CN107805067A - 一种零频率温度系数及超低损耗的低介电常数微波介质陶瓷及其制备方法 - Google Patents

一种零频率温度系数及超低损耗的低介电常数微波介质陶瓷及其制备方法 Download PDF

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CN107805067A
CN107805067A CN201711066157.4A CN201711066157A CN107805067A CN 107805067 A CN107805067 A CN 107805067A CN 201711066157 A CN201711066157 A CN 201711066157A CN 107805067 A CN107805067 A CN 107805067A
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党明召
任海深
谢天毅
彭海益
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

本发明涉及一种零频率温度系数及超低损耗的低介电常数微波介质陶瓷及其制备方法，所述微波介质陶瓷的化学通式为xMg2SiO4‑(1‑x)MgTa2O6+y wt%B，所述B为ZnO、CuO、Al2O3、Ga2O3、TiO2、ZrO2、SnO2、MnO2、Nb2O5、Sb2O5和WO3中的至少一种，其中x代表Mg2SiO4占Mg2SiO4和MgTa2O6总摩尔量的百分数，0＜x＜1；y代表B占Mg2SiO4和MgTa2O6的总质量的百分数，0≤y≤5。

Description

一种零频率温度系数及超低损耗的低介电常数微波介质陶瓷 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，随着5G通讯技术、全球定位技术迅猛发展，作为微波滤波器、谐振器及振荡器等无线通讯器件用的高性能微波介质陶瓷需求量日益增多，尤其是超低微波介电损耗和近零频率温度系数的陶瓷。这种陶瓷既可以满足实现微波通信设备的可移动性、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、大容量信息传输等工作特性要求，得到广泛关注。
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＝30，τf＝30ppm/℃)不能够满足实际需要，而Mg2SiO4同样也具有优异的微波介电性能(Qf＝270000GHz，εr＝6.8，τf＝-67ppm/℃)，也不能满足应用需求。
发明内容
针对上述问题，本发明的目的在于提供一种低介电常数、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。
一方面，本发明提供了一种低介电常数、超低介电损耗的微波介质陶瓷，所述微波介质陶瓷的化学通式为xMg2SiO4-(1-x)MgTa2O6+y wt％B，所述B为ZnO、CuO、Al2O3、Ga2O3、TiO2、ZrO2、SnO2、MnO2、Nb2O5、Sb2O5和WO3中的至少一种，其中x代表Mg2SiO4占Mg2SiO4和MgTa2O6总摩尔量的百分数，0＜x＜1；y代表B占Mg2SiO4和MgTa2O6的总质量的百分数，0≤y≤5。
本发明利用介质陶瓷复合技术对介质陶瓷的介电性能进行调节，以期满足应用需求，其机理是：利用频率温度系数相反的两种基体材料(MgTa2O6具有正的谐振频率温度系数τf＝30ppm/℃，而Mg2SiO4具有负的频率温度系数τf＝-67ppm/℃)，通过控制两相相对成分含量(即摩尔比x：(1-x)，0＜x＜1)，获得频率温度系数近零的结果。此外在两种基体材料中加入适量B物质(B与Mg2SiO4和MgTa2O6的总质量的比y wt％，0≤y≤5)，改善材料的烧结特性，稳定材料的介电性能。
较佳地，所述微波介质陶瓷的介电常数为6.9～28.3，品质因数Qf值为60000～275000GHz，谐振频率温度系数为-70～55ppm/℃。
较佳地，0.5≤x≤0.7或/和1≤y≤3。
又，较佳地，当0.5≤x≤0.7和1≤y≤3时，所述微波介质陶瓷的介电常数为12.1～15.2，优选为13～15，品质因数Qf值为120000～152000GHz，优选为125000～140000GHz，谐振频率温度系数为-11～18ppm/℃，优选为0～4ppm/℃。
另一方面，本发明提供了一种如上述的微波介质陶瓷的制备方法，包括：
将Mg2SiO4粉体和MgTa2O6粉体按xMg2SiO4-(1-x)MgTa2O6化学计量组成称量并混合，得到混合粉体；
在所得混合粉体中加入B和粘结剂，经破碎，造粒和成型后，得到坯体；
将所得坯体在1300～1450℃下烧结4～16h，得到所述微波介质陶瓷。
较佳地，以MgO、Ta2O5、SiO2为原料，分别预先合成Mg2SiO4粉体和MgTa2O6粉体。
又，较佳地，将MgO和SiO2混合后，在1000～1250℃下煅烧4～12h，得到Mg2SiO4。
又，较佳地，将MgO和Ta2O5混合后，在1000～1250℃下煅烧4～12h，得到MgTa2O6粉体。
较佳地，所述B的质量为混合粉体质量的0～5wt％，优选为1～3wt％。
较佳地，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，所述粘结剂的用量为混合粉体质量的2～4wt％。
本发明的优点是：xMg2SiO4-(1-x)MgTa2O6+y wt％B复合微波介质陶瓷材料介电常数低且可调节范围广为6.9～28.3，品质因数高60000～275000GHz，谐振频率温度系数连续可调，可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。
本发明中，所述低介电常数、高品质因数、近零频率温度系数的复合微波介质陶瓷，该微波介质陶瓷的化学式可表示为xMg2SiO4-(1-x)MgTa2O6+y wt％B。其中B可为ZnO、CuO、Al2O3、Ga2O3、TiO2、ZrO2、SnO2、MnO2、Nb2O5、Sb2O5和WO3中的至少一种。其中x代表Mg2SiO4占Mg2SiO4和MgTa2O6总摩尔量的百分数，0＜x＜1(优选为0.5≤x≤0.7)；y代表B占Mg2SiO4和MgTa2O6的总质量的百分数，0≤y≤5(优选为1≤y≤3)。若B的加入量超过5wt％，将生成新的化合物，所述微波介质陶瓷的各项性能将偏离预测值。
本发明中，所述微波介质陶瓷的介电常数为6.9～28.3，品质因数Qf值为60000～275000GHz，谐振频率温度系数为-70～55ppm/℃。当0.5≤x≤0.7，1≤y≤3时，在此范围内，复合微波介质陶瓷介电性能稳定，可重复性好，所述微波介质陶瓷的介电常数为12.1～15.2，优选为13～15，品质因数Qf值为120000～152000GHz，优选为125000～140000GHz，谐振频率温度系数为-11～18ppm/℃，优选为0～4ppm/℃。
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。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。
Mg2SiO4粉体和MgTa2O6粉体的制备。具体来说，以MgO、Ta2O5、SiO2为原料，分别预先合成Mg2SiO4粉体和MgTa2O6粉体。将MgO和SiO2或MgO和Ta2O5混合后，在1000～1250℃下煅烧4～12h，得到Mg2SiO4或MgTa2O6粉体。上述混合的方式可为球磨混合等。应注意，本发明中Mg2SiO4粉体和MgTa2O6粉体的制备并不仅限于上述制备方法。其他方法制备的Mg2SiO4粉体和MgTa2O6粉体也可用于此微波介质陶瓷的制备。
将Mg2SiO4粉体和MgTa2O6粉体按xMg2SiO4-(1-x)MgTa2O6化学计量组成称量，并在混合粉体中加入B和粘结剂，经破碎，造粒和成型后，得到所需坯体。所述B的质量为混合粉体质量的0～5wt％，优选为1～3wt％。所述粘结剂可为聚乙烯醇(PVA)、聚乙烯醇缩丁醛(PVB)和羧甲基纤维素钠(CMC)等中的至少一种。所述粘结剂的用量可为混合粉体质量的2～4wt％。所述成型方式可为干压成型、冷等静压成型等。
将所得坯体在1300℃～1450℃下烧结4～16h，得所述低介电常数微波介质陶瓷。
作为一个微波介质陶瓷的制备方法的示例，以高纯(纯度>99％)MgO、SiO2和Ta2O5为原料，在1000～1250℃(优选1000～1200℃)下煅烧4～12h合成Mg2SiO4粉体和MgTa2O6粉体，再按xMg2SiO4-(1-x)MgTa2O6化学计量组成称量，同时加入质量分数为y wt％的B，破碎后加入粘结剂进行造粒和成型，得到坯体；将所得坯体在1350～1450℃下烧结4～16h，得到所述微波介质陶瓷。
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，采用空腔法测量所制备圆柱形陶瓷材料的介电常数和介电损耗，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20～85℃，测试频率在9～16GHz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做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、SiO2和B为原料进行制备xMg2SiO4-(1-x)MgTa2O6+y wt％B陶瓷，具体实施例如下。
实施例1
(1)将MgO、Ta2O5、SiO2分别按摩尔比MgO:Ta2O5＝1:1和MgO:SiO2＝2:1称量，加入氧化锆球和去离子水。球磨1～2小时，将球磨后的原料于干燥箱中烘干后于1100℃煅烧4h合成MgTa2O6和Mg2SiO4；
(2)将合成的Mg2SiO4和MgTa2O6按照摩尔分数比为0.4:0.6、0.5:0.5、0.6:0.4、0.7:0.3、0.8:0.2称量放入加入氧化锆球、去离子水球磨罐中，球磨1～2h，烘干后，向粉料中加入质量分数为3％的PVA(聚乙烯醇)作为粘结剂造粒，压制成圆柱状胚体；
(4)把圆柱状胚体在1350℃下保温8h烧结成瓷，即获得所需的复合微波介质陶瓷；
(5)用网络分析仪和谐振腔测试步骤(4)制得的复合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：
实施例2
仿照实施例1，在实施例1的基础上选取x＝0.6组分，在第(2)步中添加B物质含量为1wt％，其余步骤与实施例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：
实施例3
仿照实施例2，在实施例2的基础上，选取B物质为ZnO，改变B物质的添加量，其余步骤与实施例1相同，测试结果详见表3。
表3为实施例3中涉及的实验结果：

Claims (10)

1.一种低介电常数、超低介电损耗的微波介质陶瓷，其特征在于，所述微波介质陶瓷的化学通式为xMg2SiO4-(1-x)MgTa2O6+ y wt% B，所述B为ZnO、CuO、Al2O3、Ga2O3、TiO2、ZrO2、SnO2、MnO2、Nb2O5、Sb2O5和WO3中的至少一种，其中x代表Mg2SiO4占Mg2SiO4和MgTa2O6总摩尔量的百分数，0＜x＜1；y代表B占Mg2SiO4和MgTa2O6的总质量的百分数，0≤y≤5。
2.根据权利要求1所述的微波介质陶瓷，其特征在于，所述微波介质陶瓷的介电常数为6.9～28.3，品质因数Qf值为60000～275000 GHz，谐振频率温度系数为-70～55 ppm/℃。
3.根据权利要求1或2所述的微波介质陶瓷，其特征在于，0.5≤x≤0.7或/和1≤y≤3。
4.根据权利要求3所述的微波介质陶瓷，其特征在于，当0.5≤x≤0.7和1≤y≤3时，所述微波介质陶瓷的介电常数为12.1～15.2，优选为13～15，品质因数Qf值为120000～152000 GHz，优选为125000～140000 GHz，谐振频率温度系数为-11～18 ppm/℃，优选为0～4 ppm/℃。
5.一种如权利要求1-4中任一项所述的微波介质陶瓷的制备方法，其特征在于，包括：
将Mg2SiO4粉体和 MgTa2O6粉体按xMg2SiO4-(1-x)MgTa2O6化学计量组成称量并混合，得到混合粉体；
在所得混合粉体中加入B和粘结剂，经破碎，造粒和成型后，得到坯体；
将所得坯体在1300～1450 ℃下烧结4～16 h，得到所述微波介质陶瓷。
6.根据权利要求5所述的制备方法，其特征在于，以MgO、Ta2O5、SiO2为原料，分别预先合成Mg2SiO4粉体和 MgTa2O6粉体。
7.根据权利要求6所述的制备方法，其特征在于，将MgO和SiO2混合后，在1000～1250℃下煅烧4～12h，得到Mg2SiO4。
8.根据权利要求6所述的制备方法，其特征在于，将MgO和Ta2O5混合后，在1000～1250℃下煅烧4～12h，得到MgTa2O6粉体。
9.根据权利要求5-8中任一项中所述的制备方法，其特征在于，所述B的质量为混合粉体质量的0～5 wt%，优选为1～3 wt%。
10.根据权利要求5-9中任一项中所述的制备方法，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，优选地所述粘结剂的用量为混合粉体质量的2～4 wt%。
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108439969A (zh) * 2018-06-29 2018-08-24 无锡鑫圣慧龙纳米陶瓷技术有限公司 一种低介电常数温度稳定型微波介质及其制备方法
CN109503163A (zh) * 2018-12-20 2019-03-22 中国科学院上海硅酸盐研究所 一种具有超高q值钽酸镁介质陶瓷及其制备方法
CN113563061A (zh) * 2021-09-26 2021-10-29 广东康荣高科新材料股份有限公司 一种用于单腔滤波器的低介电常数介质材料及其制备方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1195651A (zh) * 1997-04-09 1998-10-14 阿莫同有限公司 介电陶瓷组合物
CN103319166A (zh) * 2013-05-28 2013-09-25 电子科技大学 一种微波陶瓷介质材料及其制备方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1195651A (zh) * 1997-04-09 1998-10-14 阿莫同有限公司 介电陶瓷组合物
CN103319166A (zh) * 2013-05-28 2013-09-25 电子科技大学 一种微波陶瓷介质材料及其制备方法

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
CHANG JUN JEON等: "Microwave Dielectric Properties of MgTiO3, MgTa2O6 /Polytetrafluoroethylene Composite", 《JOURNAL OF THE KOREAN CERAMIC SOCIETY》 *
CHENG-LIANG HUANG等: "Structures and dielectric properties of a new dielectric material system xMgTiO3–(1−x)MgTa2O6 at microwave frequency", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *
宋开新: "低介电常数微波介质陶瓷", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 *
王迎军: "《新型材料科学与技术 无机材料卷 中》", 31 October 2016, 华南理工大学出版 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108439969A (zh) * 2018-06-29 2018-08-24 无锡鑫圣慧龙纳米陶瓷技术有限公司 一种低介电常数温度稳定型微波介质及其制备方法
CN109503163A (zh) * 2018-12-20 2019-03-22 中国科学院上海硅酸盐研究所 一种具有超高q值钽酸镁介质陶瓷及其制备方法
CN113563061A (zh) * 2021-09-26 2021-10-29 广东康荣高科新材料股份有限公司 一种用于单腔滤波器的低介电常数介质材料及其制备方法
CN113563061B (zh) * 2021-09-26 2021-12-21 广东康荣高科新材料股份有限公司 一种用于单腔滤波器的低介电常数介质材料及其制备方法

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