CN111320473A - 一种低烧微波介质陶瓷材料及其制备方法 - Google Patents

一种低烧微波介质陶瓷材料及其制备方法 Download PDF

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CN111320473A
CN111320473A CN202010145578.1A CN202010145578A CN111320473A CN 111320473 A CN111320473 A CN 111320473A CN 202010145578 A CN202010145578 A CN 202010145578A CN 111320473 A CN111320473 A CN 111320473A
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dielectric ceramic
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付清波
应红
杨彬
杨月霞
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Shandong Sinocera Functional Material Co Ltd
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Abstract

本发明属于微波介质材料技术领域，具体涉及一种BaZrO3体系低温烧结低介电常数C0G微波介质材料及其制备方法。本发明所述低烧微波介质陶瓷材料，以BaZrO3、Mg2SiO4为基础，通过掺杂选定组分和配比的改性添加剂和助烧剂进行制备，所得微波介质陶瓷材料的介电常数可做到12‑16，Q*f值：30000‑50000，尤其是材料的烧结温度可以达到950℃以下，其TCC符合C0G规格，具有较好的低温烧结性，可用于MLCC、微波天线等微波器件的制造。

Description

一种低烧微波介质陶瓷材料及其制备方法
技术领域
本发明属于微波介质材料技术领域，具体涉及一种BaZrO3体系低温烧结低介电常数C0G微波介质材料及其制备方法。
背景技术
微波介质陶瓷是指应用于微波频段(主要是UHF、SHF频段，
300MHz-300GHz)电路中作为介质材料并完成一种或多种功能的陶瓷，其具有高介电常数、低介电损耗、低谐振频率温度系数等优良性能，是谐振器、滤波器、双工器、天线、稳频振荡器、波导传输线等器件的重要组成元件，可广泛应用于个人便携式移动电话、微波基站、车载电话、卫星通讯、军用雷达等众多领域。尤其是近年来，随着通讯技术的迅速发展，对微波器件的需求量也日益增长，特别是5G通信时代基站数量增加导致滤波器需求增加，陶瓷介质滤波器由于具有高Q值、选频特性好、工作频率稳定性好、插入损耗小及更加小型化和集成化等优势而受到越来越多的关注，这成为近年来国内外对微波介质材料研究领域的一个热点方向。
随着微波通讯技术的发展，对元器件的小型化、集成化以及模块化的要求也越来越迫切，微波陶瓷电容器是目前世界上用量最大、发展最快的电子元件之一。微波陶瓷电容器主要应用于各类军用民用整机的震荡、耦合、滤波、旁路电路中，应用领域已经拓展到自动控制仪表、计算机、手机、数字家电、汽车、电力等行业。目前，微波陶瓷电容器已经成为了电容器市场的重要组成，全球市场的需求量增长速度近15％，不仅市场需求巨大，且产业化市场前景非常广阔。
以微波片式多层陶瓷电容器而言，目前国际上多采用中、高烧体系(烧温＞1100℃)的微波介质陶瓷材料匹配银钯内电极浆料进行制造生产。虽然电容器性能可以满足要求，但鉴于选用的微波介质材料需要在中、高温体系下才能完成烧结制造，造成整个工艺能耗较大，进而影响成本较高。
发明内容
为此，本发明所要解决的技术问题在于提供一种以BaZrO3、Mg2SiO4为主料的低温烧结低介电常数的C0G微波介质陶瓷材料，该陶瓷能够在较低温度烧结下，并且具有良好介电性能的同时温度系数满足C0G规格；
本发明所要解决的第二个技术问题在于提高上述微波介质陶瓷材料的制备方法和应用。
为解决上述技术问题，本发明所述的一种低烧微波介质陶瓷材料，以所述微波介质陶瓷材料的制备原料总量计，包括如下质量含量的组分：
Figure BDA0002400588900000021
具体的，所述改性添加剂包括Mn、Co、Al、Ca和/或Ti的氧化物和/或碳酸盐。优选的，所述改性添加剂包括MnCO3、CoO、Al2O3、CaCO3、TiO2中的一种或几种。
更优选的，所述改性添加剂包括：
Figure BDA0002400588900000022
具体的，所述助烧剂包括Li、Zn、Bi、B、Si和/或Mg的氧化物和/或碳酸盐。优选的，所述的烧结助剂包括LiOH、ZnO、Bi2O3、H3BO3、SiO2、MgO的一种或几种。
更优选的，所述助烧剂以其总量计，包括如下质量含量的组分：
Figure BDA0002400588900000031
本发明还公开了一种制备所述低烧微波介质陶瓷材料的方法，包括如下步骤：
(1)取选定成分和含量的所述助烧剂干混混匀，经玻璃熔炉熔制1200-1300℃，保温0.5-2h，将淬火处理后的玻璃研磨成粉体，备用；
(2)取选定含量的所述BaZrO3、Mg2SiO4、改性添加剂和助烧剂混合并进行球磨处理，并加入胶液进行喷雾造粒，即得所需低烧微波介质陶瓷材料。
具体的，所述低烧微波介质陶瓷材料的制备方法，还包括制备所述BaZrO3的步骤，具体包括以BaCO3、ZrO2按摩尔比1：1的比例球磨混合均匀后，于1000-1200℃进行煅烧2-5小时的步骤。
具体的，所述低烧微波介质陶瓷材料的制备方法，还包括制备所述Mg2SiO4的步骤，具体包括以Mg(OH)2、SiO2按摩尔比2：1的比例球磨混合均匀后，于1000-1200℃进行煅烧3-5小时的步骤。
具体的，所述胶液包括PVA胶液和/或丙烯酸胶液。
本发明还公开了一种微波陶瓷电容器，其特征在于，由所述低烧微波介质陶瓷材料制得。
本发明还公开了一种制备所述微波陶瓷电容器的方法，包括将所述低烧微波介质陶瓷材料经干压成型后于900-930℃进行烧结2-8h的步骤。
本发明所述低烧微波介质陶瓷材料，以BaZrO3、Mg2SiO4为基础，通过掺杂选定组分和配比的改性添加剂和助烧剂进行制备，所得微波介质陶瓷材料的介电常数可做到12-16，Q*f值：30000-50000，尤其是材料的烧结温度可以达到950℃以下，其TCC符合C0G规格，具有较好的低温烧结性，可用于MLCC、微波天线等微波器件的制造。
具体实施方式
按照摩尔比1：1取BaCO3和ZrO2球磨混合均匀后，在1100℃煅烧4小时，制得所需BaZrO3。
按照摩尔比2：1取Mg(OH)2和SiO2球磨混合均匀后，在1150℃煅烧4小时，制得所需Mg2SiO4。
分别按照下表1中列明的含量取所述BaZrO3和Mg2SiO4，并加入如下表1所述组分及含量的改性添加剂和助烧剂混合，并进行球磨处理；将球磨后的物料加入丙烯酸胶液(胶含量5wt％)，采用喷雾干燥机进行喷雾造粒，控制进口温度210±10℃，出口温度130±10℃，即得所需低烧微波介质陶瓷材料。
所述助烧剂为按照如下表1中选定成分和含量组分混匀，经玻璃熔炉熔制1200℃，保温2h后淬火处理制得，并研磨成粉体。
表1低烧微波介质陶瓷材料的成分及用量表(kg)
Figure BDA0002400588900000041
Figure BDA0002400588900000051
实验例
将上述造粒后的物料分别进行干压成型，并分别将压制的生坯进行保温煅烧3h，并记录可使各材料生坯成型的烧结温度。
分别对上述实施例1-5及对比例1-4中制得的微波介质陶瓷材料进行性能测试，具体包括材料的介电常数、25℃的f*Q值、以及频率温度系数τf；
所述介电常数、25℃的f*Q值采用现有技术已知方法即可；
所述频率温度系数τf代表具有良好的温度特性，通过分别测试-40℃、25℃、110℃时的共振频率f，并按照如下公式计算：
τf＝[(f110℃-f-40℃)/f25℃]/150*106(ppm/℃)。
测定及计算结果见下表2。
表2微波介质陶瓷材料的性能测试结果
编号 f*Q(GHz) τf(ppm/℃)(-40℃-110℃) 介电常数 烧结温度(℃)
实施例1 50363 -8.53 12.25 915
实施例2 32761 -0.39 15.86 915
实施例3 48623 -6.55 13.47 915
实施例4 39462 -7.01 13.21 915
实施例5 37596 -4.63 14.62 915
对比例1 200 150 40 1550
对比例2 185 87 36 1150
对比例3 163093 -57.82 7 1450
对比例4 124231 -44.62 6.51 1150
可见，本发明所述复合微波介质陶瓷材料品质因数较高，介电常数在12-16左右，25℃的f*Q值为30000-50000，尤其是材料的烧结温度仅为950℃以下，其TCC符合C0G规格，低温烧结性能大幅提升，可以大批稳定生产，可用于MLCC、微波天线等微波器件的制造。
显然，上述实施例仅仅是为清楚地说明所作的举例，而并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。

Claims (10)

1.一种低烧微波介质陶瓷材料，其特征在于，以所述微波介质陶瓷材料的制备原料总量计，包括如下质量含量的组分：
Figure FDA0002400588890000011
2.根据权利要求1所述的低烧微波介质陶瓷材料，其特征在于，所述改性添加剂包括Mn、Co、Al、Ca和/或Ti的氧化物和/或碳酸盐。
3.根据权利要求2所述的低烧微波介质陶瓷材料，其特征在于，所述改性添加剂包括：
Figure FDA0002400588890000012
4.根据权利要求1-3任一项所述的低烧微波介质陶瓷材料，其特征在于，所述助烧剂包括Li、Zn、Bi、B、Si和/或Mg的氧化物和/或碳酸盐。
5.根据权利要求4所述的低烧微波介质陶瓷材料，其特征在于，所述助烧剂以其总量计，包括如下质量含量的组分：
Figure FDA0002400588890000013
Figure FDA0002400588890000021
6.一种制备权利要求1-5任一项所述低烧微波介质陶瓷材料的方法，其特征在于，包括如下步骤：
(1)取选定成分和含量的所述改性添加剂混匀，经熔制及淬火处理后，研磨成粉体，备用；
(2)取选定成分和含量的所述助烧剂混匀，经熔制及淬火处理后，研磨成粉体，备用；
(3)取选定含量的所述BaZrO3、Mg2SiO4、改性添加剂和助烧剂混合并进行球磨处理，并加入胶液进行喷雾造粒，即得所需低烧微波介质陶瓷材料。
7.根据权利要求6所述低烧微波介质陶瓷材料的制备方法，其特征在于，还包括制备所述BaZrO3的步骤，具体包括以BaCO3、ZrO2按摩尔比1：1的比例球磨混合均匀后，于1000-1100℃进行煅烧2-5小时的步骤。
8.根据权利要求6或7所述低烧微波介质陶瓷材料的制备方法，其特征在于，还包括制备所述Mg2SiO4的步骤，具体包括以Mg(OH)2、SiO2按摩尔比2：1的比例球磨混合均匀后，于1000-1200℃进行煅烧3-5小时的步骤。
9.一种微波陶瓷电容器，其特征在于，由权利要求1-5任一项所述低烧微波介质陶瓷材料制得。
10.一种制备权利要求9所述微波陶瓷电容器的方法，其特征在于，包括将权利要求1-5任一项所述低烧微波介质陶瓷材料经干压成型后于900℃-930℃进行烧结2-8h的步骤。
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