CN107382313B - 一种超高品质因数、中低介电常数及近零温度系数的微波介质陶瓷及其制备方法 - Google Patents

一种超高品质因数、中低介电常数及近零温度系数的微波介质陶瓷及其制备方法 Download PDF

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CN107382313B
CN107382313B CN201710407942.5A CN201710407942A CN107382313B CN 107382313 B CN107382313 B CN 107382313B CN 201710407942 A CN201710407942 A CN 201710407942A CN 107382313 B CN107382313 B CN 107382313B
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dielectric ceramic
microwave dielectric
magnesium tantalate
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tanbo
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党明召
任海深
谢天毅
张良柱
姜少虎
姚晓刚
赵相毓
林慧兴
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Shanghai Institute of Ceramics of CAS
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Abstract

本发明涉及一种超高品质因数、中低介电常数及近零温度系数的微波介质陶瓷及其制备方法。钽酸镁系微波介质陶瓷的化学通式为Mg2.5+xTaNbO7.5+x+y wt% B2O3+z wt% C，其中0≤x≤0.2，B2O3的重量百分含量y wt%以Mg2.5+xTaNbO7.5+x的重量为100%计，1≤y≤2，C的重量百分含量z wt%以Mg2.5+xTaNbO7.5+x和B2O3的重量之和为100%计，0≤z≤1；其中C为ZnO、CuO、Al2O3、MnO2、WO3、ZrO2和SnO2中的至少一种。利用Mg元素和Nb元素对钽酸镁系微波介质陶瓷的介电常数进行调节，其频率温度系数也可以做出相应的调整。

Description

一种超高品质因数、中低介电常数及近零温度系数的微波介 质陶瓷及其制备方法
技术领域
本发明属于微波介质陶瓷技术领域，具体涉及一种中低介电常数、超低介电损耗、频率温度系数近零的微波介质陶瓷及其制备方法。
背景技术
近年来，5G通讯技术的迅速发展，对微波器件的需求量也日益增长，尤其是中低介电常数、极低微波损耗和近零频率温度系数系列陶瓷。这种陶瓷既可以满足通信机的可移动性、便携性、小型化、微型化的要求，又可以满足在微波范围具有高性能、高可靠性工作特性要求，得到广泛关注。
MgO-Ta2O5二元体系中，稳定相MgTa2O6具有较高的品质因数Qf值，中低介电常数εr和正的谐振频率温度系数τf(Qf＝60000GHz，εr＝24，τf＝30ppm/℃)不能够满足实际需要。
发明内容
针对上述问题，本发明的目的在于提供一种中低介电常数、极低介电损耗、频率温度系数近零的微波介质陶瓷及其制备方法。
一方面，本发明提供了一种中低介电常数、超低损耗和近零频率温度系数的钽酸镁系微波介质陶瓷，所述钽酸镁系微波介质陶瓷的化学通式为Mg2.5+xTaNbO7.5+x+y wt％B2O3+z wt％C，其中0≤x≤0.2，B2O3的重量百分含量y wt％以Mg2.5+xTaNbO7.5+x的重量为100％计，1≤y≤2，C的重量百分含量z wt％以Mg2.5+xTaNbO7.5+x和B2O3的重量之和为100％计， 0≤z≤1；
其中C为ZnO、CuO、Al2O3、MnO2、WO3、ZrO2和SnO2中的至少一种。
本发明中利用Mg元素和Nb元素对钽酸镁系微波介质陶瓷的介电常数进行调节，其频率温度系数也可以做出相应的调整，其机理是：Mg元素的加入，生成了新的Mg4Ta2O9相，此相εr＝12，Qf＝340000 GHz，τf＝-70 ppm/℃即促进了Qf值的提升又调整了材料的频率温度系数；Nb元素的添加，促进MgTa2O6和Mg4Ta2O9晶格发生畸变，保证材料的Qf值基本不变的前提下，降低了生产成本。此外B2O3的加入引入了低熔点液相，低了陶瓷的烧结温度，适量C物质的添加对稳定材料的Qf值，微量调节频率温度系数起到一定作用。
较佳地，x＝0.1、y＝1时，0.3≤z≤0.6，在此范围内，钽酸镁系微波介质陶瓷介电性能稳定，可重复性好。
较佳地，所述钽酸镁系微波介质陶瓷的介电常数为16.08～19.53，优选为17～18，品质因数Qf值为165000～230000GHz，优选为180000～200000GHz，谐振频率温度系数为-11.69～9.42ppm/℃，优选为-9～9ppm/℃。
另一方面，本发明还提供了一种上述的钽酸镁系微波介质陶瓷的制备方法，包括：
以MgO、Ta2O5、Nb2O5、H3BO3为原料，按Mg2.5+xTaNbO7.5+x+y wt％B2O3化学计量组成称量并混合，先于1000℃～1150℃下预烧4～8小时，得到预烧粉体；
在所得预烧粉体中加入C和粘结剂，经造粒和成型后，得到坯体，所述C的质量为预烧粉体的0～1wt％；
将所得坯体在1250℃～1300℃下烧结4～8小时，得到所述钽酸镁系微波介质陶瓷。
较佳地，所述粘结剂为聚乙烯醇、聚乙烯醇缩丁醛PVB和羧甲基纤维素钠CMC中的至少一种。较佳地，所述粘结剂的用量为预烧粉体的2～3wt％。
本发明的优点是：Mg2.5+xTaNbO7.5+x(0≤x≤0.2)+ywt％B2O3(1≤y≤2)+zwt％C (0≤z≤1)系列微波介质陶瓷材料其烧结范围为1200～1350℃，介电常数为16～18，品质因数180000～200000GHz，谐振频率温度系数为-12～10ppm/℃。此微波介质陶瓷损耗极低，可以满足新一代通讯需求。
具体实施方式
以下通过下述实施方式进一步说明本发明，应理解，下述实施方式仅用于说明本发明，而非限制本发明。
本发明公开了一种超高品质因数、中低介电常数、频率温度系数近零的钽酸镁系微波介质陶瓷，该微波介质陶瓷的化学式为Mg2.5+xTaNbO7.5+x(0≤x≤0.2，优选x＝0.1)+ywt％B2O3(1≤y≤2，优选y＝1)+z wt％C(0≤z≤1，优选0.3≤z≤0.6)，其中 Ta:Nb＝1:1，B2O3的重量百分含量y wt％以Mg2.5+xTaNbO7.5+x的重量为100％计，1≤y≤2，C 的重量百分含量z wt％以Mg2.5+xTaNbO7.5+x和B2O3的重量之和为100％计，0＜z≤1，其中C 为ZnO、CuO、Al2O3、MnO2、WO3、ZrO2和SnO2中的至少一种。该组成介电常数为16～ 20，品质因数Qf为180000～200000GHz，谐振频率温度系数-10ppm/℃～10ppm/℃，有望满足未来5G通讯的需求。
本发明的微波介质陶瓷，制备工艺简单，重复性良好，且微波介电性能优异，烧结温度较低。以下示例性地说明本发明提供的中低介电常数、极低介电损耗、频率温度系数近零的微波介质陶瓷的制备方法。
以MgO、Ta2O5、Nb2O5、H3BO3为原料，按Mg2.5+xTaNbO7.5+x(0≤x≤0.2)+y wt％ B2O3(1≤y≤2)化学计量组成称量并混合，先于1000℃～1150℃下预烧4～8小时，得到预烧粉体。具体来说，将化学原料MgO、Ta2O5、Nb2O5、H3BO3分别按Mg2.5+xTaNbO7.5+x (0≤x≤0.2)+y wt％B2O3(1≤y≤2)化学计量组成称量配料；然后将配制好的化学原料放入含有氧化锆球的球磨罐中球磨1～2h，球磨介质为去离子水。球磨后置于干燥箱中烘干。最后将混合均匀的粉料在1100℃煅烧4～8h，得预烧粉体。在所得预烧粉体中加入C和粘结剂，经造粒和成型后，得到坯体。所述C的质量可为预烧粉体的0～1wt％。
将坯体在1250～1300℃下煅烧4～8小时，得到所述钽酸镁系微波介质陶瓷。作为一个示例，将圆柱状胚体在1250～1300℃保温4～8h烧结成瓷，即获得所需的微波介质陶瓷。
测试制得陶瓷的微波介电性能。样品的直径和厚度使用千分尺测量。借助AgilentE8363A PNA网络分析仪，采用Krupka法(空腔法)测量所制备圆柱形陶瓷材料的介电常数，将测试样品放入ESPEC MC-710F型高低温循环箱进行谐振频率温度系数的测量，温度范围为20～60℃，测试频率在8～14GHz范围内。
下面进一步例举实施例以详细说明本发明。同样应理解，以下实施例只用于对本发明进行进一步说明，不能理解为对本发明保护范围的限制，本领域的技术人员根据本发明的上述内容作出的一些非本质的改进和调整均属于本发明的保护范围。下述示例具体的工艺参数等也仅是合适范围中的一个示例，即本领域技术人员可以通过本文的说明做合适的范围内选择，而并非要限定于下文示例的具体数值。
本发明采用高纯度的MgO、Ta2O5、Nb2O5、H3BO3、C为原料进行制备 Mg2.5+xTaNbO7.5+x(0≤x≤0.2)+ywt％B2O3(1≤y≤2)+zwt％C(0≤z≤1)陶瓷，具体实施例如下。
实施例1
(1)将MgO、Ta2O5、Nb2O5分别按摩尔比2.5:0.5:0.5、2.6:0.5:0.5、2.7:0.5:0.5称量，再加入等效1wt％B2O3的H3BO3，加入氧化锆球和去离子水。球磨1～2h，将球磨后的原料于干燥箱中烘干；
(2)混合均匀的粉料在1100℃煅烧4h；
(3)将步骤(2)煅烧后的原料放入球磨罐中加入氧化锆球和去离子水，球磨1～2h，烘干，向烘干的粉料中加入质量分数为3％的PVA(聚乙烯醇)做为粘结剂造粒，压制成圆柱状胚体；
(4)把圆柱状胚体在1250℃～1300℃下保温4h烧结成瓷，即获得所需的低损耗温度系数近零钽酸镁系微波介质陶瓷；
(5)用网络分析仪和谐振腔测试步骤(4)制得的低损耗温度系数近零钽酸镁微波介质陶瓷微波介电性能；
具体实施例的相关工艺参数和微波介电性能的测试结果详见表1。
表1为实施例1中涉及的实验结果：
Figure BDA0001311489700000041
实施例2
仿照实施例1，在实施例1的基础上选取x＝0.1、y＝1组分添加zwt％C物质，其余与实施例 1相同，测试结果详见表2。
表2为实施例2中涉及的实验结果：
Figure BDA0001311489700000042

Claims (7)

1.一种钽酸镁系微波介质陶瓷，其特征在于，所述钽酸镁系微波介质陶瓷的化学通式为Mg2.5+xTaNbO7.5+x+ y wt% B2O3 + z wt% C，其中0≤x≤0.2，B2O3的重量百分含量y wt%以Mg2.5+xTaNbO7.5+x的重量为100%计，1≤y≤2，C的重量百分含量z wt%以Mg2.5+xTaNbO7.5+x和B2O3的重量之和为100%计，0≤z≤1；
其中C为ZnO、CuO、Al2O3、MnO2、WO3、ZrO2和SnO2中的至少一种。
2.根据权利要求1所述的钽酸镁系微波介质陶瓷，其特征在于，x=0.1、y=1时，0.3≤z≤0.6。
3.根据权利要求1或2所述的钽酸镁系微波介质陶瓷，其特征在于，所述钽酸镁系微波介质陶瓷的介电常数为16.08～19.53，品质因数Qf值为165000～230000 GHz ，谐振频率温度系数为-11.69～9.42 ppm/℃。
4.根据权利要求3所述的钽酸镁系微波介质陶瓷，其特征在于，所述钽酸镁系微波介质陶瓷的介电常数为17～18，品质因数Qf值为180000～200000 GHz，谐振频率温度系数为为-9～9 ppm/℃。
5.一种如权利要求1-4中任一项所述的钽酸镁系微波介质陶瓷的制备方法，其特征在于，包括：
以MgO、Ta2O5、Nb2O5、H3BO3为原料，按Mg2.5+xTaNbO7.5+x+ y wt% B2O3化学计量组成称量并混合，先于1000℃～1150℃下预烧4～8小时，得到预烧粉体；
在所得预烧粉体中加入C和粘结剂，经造粒和成型后，得到坯体，所述C的质量为预烧粉体的0～1wt%；
将所得坯体在1250℃～1300℃下烧结4-8小时，得到所述钽酸镁系微波介质陶瓷。
6.根据权利要求5所述的制备方法，其特征在于，所述粘结剂为聚乙烯醇PVA、聚乙烯醇缩丁醛PVB和羧甲基纤维素钠CMC中的至少一种。
7.根据权利要求5或6所述的制备方法，其特征在于，所述粘结剂的用量为预烧粉体的2～3wt%。
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