堆叠方式同轴粘合，自上到下每层的厚度占比为30.4％、39.2％、30.4％，得到微波介质陶瓷。
实施例6
(1)按照实施例4(1)(2)步骤分别得到A基片和B基片。
(2)将两种基片按照A基片在上、B基片在下的堆叠方式同轴粘合，自上到下每层的厚度占比为59.6％、40.4％，得到微波介质陶瓷。
实施例7
(1)按照质量分数16.8％BaO、8.6％Nd2O3、35.7％Sm2O3、36.1％TiO2、2.8％Al2O3的配比，称量碳酸钡、氧化钕、氧化钐、二氧化钛(金红石相)、氧化铝，加入无水乙醇行星球磨混合，干燥后过60目筛，在1150℃下预烧4小时；将预烧后的粉体再次行星球磨，干燥后过60目筛，加入聚乙烯醇(PVA)水溶液，造粒并干压成型；对生坯在600℃进行4小时的排胶处理，而后在1350℃烧结4小时，得到A基片。
(2)按照质量分数21.4％CaO、29.5％Sm2O3、40.5％TiO2、8.6％Al2O3的配比，称量碳酸钙、氧化钐、二氧化钛(金红石相)、氧化铝，加入无水乙醇行星球磨混合，干燥后过60目筛，在1100℃下预烧3小时；将预烧后的粉体再次行星球磨，干燥后过60目筛，加入聚乙烯醇(PVA)水溶液，造粒并干压成型；对生坯在600℃进行4小时的排胶处理，而后在1350℃烧结4小时，得到B基片。
(3)将两种基片按照A基片在上、B基片在中、A基片在下的堆叠方式同轴粘合，自上到下每层的厚度占比为40.9％、19.8％、40.9％，得到微波介质陶瓷。
实施例8
(1)按照实施例7(1)(2)步骤分别得到A基片和B基片。
(2)将两种基片按照B基片在上、A基片在中、B基片在下的堆叠方式同轴粘合，自上到下每层的厚度占比为33.1％、33.8％、33.1％，得到微波介质陶瓷。
实施例9
(1)按照实施例7(1)(2)步骤分别得到A基片和B基片。
(2)将两种基片按照A基片在上、B基片在下的堆叠方式同轴粘合，自上到下每层的厚度占比为55.4％、44.6％，得到微波介质陶瓷。
性能测试
测试实施例1～9中所得微波介质陶瓷的性能，所得结果如表1所示。
表1
实施例 介电常数 Q×f值(GHz) 谐振频率温度系数(ppm/℃)
实施例1 78 13560 -2.7
实施例2 80 16280 +1.8
实施例3 80 14520 -3.6
实施例4 69 15920 +0.9
实施例5 70 20610 -2.6
实施例6 70 18130 -0.9
实施例7 63 20320 -0.8
实施例8 64 20630 -3.3
实施例9 63 21050 -0.8
以上实施例仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应该以权利要求的保护范围为准。

Claims (5)

1.一种层状中高介电常数低损耗微波介质陶瓷，其特征在于，该陶瓷由A基片和B基片层状粘合而成；所述A基片由质量百分比为16％～17％的BaO、6.5％～45％的Sm2O3、8.5％～37％的Nd2O3、36％～40％的TiO2和0.0％～3.0％的Al2O3构成；所述B基片由质量百分比为21％～22％的CaO、29％～30％的Sm2O3、30％～50％的TiO2和0.0％～18％的Al2O3构成；所述微波介质陶瓷的介电常数为60～80，Q×f值为13000～22000GHz，谐振频率温度系数为-5～+5ppm/℃。
2.一种权利要求1所述层状中高介电常数低损耗微波介质陶瓷的制备方法，其特征在于，包括以下步骤：
步骤1：按质量百分比称取A基片的原料粉体，加入无水乙醇行星球磨混合，干燥后过60目筛并进行预烧；将预烧后的粉体再次行星球磨，干燥后再过60目筛，加入聚乙烯醇水溶液，造粒并干压成圆柱状；对生坯进行排胶处理和烧结，得到A基片；
步骤2：按质量百分比称取B基片的原料粉体，加入无水乙醇行星球磨混合，干燥后过60目筛并进行预烧；将预烧后的粉体再次行星球磨，干燥后再过60目筛，加入聚乙烯醇水溶液，造粒并干压成圆柱状；对生坯进行排胶处理和烧结，得到B基片；
步骤3：将烧结后的A基片与B基片的两底面打磨、抛光，采用堆叠方式同轴粘合。
3.根据权利要求2所述层状中高介电常数低损耗微波介质陶瓷的制备方法，其特征在于，所述步骤1中A基片预烧的温度范围为1100～1200℃，预烧时间为2～4小时；干压的压力范围为100～200兆帕且施加压力方式为轴向施压；排胶处理的温度为600℃，排胶时间为2～4小时；烧结的温度范围为1300～1450℃，烧结时间为2～8小时。
4.根据权利要求2所述层状中高介电常数低损耗微波介质陶瓷的制备方法，其特征在于，所述步骤2中B基片预烧的温度范围为1100～1300℃，预烧时间为2～4小时；干压的压力范围为100～200兆帕且施加压力方式为轴向施压；排胶处理的温度为600℃，排胶时间为2～4小时；烧结的温度范围为1300～1550℃，烧结时间为2～8小时。
5.根据权利要求2所述层状中高介电常数低损耗微波介质陶瓷的制备方法，其特征在于，所述步骤3中的堆叠方式为A基片在上、B基片在中、A基片在下，或B基片在上、A基片在中、B基片在下，或A基片在上、B基片在下。
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