CN109133871B - 低成本、低密度、低烧结温度型微波介质材料及制备方法 - Google Patents

低成本、低密度、低烧结温度型微波介质材料及制备方法 Download PDF

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CN109133871B
CN109133871B CN201811059342.5A CN201811059342A CN109133871B CN 109133871 B CN109133871 B CN 109133871B CN 201811059342 A CN201811059342 A CN 201811059342A CN 109133871 B CN109133871 B CN 109133871B
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周焕福
卢承铭
陈秀丽
刘晓斌
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Abstract

本发明公开了一种低成本、低密度、低烧结温度型微波介质材料及制备方法。该微波介质材料的化学配比为：4NiO‑B2O3‑V2O5。(1)以纯度≥99%的NiO、B2O3和V2O5为原料，按4NiO‑B2O3‑V2O5的化学计量比进行称料；(2)将步骤(1)原料湿式球磨混合4h，以乙醇及氧化锆球为球磨介质，干燥后在550℃下预烧4h；(3)将预烧后的粉体进行二次球磨后添加5 wt%聚乙烯醇进行造粒，造粒后压制成型，最后将坯体排胶后在575~675℃下烧结4小时。本发明制备的微波介质陶瓷烧结温度低（≤900℃），并且低的介电常数（ε r ），较高的Q×f值以及低的τ f 值，表明具有很好商业应用前景。

Description

低成本、低密度、低烧结温度型微波介质材料及制备方法
技术领域
本发明属于电子陶瓷及其制造领域，涉及用在微波频段（300MHz~300GHz）使用的谐振器、滤波器、介质天线等电子元器件的介电陶瓷材料的制备方法。
背景技术
低温共烧陶瓷技术（LTCC，Low Temperature Co-fired Ceramics）以其优异的电学、机械、热学及工艺特性，已经成为电子器件模块化的主要技术之一。低温共烧陶瓷系统的烧结温度低，可用电阻率低的金属作为多层布线的导体材料，可以提高组装密度、信号传输速度，并且可内埋多层基板一次烧成的各种层式微波电子器件，因此广泛用在高速高密度互连多元陶瓷组件（MCM）之中。LTCC共烧技术具有组装密度高、介电损耗低、可用于高微波频段、可靠性高、与IC热匹配好等特点，因此有着极为广泛的应用前景。LTCC的关键技术要求微波介质材料在具有优良的微波介电性能的同时还应该具有低的烧结温度（≤960℃）并且能与Ag电极共烧兼容。而且高的烧结温度不仅增加了生产成本，还不能与Ag电极共烧，无法应用于LTCC器件上，影响了其在商业上大规模的应用。
近年来，随着微波元器件不断向低成本化、小型化以及轻量化方向的发展，要求微波介质材料具有优良的微波介电性能（高的Q×f值，适合的介电常数、低的τ f 值）的同时还要有低的生产成本、低的密度以及低的烧结温度。比如，目前报道了很多性能优异的微波介电材料Ba(Zn1/3Nb2/3)O3、Ba(Mg1/3Nb2/3)O3和Ba(Y1/2Ta1/2)O3等。它们高的烧结温度（>1100℃）、大的密度（>6g/cm3）以及较贵的生产原料限制了其在商业上的应用。因此，选用低价格的生产原料制备出低成本、低密度、低烧结温度的微波介质材料已经是尤为重要。
发明内容
本发明涉及的微波介质陶瓷材料的化学配比为：4NiO-B2O3-V2O5。
微波介质陶瓷材料的制备方法具体步骤为：
((1)以纯度≥99%的高纯粉NiO、B2O3和V2O5为原料，按4NiO-B2O3-V2O5的化学计量比进行称料。按照原料、氧化锆球和无水乙醇1：2：1的质量比向原料中加入氧化锆球和无水乙醇，球磨4h后，在110~120℃下快速烘干。将烘干粉料压制成圆柱体，放置在氧化铝坩埚内进行预烧，其温度为550℃，保温时间为4h，升温速率为5℃/min。
(2)将步骤(1)中得到的预烧体在研钵中进行初步研磨之后，按照粉体、氧化锆球与无水乙醇1：2：1的质量比放入到尼龙罐中球磨4h，并在110~120℃下烘干，向烘干后的粉体加入5 wt%聚乙烯醇（PVA）进行造粒，再将粉体压制成直径为12mm，厚度为6mm的小圆柱。最后，在550℃下排胶4h，其升温速率为1℃/min，并将排完胶的小圆柱分别在575~675℃下烧结4h，即得到所需的微波介质陶瓷。
本发明制备的微波介质陶瓷，其烧结温度较低（低至675℃），密度较小，微波性能优异（低的介电常数（εr），较高的Q×f值以及低的τ f 值），具有商业应用前景。
具体实施方式
实施例:
下表列出了5个不同烧结温度的实施例及其密度和微波介电性能（制备过程如上所述）。
Figure 666585DEST_PATH_IMAGE001

Claims (1)

1.一种低成本、低密度、低烧结温度型微波介质材料，其特征在于该微波介质陶瓷材料的化学配比为：4NiO-B2O3-V2O5；
所述微波介质陶瓷材料的制备方法具体步骤为：
(1)以纯度≥99%的高纯粉NiO、B2O3和V2O5为原料，按4NiO-B2O3-V2O5的化学计量比进行称料，按照原料、氧化锆球和无水乙醇1：2：1的质量比向原料中加入氧化锆球和无水乙醇，球磨4h后，在110~120℃下快速烘干，将烘干粉料压制成圆柱体，放置在氧化铝坩埚内进行预烧，其温度为550℃，保温时间为4h，升温速率为5℃/min；
(2)将步骤(1)中得到的预烧体在研钵中进行初步研磨之后，按照粉体、氧化锆球与无水乙醇1：2：1的质量比放入到尼龙罐中球磨4h，并在110~120℃下烘干，向烘干后的粉体加入5 wt%聚乙烯醇（PVA）进行造粒，再将粉体压制成直径为12mm，厚度为6mm的小圆柱，最后，在550℃下排胶4h，其升温速率为1℃/min，并将排完胶的小圆柱分别在575~675℃下烧结4h，即得到所需的微波介质陶瓷。
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CN101786875A (zh) * 2010-01-02 2010-07-28 桂林理工大学 低温烧结尖晶石结构微波介质陶瓷材料及制备方法
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CN102320825B (zh) * 2011-08-16 2013-04-10 广西新未来信息产业股份有限公司 一种低温烧结微波介质陶瓷及其烧结方法
CN106986641A (zh) * 2017-04-24 2017-07-28 桂林理工大学 一种含钒的硼酸盐超低介电常数微波介电陶瓷

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CN105236977A (zh) * 2015-10-18 2016-01-13 桂林理工大学 超低介电常数微波介电陶瓷La4VBO10及其制备方法
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