CN116730717A - 高功率、低损耗石榴石铁氧体及其制备方法 - Google Patents

高功率、低损耗石榴石铁氧体及其制备方法 Download PDF

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CN116730717A
CN116730717A CN202310602858.4A CN202310602858A CN116730717A CN 116730717 A CN116730717 A CN 116730717A CN 202310602858 A CN202310602858 A CN 202310602858A CN 116730717 A CN116730717 A CN 116730717A
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garnet ferrite
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燕周民
李慧琴
张静
张元松
褚涛
王渝
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Guizhou Zhenhua Hongyun Electronics Co ltd
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Abstract

本发明公开了一种高功率、低损耗石榴石铁氧体及其制备方法，属于铁氧体及其制备方法。本发明提供的石榴石铁氧体化学式为Y3‑x‑y‑ a Ca x Gd y Dy a Sn x In b Fe5‑x‑b‑δ O12，x=0.2～0.5、y=0～1.4、a=0～0.1、b=0～0.3、缺铁量δ=0.01～0.04。本发明提供的制备方法是按化学式配比称取Y2O3、Fe2O3、CaCO3、Gd2O3、Dy2O3、In2O3、SnO2，混合后球磨，烘干粉碎后预烧，预烧料加入Bi2O3、球磨，二次球磨料中加入PVA、模压成生坯，将生坯加热至1150～1250℃，然后按快速升降温方法进行热处理。本发明提供的石榴石铁氧体材料具有低铁磁共振线宽、低介电损耗、高自旋波线宽等优异特性。

Description

高功率、低损耗石榴石铁氧体及其制备方法
技术领域
本发明涉及一种铁氧体及其制备方法，尤其涉及一种高功率、低损耗石榴石铁氧体及其制备方法；属于电子材料技术领域。
背景技术
环行器/隔离器作为5G基站及相控阵雷达系统的关键部件，是系统天线大量收发单元中不可或缺的组成部分，因此环行器/隔离器在整个5G基站及雷达系统中有着举足轻重的作用。而微波铁氧体材料是上述器件的核心，器件的带宽、插入损耗、隔离度以及高功率承受能力，在很大程度上取决于微波铁氧体材料的性能。（见文献1韩志全.微波铁氧体材料近期进展述评[J].磁性材料及器件，2010，41（4）：5-13）。无论是5G通信要求的小型化、高功率器件，还是相控阵雷达需求的超视距要求，都促使材料往更高的功率和更低的损耗方向发展。
微波铁氧体材料按晶体结构可分为石榴石型、尖晶石型和磁铅石型。石榴石相较于其它两种铁氧体具有最低的铁磁共振线宽(ΔH)和介电损耗(tanδ ε )。目前对石榴石型铁氧体材料的研究主要集中在低损耗和大功率两个方向（见文献2穆祯宗.微波铁氧体材料的现状与发展[J].中国新通信，2018，020（005）：244-245.）。
关于高功率、低损耗石榴石铁氧体材料及制造方法的专利文献已有一些，如中国专利CN105347782B采用Sm3+、Gd3+、In3+、Sn4+、V5+、Ti4+、Mn2+等多种离子取代，以达到提高自旋波线宽、提高介电常数、降低铁磁共振线宽、降低介电损耗等目的，其ΔH在40～70Oe范围，但缺乏ΔH k 数据。另一中国专利CN101591167提供了一种高功率、低损耗石榴石铁氧体材料的制备方法，采用Bi3+、Ge4+、In3+、Sn4+、Sn4+、Ti4+对石榴石铁氧体进行离子取代，其铁氧体4πM s 约为250～600Gs，ΔH约为15～30Oe，tanδ ε 约为（0.5～1.2）×10-4，但同样缺乏ΔH k 数据。长期以来，关于低损耗或高功率石榴石铁氧体材料的研究虽已经取得丰硕的成果，但同时兼具低损耗与高功率特性的石榴石铁氧体材料却鲜有报道。
发明内容
针对现有技术中存在的上述缺陷，本发明旨在提供一种具有高功率、低损耗石榴石铁氧体；本发明的另一个目的是提供一种制备该石榴石铁氧体的方法。
为了实现上述目的，本发明所提供的石榴石铁氧体的化学式为：Y3-x-y- a Ca x Gd y Dy a Sn x In b Fe5-x-b-δ O12，其中，x=0.2～0.5、y=0～1.4、a=0～0.1、b=0～0.3、缺铁量δ=0.01～0.04。
本发明所提供的制备石榴石铁氧体的方法如下：
1）按化学式Y3-x-y-a Ca x Gd y Dy a Sn x In b Fe5-x-b-δ O12称取原料Y2O3、Fe2O3、CaCO3、Gd2O3、Dy2O3、In2O3、SnO2，该化学式中的x=0.2～0.5、y=0～1.4、a=0～0.1、b=0～0.3、δ=0.01～0.04、δ为缺铁量；
2）将上述各原料混合后球磨4～8小时，得一次磨料；
3）将所述一次磨料烘干、粉碎、过筛，1150～1250℃温度预烧2～4h，得预烧料；
4）将所述预烧料粉碎、过筛后加入0.1～0.3wt% Bi2O3，球磨12～18h，控制出料粒径为0.4～1.2μm，得到二次磨料；
5）将所述二次磨料烘干粉碎，加入6～12wt% PVA，混匀造粒、模压成生坯；
6）将所述生坯加热至1150～1250℃，先按4～8℃/min的速率升温至1350～1450℃、再按4～6℃/min的速率降温30℃，保温4～8小时，然后随炉冷却至室温。
与现有技术比较，本发明考虑到添加快弛豫杂质离子虽然可增大自旋波线宽，但同时会增大铁磁共振线宽和有效线宽；因此在微量掺杂稀土弛豫离子的同时，在预烧温度至烧结保温阶段还采用快速升降温处理工艺。
本发明在利用少量快弛豫离子取代的基础上（同时引入Gd3+、Dy3+、Sn4+、In3+取代），在烧结过程中采用快速升降温处理工艺，因此可使材料微观形貌致密，晶界明显，晶粒尺寸均匀、气孔减少、提高致密性；既增大了自旋波线宽，又大大降低了铁磁共振线宽。另外，本发明配方采用适量缺铁，可有效遏制Fe2+产生，从而可显著降低介电损耗。
经测试，本发明提供的石榴石铁氧体材料4πM s 为1000~1800Gs，ΔH<60Oe，ΔH k >12Oe，tanδ ε <2×10-4，兼顾了器件对材料低损耗与高功率的双重要求。
具体实施方式
下面结合具体的实施例对本发明作进一步说明：
实施例1 制备化学式为Y3-x-y-a Ca x Gd y Dy a Sn x In b Fe5-x-b-δ O12，x=0.3、y=0.2、a=0.01、b=0.1、缺铁量δ=0.02的石榴石铁氧体。方法如下：
1）按上述化学式配比称取原料Y2O3、Fe2O3、CaCO3、Gd2O3、Dy2O3、In2O3、SnO2；
2）将上述各原料混合后球磨（球磨介质为锆球）6小时，得一次磨料；
3）将所述一次磨料烘干、粉碎、过筛，1200℃温度预烧2h，得预烧料；
4）将所述预烧料粉碎、过筛后加入0.1wt% Bi2O3，球磨12h，控制出料粒径为0.4～1.2μm，得到二次磨料；
5）将所述二次磨料烘干粉碎，加入8wt% PVA，混匀造粒、模压成生坯；
6）将所述生坯加热至1200℃，先按6℃/min的速率升温至1450℃、再按5℃/min的速率降温30℃（即降至1420℃），保温6小时，然后随炉冷却至室温。
实施例2 制备化学式为Y3-x-y-a Ca x Gd y Dy a Sn x In b Fe5-x-b-δ O12，x=0.1、y=0.4、a=0.02、b=0.3、缺铁量δ=0.01的石榴石铁氧体。方法如下：
1）按上述化学式配比称取原料Y2O3、Fe2O3、CaCO3、Gd2O3、Dy2O3、In2O3、SnO2；
2）将上述各原料混合后球磨（球磨介质为锆球）4小时，得一次磨料；
3）将所述一次磨料烘干、粉碎、过筛，1220℃温度预烧4h，得预烧料；
4）将所述预烧料粉碎、过筛后加入0.2wt% Bi2O3，球磨18h，控制出料粒径为0.4～1.2μm，得到二次磨料；
5）将所述二次磨料烘干粉碎，加入6wt% PVA，混匀造粒、模压成生坯；
6）将所述生坯加热至1220℃，先按6℃/min的速率升温至1480℃、再按5℃/min的速率降温30℃（即降至1450℃），保温4小时，然后随炉冷却至室温。
实施例3 制备化学式为Y3-x-y-a Ca x Gd y Dy a Sn x In b Fe5-x-b-δ O12，x=0、y=0.2、a=0.01、b=0.4、缺铁量δ=0.02的石榴石铁氧体。方法如下：
1）按上述化学式配比称取原料Y2O3、Fe2O3、CaCO3、Gd2O3、Dy2O3、In2O3、SnO2；
2）将上述各原料混合后球磨（球磨介质为锆球）8小时，得一次磨料；
3）将所述一次磨料烘干、粉碎、过筛，1250℃温度预烧3h，得预烧料；
4）将所述预烧料粉碎、过筛后加入0.15wt% Bi2O3，球磨15h，控制出料粒径为0.4～1.2μm，得到二次磨料；
5）将所述二次磨料烘干粉碎，加入8wt% PVA，混匀造粒、模压成生坯；
6）将所述生坯加热至1150℃，先按6℃/min的速率升温至1380℃、再按5℃/min的速率降温30℃（即降至1350℃），保温8小时，然后随炉冷却至室温。
实施例4 制备化学式为Y3-x-y-a Ca x Gd y Dy a Sn x In b Fe5-x-b-δ O12，x=0.2、y=0.6、a=0.02、b=0.2、缺铁量δ=0.02的石榴石铁氧体。方法如下：
1）按上述化学式配比称取原料Y2O3、Fe2O3、CaCO3、Gd2O3、Dy2O3、In2O3、SnO2；
2）将上述各原料混合后球磨（球磨介质为锆球）7小时，得一次磨料；
3）将所述一次磨料烘干、粉碎、过筛，1250℃温度预烧3h，得预烧料；
4）将所述预烧料粉碎、过筛后加入0.3wt% Bi2O3，球磨13h，控制出料粒径为0.4～1.2μm，得到二次磨料；
5）将所述二次磨料烘干粉碎，加入10wt% PVA，混匀造粒、模压成生坯；
6）将所述生坯加热至1220℃，先按6℃/min的速率升温至1480℃、再按5℃/min的速率降温30℃（即降至1450℃），保温6小时，然后随炉冷却至室温。
以下是实施例1～4制备的石榴石铁氧体电磁性能参数。
表1：实施例1-4制备的石榴石铁氧体的电磁性能
实施例 4πM s （Gs） ΔH（Oe） ΔH k （Oe） tanδ ε （×10-4）
实施例1 1750 53 13 1.5
实施例2 1640 57 18 1.8
实施例3 1780 47 15 1.2
实施例4 1530 59 21 1.9

Claims (2)

1.一种高功率、低损耗石榴石铁氧体，其特征在于化学式为：Y3-x-y- a Ca x Gd y Dy a Sn x In b Fe5-x-b-δ O12，其中，x=0.2～0.5、y=0～1.4、a=0～0.1、b=0～0.3、缺铁量δ=0.01～0.04。
2.一种制备权力要求1所述的高功率、低损耗石榴石铁氧体的方法，其特征在于步骤如下：
1）按化学式Y3-x-y-a Ca x Gd y Dy a Sn x In b Fe5-x-b-δ O12称取原料Y2O3、Fe2O3、CaCO3、Gd2O3、Dy2O3、In2O3、SnO2，该化学式中的x=0.2～0.5、y=0～1.4、a=0～0.1、b=0～0.3、δ=0.01～0.04、δ为缺铁量；
2）将上述各原料混合后球磨4～8小时，得一次磨料；
3）将所述一次磨料烘干、粉碎、过筛，1150～1250℃温度预烧2～4h，得预烧料；
4）将所述预烧料粉碎、过筛后加入0.1～0.3wt% Bi2O3，球磨12～18h，控制出料粒径为0.4～1.2μm，得到二次磨料；
5）将所述二次磨料烘干粉碎，加入6～12wt% PVA，混匀造粒、模压成生坯；
6）将所述生坯加热至1150～1250℃，先按4～8℃/min的速率升温至1350～1450℃、再按4～6℃/min的速率降温30℃，保温4～8小时，然后随炉冷却至室温。
CN202310602858.4A 2023-05-26 2023-05-26 高功率、低损耗石榴石铁氧体及其制备方法 Pending CN116730717A (zh)

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