CN114702303A - 一种微波介质材料Ca3B2O6及其制备方法 - Google Patents

一种微波介质材料Ca3B2O6及其制备方法 Download PDF

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CN114702303A
CN114702303A CN202210343489.7A CN202210343489A CN114702303A CN 114702303 A CN114702303 A CN 114702303A CN 202210343489 A CN202210343489 A CN 202210343489A CN 114702303 A CN114702303 A CN 114702303A
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李波
郑宇欣
王童
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University of Electronic Science and Technology of China
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Abstract

本发明属于电子材料及其制造领域，提供了一种微波介质材料Ca3B2O6及其制备方法。本发明提供的微波介质材料的化学式为Ca3B2O6，微观结构为六方晶系的Ca3B2O6晶相，在1175～1250℃烧结具有优良的微波介电性能：介电常数为7.0～7.2、Q×f值为26000～33000GHz、谐振频率温度系数为‑128～‑90ppm/℃；该微波介质材料制备工艺简单、生产成本低，有利于实现工业化生产。

Description

一种微波介质材料Ca3B2O6及其制备方法
技术领域
本发明属于电子材料及其制造领域，具体提供一种微波介质材料Ca3B2O6及其制备方法。
背景技术
随着5G通信技术的高速发展，对微波器件的小型化和集成化提出了更高的要求，这离不开新型微波介质材料的开发和应用。硼酸盐微波介质材料具有烧结温度低、成本低等优点，具有良好的应用前景，近年来得到了较为广泛地研究，比如，Urban Dosler等人在文献“The synthesis and microwave dielectric properties of Mg3B2O6 and Mg2B2O5ceramics”中报道了Mg3B2O6微波介质材料，但是必须在1300℃烧结10小时，并且以2℃/min的降温速率耗时很长，导致其制备周期长，成为限制其工业化生产的瓶颈。
基于此背景，本发明提供一种微波介质材料Ca3B2O6及其制备方法。
发明内容
本发明提供一种微波介质材料Ca3B2O6及其制备方法，具体技术方案为：
步骤1：根据化学式Ca3B2O6中B与Ca的摩尔比，使用H3BO3、Ca(OH)2配料；
步骤2：按照原料：酒精：锆球＝1:1.5:5的质量比混合，置于球磨罐中球磨7小时，球磨出料，然后料浆置于烘箱中于60～70℃烘干；
步骤3：将干燥粉体过筛后，为防止B挥发，置于加盖的坩埚中800℃预烧3小时，获得主晶相为Ca3B2O6的预烧料；
步骤4：按照预烧料：酒精：锆球为1:1:5的质量比，置于球磨罐中球磨7小时，球磨后出料，然后料浆置于烘箱中于60～70℃烘干；
步骤5：将干燥粉体用50wt％丙烯酸造粒，并于10MPa下压制成生坯；
步骤6：将生坯在烧结炉中于450℃保温2～3小时，于1175～1250℃烧结5小时，得到所述的微波介质材料。
本发明的有益效果在于：
本发明提供了一种微波介质材料Ca3B2O6，其烧结温度为1175～1250℃，介电常数为7.0～7.2，Q×f值为26000～33000GHz，谐振频率温度系数为-128～-90ppm/℃。该微波介质材料微观结构致密、晶粒生长均匀、无第二相产生。
本发明提供了微波介质材料Ca3B2O6的制备工艺，其关键步骤在于，将过筛粉体置于加盖的坩埚中预烧，有效的防止高温下B挥发导致的B不足，从而生成第二相影响介电性能的情况。并且其制备工艺简单、周期短，便于批量化生产。
附图说明
图1为实施例3中微波介质材料的XRD图。
图2为实施例3中微波介质材料的SEM图。
具体实施方案
下面结合附图和实施例对本发明做进一步详细说明。
本发明具体提供4个实施例，其制备方法包括以下步骤：
步骤1：根据化学式Ca3B2O6中B与Ca的摩尔比，使用H3BO3、Ca(OH)2配料；
步骤2：按照原料：酒精：锆球＝1:1.5:5的质量比混合，置于球磨罐中球磨7小时，球磨出料，然后料浆置于烘箱中于60～70℃烘干；
步骤3：将干燥粉体过筛后，为防止B挥发，置于加盖的坩埚中800℃预烧3小时，获得主晶相为Ca3B2O6的预烧料；
步骤4：按照预烧料：酒精：锆球为1:1:5的质量比，置于球磨罐中球磨7小时，球磨后出料，然后料浆置于烘箱中于60～70℃烘干；
步骤5：将干燥粉体用50wt％丙烯酸造粒，并于10MPa下压制成生坯；
步骤6：将生坯在烧结炉中于450℃保温2～3小时，于1175～1250℃烧结5小时，得到所述的微波介质材料。
每个实施例的制备工艺参数及微波介电性能如下表所示：
编号 化学组成 烧结温度 烧结时长 ε<sub>r</sub> Q×f值 τ<sub>f</sub>
实施例1 Ca<sub>3</sub>B<sub>2</sub>O<sub>6</sub> 1175 5 7.09 26305 -127.54
实施例2 Ca<sub>3</sub>B<sub>2</sub>O<sub>6</sub> 1200 5 7.16 29028 -90.21
实施例3 Ca<sub>3</sub>B<sub>2</sub>O<sub>6</sub> 1225 5 7.07 32877 -98.19
实施例4 Ca<sub>3</sub>B<sub>2</sub>O<sub>6</sub> 1250 5 7.01 32166 -105.03
由上表可见，本发明提供微波介质材料Ca3B2O6，其在1175～1250℃烧结温度下拥有优良的微波介电性能：介电常数为7.0～7.2、Q×f值为26000～33000GHz、谐振频率温度系数为-128～-90ppm/℃，符合微波介质材料的应用需求。另外，实施例3制备得微波介质材料C a3B2O6的XRD、SEM如图1、图2所示，由图可见，XRD衍射图谱的特征峰与PDF#70-0868匹配完好，表明所制介质材料为单一晶相的Ca3B2O6，由SEM结果可知介质材料微观结构致密、气孔率小，从而获得低介电损耗。
以上所述，仅为本发明的具体实施方案，本说明书中所公开的任一特征，除非特别叙述，均可被其他等效或具有类似目的的替代特征加以替换；所公开的所有特征、或所有方法或过程中的步骤，除了互相排斥的特征和/或步骤以外，均可以任何方式组合。

Claims (3)

1.一种微波介质材料，其特征在于，所述微波介质材料的化学式为Ca3B2O6。
2.按权利要求1所述微波介质材料，其特征在于，所述微波介质材料的主晶相为Ca3B2O6，属于六方晶系。
3.按权利要求1所述微波介质材料及其制备方法，其特征在于，包括以下步骤：
步骤1：根据化学式Ca3B2O6中B与Ca的摩尔比，使用H3BO3、Ca(OH)2配料；
步骤2：按照原料：酒精：锆球＝1:1.5:5的质量比混合，置于球磨罐中球磨7小时，球磨出料，然后料浆置于烘箱中于60～70℃烘干；
步骤3：将干燥粉体过筛后，为防止B挥发，置于加盖的坩埚中800℃预烧3小时，获得主晶相为Ca3B2O6的预烧料；
步骤4：按照预烧料：酒精：锆球为1:1:5的质量比，置于球磨罐中球磨7小时，球磨后出料，然后料浆置于烘箱中于60～70℃烘干；
步骤5：将干燥粉体用50wt％丙烯酸造粒，并于10MPa下压制成生坯；
步骤6：将生坯在烧结炉中于450℃保温2～3小时，于1175～1250℃烧结5小时，得到所述的微波介质材料。
CN202210343489.7A 2022-03-31 2022-03-31 一种微波介质材料Ca3B2O6及其制备方法 Pending CN114702303A (zh)

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CN116199498B (zh) * 2023-02-28 2023-10-20 齐鲁工业大学(山东省科学院) 一种低介电常数硼酸盐微波介质陶瓷及其冷烧结制备方法

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Application publication date: 20220705