CN111410528A - 一种微波介电陶瓷及一种微波介电陶瓷的制作方法 - Google Patents
一种微波介电陶瓷及一种微波介电陶瓷的制作方法 Download PDFInfo
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- 238000005496 tempering Methods 0.000 claims abstract description 48
- 238000010791 quenching Methods 0.000 claims abstract description 47
- 230000000171 quenching effect Effects 0.000 claims abstract description 47
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- 239000000843 powder Substances 0.000 claims description 100
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- 239000000463 material Substances 0.000 claims description 15
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- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Inorganic materials [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 9
- 229920005596 polymer binder Polymers 0.000 claims description 8
- 229910016459 AlB2 Inorganic materials 0.000 claims description 6
- 229910002116 Bi12TiO20 Inorganic materials 0.000 claims description 6
- 229910002900 Bi2MoO6 Inorganic materials 0.000 claims description 6
- 229910002118 Bi2Ti2O7 Inorganic materials 0.000 claims description 6
- 229910003122 ZnTiO3 Inorganic materials 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- 238000005238 degreasing Methods 0.000 claims description 6
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- 229910014780 CaAl2 Inorganic materials 0.000 claims description 3
- 229910002971 CaTiO3 Inorganic materials 0.000 claims description 3
- 229910002230 La2Zr2O7 Inorganic materials 0.000 claims description 3
- 229910017676 MgTiO3 Inorganic materials 0.000 claims description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 3
- 229910002113 barium titanate Inorganic materials 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
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- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 3
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 3
- 229920006324 polyoxymethylene Polymers 0.000 claims description 3
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- 229930040373 Paraformaldehyde Natural products 0.000 claims 1
- -1 polyoxymethylene Polymers 0.000 claims 1
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- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
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Abstract
本发明提供的微波介电陶瓷，包括若干微观单元，所述微观单元包括主晶相和用于调整所述主晶相的微波介电特性的调质修饰相，通过使调质修饰相包裹在主晶相的外表面，既能够通过调质修饰相对主晶相的微波介电特性进行调整，使微波介电陶瓷具有较好的微波介电性能的同时，又能够使微波介电陶瓷具有很高的致密性；本发明提供的微波介电陶瓷的制作方法，通过分别煅烧主晶相和用于调整主晶相的微波介电特性的调质修饰相，将主晶相和调质修饰相按比例混合后在介于调质修饰相的烧结温度和主晶相的烧结温度之间的温度下烧结，得到微波介电陶瓷，该方法能耗低成本低，能够避免烧结时主晶相发生反应的现象，使微波介电陶瓷的微波介电性能更加稳定。
Description
技术领域
本申请涉及微波介电陶瓷技术领域，具体涉及一种微波介电陶瓷及一种微波介电陶瓷的制作方法。
背景技术
微波介电陶瓷是近年来迅速发展起来的新型功能电子陶瓷，具有优良的介电性能，广泛应用于介质谐振器、介质滤波器、天线等微波元气件的制作，随着现代移动通信和卫星通信的发展，对微波介电陶瓷的小型化和微波介电性能的要求越来越高，需要微波介电陶瓷具有高介电常数、高质量因子、近零的谐振频率温度系数和高致密性，为解决这一问题，市场上的微波介电陶瓷多由主晶相（100）、调质修饰相（200）及玻璃相（300）组合而成，如图1所示，主晶相（100）是微波介电陶瓷的主体，其所占的百分比越高产品的微波介电性能越大，调质修饰相（200）用于调整主晶相（100）在某些性能方面的不足，其所占的百分比并不大，玻璃相（300）主要用于使产品致密化，但是玻璃相（300）的加入对产品的介电常数、质量因子及谐振频率温度系数并无帮助，反而因玻璃相（300）的加入会导致主晶相（100）所占的百分比降低，从而影响产品的微波介电性能。
制作上述微波介电陶瓷主要采用以下三种方式：
第一种方式为，将所有主晶相、调质修饰相、玻璃相的氧化物陶瓷粉体按设计比例配制后经过混粉、烘干、造粒、成型、烧结的方式制成，如中国专利CN103570349、CN105399422A、CN105000884A就采用了这一方式，但这种方式对于氧化物陶瓷粉体间的反应顺序及反应结果无法有效掌控，容易生成设计外的晶相结构，如俗称的焦绿石相，进而导致产品的微波介电性能不可控制，使产品的微波介电性能变差；
第二种方式为，先完成主晶相烧结后再添加玻璃相一起烧结的方式，如中国专利CN108383519A就采用了这一方式，但这种方式因主晶相和玻璃相反应能的差异（部分有共晶反应），容易造成微波介电陶瓷的主晶相的结构不稳定或不完全，影响产品的微波介电性能；
第三种方式为，先烧结玻璃相后，再按比例加入主晶相及调质修饰相，然后以高于主晶相的烧结温度烧制产品，如中国专利CN109761603A就采用了这一方式，但这种方式最终的烧结温度远高于玻璃相的熔点，不仅能耗高、成本高，而且容易使玻璃相与主晶相之间发生反应生成不需要的相，如焦绿石相等，影响产品的微波介电性能，且添加的玻璃相主要用于增加致密性，并不能有效提升产品的微波介电性能。
发明内容
本发明的目的是为了克服现有技术的缺点，提供一种具有高介电常数、高质量因子、近零的谐振频率温度系数和高致密性的微波介电陶瓷，本发明还提供一种低能耗、低成本的微波介电陶瓷的制作方法，该方法制作出的微波介电陶瓷的微波介电性能更加稳定。
为实现上述目的，本发明提供的技术方案中的产品是，一种微波介电陶瓷，由若干微观单元构成，所述微观单元包括：
主晶相；
调质修饰相，所述调质修饰相用于调整所述主晶相的微波介电特性；
所述调质修饰相包裹在所述主晶相的外表面。
优选地，所述主晶相的内部不含有所述调质修饰相。
进一步优选地，所述主晶相的材料结构包括钙钛矿结构、类钙钛矿结构、钨青铜结构、尖晶石结构、层状钙钛矿结构中的任意一种；所述钙钛矿结构的成分为CaTiO3、MgTiO3 、BaTiO3中的任意一种或其混合物，所述类钙钛矿结构的成分为BaTi4O9、MgTi4O9、SrTi4O9中的任意一种或其混合物，所述钨青铜结构的成分为Ba5LnMNb9O30，所述尖晶石结构的成分为MgAl2O3、SrAl2O3、CaAl2O3、BaAl2O3中的任意一种或其混合物，所述层状钙钛矿结构的成分为La2Ti2O7、Y2Ti2O7、Nd2Ti2O7、La2Zr2O7、Y2Zr2O7、Nd2Zr2O7、La2Nb4O13、Y2Nb4O13、Nd2Nb4O13中的任意一种或其混合物。
进一步优选地，所述调质修饰相的成分为Bi4Ti3O12、Bi2Ti4O11、Bi12TiO20、Bi2Ti2O7、Bi2MoO6、Bi2Mo2O9、BiVO4、BiNbO4、ZnTiO3、Li3AlB2O6中的任意一种或其混合物。
为实现上述目的，本发明提供的技术方案中的方法是，一种微波介电陶瓷的制作方法，包括如下步骤：
分别煅烧主晶相和用于调整所述主晶相的微波介电特性的调质修饰相，所述主晶相的烧结温度高于所述调质修饰相的烧结温度；
将所述主晶相和所述调质修饰相按比例混合得到混合物；
对所述混合物在温度t下进行烧结，得到所述微波介电陶瓷；
所述温度t介于所述调质修饰相的烧结温度和所述主晶相的烧结温度之间，所述调质修饰相包裹在所述主晶相的外表面。
优选地，在对所述混合物进行烧结之前，还包括如下步骤：将所述混合物经喷雾造粒或密炼制程的方式制成陶瓷注塑烧结所需的喂料，将所述喂料通过注塑成型的方式制成生胚，对所述生胚进行脱脂、烧结。
进一步优选地，所述主晶相的材料结构为钙钛矿结构，所述钙钛矿结构的所述主晶相由A粉体及TiO2粉体按摩尔比1:1经球磨混合后，在950℃~1300℃煅烧而成，所述A粉体为CaCO3粉体、MgO粉体、BaCO3粉体中的任意一种或其混合物；
或，所述主晶相的材料结构为类钙钛矿结构，所述类钙钛矿结构的所述主晶相由B粉体及TiO2粉体按摩尔比1:4经球磨混合后，在1000℃~1350℃煅烧而成，所述B粉体为BaCO3 粉体、MgO粉体、SrCO3粉体中的任意一种或其混合物；
或，所述主晶相的材料结构为尖晶石结构，所述尖晶石结构的所述主晶相由C粉体及TiO2粉体按摩尔比1:1经球磨混合后，在1000℃~1300℃煅烧而成，所述C粉体为MgO粉体、SrCO3粉体、CaCO3粉体、BaCO3粉体中的任意一种或其混合物；
或，所述主晶相的材料结构为层状钙钛矿结构，所述层状钙钛矿结构的所述主晶相由D粉体及E粉体按摩尔比1:2经球磨混合后，在1100℃~1400℃煅烧而成，所述D粉体为La2O3粉体、Y2O3粉体、Nd2O3粉体中的任意一种或其混合物，所述E粉体为TiO2粉体、ZrO2粉体、Nb2O5粉体中的任意一种或其混合物。
优选地，所述调质修饰相的成分为Bi4Ti3O12、Bi2Ti4O11、Bi12TiO20、Bi2Ti2O7、Bi2MoO6、Bi2Mo2O9、Bi2VO4、BiNbO4、ZnTiO3、Li3AlB2O6中的任意一种或其混合物。
进一步优选地，所述混合物在制成所述喂料时添加有高分子粘结剂，所述脱脂用于脱去所述高分子粘结剂。
进一步优选地，所述高分子粘结剂包括聚甲醛高分子粘结剂。
由于上述技术方案的运用，本发明与现有技术相比具有下列优点：
本发明提供的微波介电陶瓷，包括若干微观单元，所述微观单元包括主晶相和用于调整所述主晶相的微波介电特性的调质修饰相，通过使调质修饰相包裹在主晶相的外表面，既能够通过调质修饰相对主晶相的微波介电特性进行调整，使微波介电陶瓷具有高介电常数、高质量因子、近零的谐振频率温度系数的特性，又能够使微波介电陶瓷具有很高的致密性；本发明提供的微波介电陶瓷的制作方法，通过分别煅烧主晶相和用于调整所述主晶相的微波介电特性的调质修饰相，将主晶相和调质修饰相按比例混合得到混合物，对混合物在调质修饰相的烧结温度和主晶相的烧结温度之间的温度下进行烧结，得到调质修饰相包裹在主晶相的外表面微波介电陶瓷，该方法降低了最终的烧结温度，降低了能耗和成本，同时，还避免了最终烧结时主晶相发生反应产生不良相的现象，使制成的微波介电陶瓷微波介电性能更加稳定。
附图说明
图1为现有技术微波介电陶瓷结构示意图。
图2为本发明提供的微波介电陶瓷的一种实施例的结构示意图。
图3为本发明中微波介电陶瓷制作方法的一种实施例的流程图。
其中：100.主晶相；200.调质修饰相；300.玻璃相；400.微观单元。
具体实施方式
下面结合附图对本发明的较佳实施例进行详细阐述，以使本发明的优点和特征更易于被本领域技术人员理解，从而对本发明的保护范围做出更为清楚明确的界定。
如图2所示，本发明提供的微波介电陶瓷，由若干微观单元400构成，微观单元400包括：主晶相100和调质修饰相200，调质修饰相200用于调整主晶相100的微波介电特性，调质修饰相200包裹在主晶相100的外表面，所有微观单元400的调质修饰相200互相连接，并在所述微波介电陶瓷的表面形成一个致密层，该整体还填充相邻的微观单元400之间的间隙，使所述微波介电陶瓷的内部更加致密。
主晶相100的内部不含有调质修饰相200。
主晶相100的材料结构可以为钙钛矿结构、类钙钛矿结构、钨青铜结构、尖晶石结构、层状钙钛矿结构中的任意一种，其中，钙钛矿结构的成分为CaTiO3、MgTiO3 、BaTiO3中的任意一种或其混合物，类钙钛矿结构的成分为BaTi4O9、MgTi4O9、SrTi4O9中的任意一种或其混合物，钨青铜结构的成分为Ba5LnMNb9O30，尖晶石结构的成分为MgAl2O3、SrAl2O3、CaAl2O3、BaAl2O3中的任意一种或其混合物，层状钙钛矿结构的成分为La2Ti2O7、Y2Ti2O7、Nd2Ti2O7、La2Zr2O7、Y2Zr2O7、Nd2Zr2O7、La2Nb4O13、Y2Nb4O13、Nd2Nb4O13中的任意一种或其混合物。
调质修饰相200的成分为Bi4Ti3O12、Bi2Ti4O11、Bi12TiO20、Bi2Ti2O7、Bi2MoO6、Bi2Mo2O9、BiVO4、BiNbO4、ZnTiO3、Li3AlB2O6中的任意一种或其混合物。
本发明提供的微波介电陶瓷，包括若干微观单元，所述微观单元包括主晶相和用于调整所述主晶相的微波介电特性的调质修饰相，通过使调质修饰相包裹在主晶相的外表面，既能够通过调质修饰相对主晶相的微波介电特性进行调整，使微波介电陶瓷具有高介电常数、高质量因子、近零的谐振频率温度系数的特性，又能够使微波介电陶瓷具有很高的致密性。
本发明还提供一种微波介电陶瓷的制作方法，包括如下步骤：
分别煅烧主晶相和用于调整所述主晶相的微波介电特性的调质修饰相，所述主晶相的烧结温度高于所述调质修饰相的烧结温度；
将所述主晶相和所述调质修饰相按比例混合得到混合物；
对所述混合物在温度t下进行烧结，得到所述微波介电陶瓷；
所述温度t介于所述调质修饰相的烧结温度和所述主晶相的烧结温度之间，所述调质修饰相包裹在所述主晶相的外表面。
优选地，在对所述混合物进行烧结之前，还包括如下步骤：将所述混合物经喷雾造粒或密炼制程的方式制成陶瓷注塑烧结所需的喂料，将所述喂料通过注塑成型的方式制成生胚，对所述生胚进行脱脂、烧结。
进一步优选地，所述主晶相的材料结构为钙钛矿结构，所述钙钛矿结构的所述主晶相由A粉体及TiO2粉体按摩尔比1:1经球磨混合后，在950℃~1300℃煅烧而成，所述A粉体为CaCO3粉体、MgO粉体、BaCO3粉体中的任意一种或其混合物；
或，所述主晶相的材料结构为类钙钛矿结构，所述类钙钛矿结构的所述主晶相由B粉体及TiO2粉体按摩尔比1:4经球磨混合后，在1000℃~1350℃煅烧而成，所述B粉体为BaCO3 粉体、MgO粉体、SrCO3粉体中的任意一种或其混合物；
或，所述主晶相的材料结构为尖晶石结构，所述尖晶石结构的所述主晶相由C粉体及TiO2粉体按摩尔比1:1经球磨混合后，在1000℃~1300℃煅烧而成，所述C粉体为MgO粉体、SrCO3粉体、CaCO3粉体、BaCO3粉体中的任意一种或其混合物；
或，所述主晶相的材料结构为层状钙钛矿结构，所述层状钙钛矿结构的所述主晶相由D粉体及E粉体按摩尔比1:2经球磨混合后，在1100℃~1400℃煅烧而成，所述D粉体为La2O3粉体、Y2O3粉体、Nd2O3粉体中的任意一种或其混合物，所述E粉体为TiO2粉体、ZrO2粉体、Nb2O5粉体中的任意一种或其混合物。
优选地，所述调质修饰相的成分为Bi4Ti3O12、Bi2Ti4O11、Bi12TiO20、Bi2Ti2O7、Bi2MoO6、Bi2Mo2O9、Bi2VO4、BiNbO4、ZnTiO3、Li3AlB2O6中的任意一种或其混合物。
进一步优选地，所述混合物在制成所述喂料时添加有高分子粘结剂，所述脱脂用于脱去所述高分子粘结剂。
进一步优选地，所述高分子粘结剂包括聚甲醛高分子粘结剂。
本发明提供的微波介电陶瓷的制作方法，通过分别煅烧主晶相和用于调整所述主晶相的微波介电特性的调质修饰相，将主晶相和调质修饰相按比例混合得到混合物，对混合物在调质修饰相的烧结温度和主晶相的烧结温度之间的温度下进行烧结，得到调质修饰相包裹在主晶相的外表面微波介电陶瓷，该方法降低了最终的烧结温度，降低了能耗和成本，同时，还避免了最终烧结时主晶相发生反应产生不良相的现象，使制成的微波介电陶瓷微波介电性能更加稳定。
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围，凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。
Claims (10)
1.一种微波介电陶瓷，由若干微观单元构成，所述微观单元包括：
主晶相；
调质修饰相，所述调质修饰相用于调整所述主晶相的微波介电特性；
其特征在于：
所述调质修饰相包裹在所述主晶相的外表面。
2.根据权利要求1所述的微波介电陶瓷，其特征在于，所述主晶相的内部不含有所述调质修饰相。
3.根据权利要求1或2中任意一项权利要求所述的微波介电陶瓷，其特征在于，所述主晶相的材料结构包括钙钛矿结构、类钙钛矿结构、钨青铜结构、尖晶石结构、层状钙钛矿结构中的任意一种；所述钙钛矿结构的成分为CaTiO3、MgTiO3 、BaTiO3中的任意一种或其混合物，所述类钙钛矿结构的成分为BaTi4O9、MgTi4O9、SrTi4O9中的任意一种或其混合物，所述钨青铜结构的成分为Ba5LnMNb9O30，所述尖晶石结构的成分为MgAl2O3、SrAl2O3、CaAl2O3、BaAl2O3中的任意一种或其混合物，所述层状钙钛矿结构的成分为La2Ti2O7、Y2Ti2O7、Nd2Ti2O7、La2Zr2O7、Y2Zr2O7、Nd2Zr2O7、La2Nb4O13、Y2Nb4O13、Nd2Nb4O13中的任意一种或其混合物。
4.根据权利要求1或2中任意一项权利要求所述的微波介电陶瓷，其特征在于，所述调质修饰相的成分为Bi4Ti3O12、Bi2Ti4O11、Bi12TiO20、Bi2Ti2O7、Bi2MoO6、Bi2Mo2O9、BiVO4、BiNbO4、ZnTiO3、Li3AlB2O6中的任意一种或其混合物。
5.一种微波介电陶瓷的制作方法，其特征在于，包括如下步骤：
分别煅烧主晶相和用于调整所述主晶相的微波介电特性的调质修饰相，所述主晶相的烧结温度高于所述调质修饰相的烧结温度；
将所述主晶相和所述调质修饰相按比例混合得到混合物；
对所述混合物在温度t下进行烧结，得到所述微波介电陶瓷；
其特征在于：
所述温度t介于所述调质修饰相的烧结温度和所述主晶相的烧结温度之间，使得所述调质修饰相熔化后包裹在所述主晶相的外表面。
6.根据权利要求5所述的微波介电陶瓷的制作方法，其特征在于，在对所述混合物进行烧结之前，还包括如下步骤：将所述混合物经喷雾造粒或密炼制程的方式制成陶瓷注塑烧结所需的喂料，将所述喂料通过注塑成型的方式制成生胚，对所述生胚进行脱脂、烧结。
7.根据权利要求5或6中任意一项权利要求所述的微波介电陶瓷的制作方法，其特征在于，
所述主晶相的材料结构为钙钛矿结构，所述钙钛矿结构的所述主晶相由A粉体及TiO2粉体按摩尔比1:1经球磨混合后，在950℃~1300℃煅烧而成，所述A粉体为CaCO3粉体、MgO粉体、BaCO3粉体中的任意一种或其混合物；
或，所述主晶相的材料结构为类钙钛矿结构，所述类钙钛矿结构的所述主晶相由B粉体及TiO2粉体按摩尔比1:4经球磨混合后，在1000℃~1350℃煅烧而成，所述B粉体为BaCO3 粉体、MgO粉体、SrCO3粉体中的任意一种或其混合物；
或，所述主晶相的材料结构为尖晶石结构，所述尖晶石结构的所述主晶相由C粉体及TiO2粉体按摩尔比1:1经球磨混合后，在1000℃~1300℃煅烧而成，所述C粉体为MgO粉体、SrCO3粉体、CaCO3粉体、BaCO3粉体中的任意一种或其混合物；
或，所述主晶相的材料结构为层状钙钛矿结构，所述层状钙钛矿结构的所述主晶相由D粉体及E粉体按摩尔比1:2经球磨混合后，在1100℃~1400℃煅烧而成，所述D粉体为La2O3粉体、Y2O3粉体、Nd2O3粉体中的任意一种或其混合物，所述E粉体为TiO2粉体、ZrO2粉体、Nb2O5粉体中的任意一种或其混合物。
8.根据权利要求5所述的微波介电陶瓷的制作方法，其特征在于，所述调质修饰相的成分为Bi4Ti3O12、Bi2Ti4O11、Bi12TiO20、Bi2Ti2O7、Bi2MoO6、Bi2Mo2O9、Bi2VO4、BiNbO4、ZnTiO3、Li3AlB2O6中的任意一种或其混合物。
9.根据权利要求6所述的微波介电陶瓷的制作方法，其特征在于，所述混合物在制成所述喂料时添加有高分子粘结剂，所述脱脂用于脱去所述高分子粘结剂。
10.根据权利要求9所述的微波介电陶瓷的制作方法，其特征在于，所述高分子粘结剂包括聚甲醛高分子粘结剂。
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