CN114644516A - 一种低损耗yig材料及其制备方法 - Google Patents

一种低损耗yig材料及其制备方法 Download PDF

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CN114644516A
CN114644516A CN202210284071.3A CN202210284071A CN114644516A CN 114644516 A CN114644516 A CN 114644516A CN 202210284071 A CN202210284071 A CN 202210284071A CN 114644516 A CN114644516 A CN 114644516A
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yig
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刘颖力
汪鑫
殷齐声
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University of Electronic Science and Technology of China
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Abstract

本发明提供一种低损耗的YIG材料及制备方法，材料结构式为Y2.7Ca0.3Fe(4.7‑x)Sn0.3O12，其中，0≤x≤0.325。制备方法包括以下步骤：(1)预烧料的制备：(2)二次球磨；(3)成型，烧结：1.本发明采用Sn4+离子取代八面体位的Fe3+以降低各向异性常数和铁磁共振线宽。同时，对于缺铁量设置梯度，以降低八面体(a位)和四面体(d位)间的铁离子之间的电子转移，从而降低材料的介电损耗。最终得到了低成本样品且其铁磁共振线宽为127Oe，介电常数为15.6，介电损耗正切为4×10‑4，本发明通过Sn4+离子取代八面体位Fe3+离子，增大铁氧体材料的分子磁矩，得到YIG样品饱和磁化强度为1865Gs。

Description

一种低损耗YIG材料及其制备方法
技术领域
本发明属于电子陶瓷材料技术领域，具体涉及一种低介电损耗、窄铁磁共振线宽、高饱和磁化强度的YIG铁氧体材料及其制备方法。
背景技术
微波铁氧体期间在雷达、微波通讯、人造卫星及医疗设备等领域应用十分广泛。伴随着电子系统向小型集成化、多功能化、高频化方向发展，石榴石型微波铁氧体材料由于其具有的很窄的铁磁共振线宽、低的介电损耗以及小的磁晶各向异性等优良性能，目前在微波铁氧体器件的应用中占有统治地位。
有关YIG铁氧体材料的研究报道：公开号为CN 102976740 A的专利申请公开了一种窄线宽高介电常数石榴石微波铁氧体制造方法，采用In3+、Sn4+、Ti4+等离子联合取代八面体位Fe3+和用Bi3+取代十二面体位的Y3+的方法，制得了饱和磁化强度为1608Gs，铁磁共振线宽10Oe,介电常数14.5，介电损耗0.7×10-4，居里温度大于225℃的样品。该方法缺点在于掺杂离子太多且部分离子成本太高，并且样品的饱和磁化强度偏低。公开号为CN 106747397A的专利申请公开了一种YIG材料及其制备方法，采用Sn4+离子取代Fe3+离子，同时加入高活性纳米掺杂剂，制成了铁磁共振线宽26.26Oe,介电常数14.8，饱和磁化强度1960Gs的样品。该制备方法对于工艺的要求较高，同时需要添加纳米级BaTiO3，掺杂配比也较难把握。公开号为CN 112898008 A,发明名称“一种低损耗YIG铁氧体及其制备方法”的专利申请，公开了一种低损耗、窄线宽、高居里温度的YIG铁氧体材料及制备方法，该方法主要的采用Ti4+离子取代Fe3+离子以增加分子磁矩，制得了饱和磁化强度为1960Gs，铁磁共振线宽26Oe，居里温度251℃，介电常数14.6，介电损耗4×10-4。该制备方法是基于固定缺铁量，改变掺杂量和温度设置了3组实施例。
综上所述，为了满足新一代微波铁氧体器件对于材料的要求，制备出的YIG材料需要在降低原料成本的前提下，获得较低铁磁共振线宽与介电损耗，同时保持较高饱和磁化强度。成分简单、成本低廉、性能优良的铁氧体材料具有广阔的市场前景。
发明内容
本发明的目的在于解决现有的YIG铁氧体材料存在的铁磁共振线宽大，介电损耗高或者线宽小但是原材料成本过高等问题，提出一种具有小线宽、低介电损耗、高饱和磁化强度、原材料廉价易得、工艺简单易复制的微波铁氧体材料及其制备方法。
为实现上述发明目的，本发明技术方案如下：
一种低损耗的YIG材料，材料结构式为Y2.7Ca0.3Fe(4.7-x)Sn0.3O12，其中，0≤x≤0.325。
作为优选方式，采用Sn4+离子取代八面体位的Fe3+以降低各向异性常数和铁磁共振线宽，同时，缺铁以降低八面体a位和四面体d位间的铁离子之间的电子转移，从而控制材料的介电损耗。
本发明还提供一种低损耗YIG材料的制备方法，包括以下步骤：
(1)步骤1、预烧料的制备：
(1.1)以氧化铁、氧化钙、氧化钇、氧化锡为原料，按照Y2.7Ca0.3Fe(4.7-x)Sn0.3O12、0≤x≤0.325的比例称取原料，然后置于尼龙罐中以去离子水为介质一次球磨6-9h；
(1.2)将步骤1.1得到的一次球磨料烘干、过筛后，在1200℃下预烧4-5h，随后随炉冷却至室温；
(2)步骤2、二次球磨：
将步骤1得到的预烧料置于尼龙罐中加入去离子水进行二次球磨6-8h，球磨完成后烘干；
(3)步骤3、成型，烧结：
(3.1)将步骤2得到的二次球磨料过筛后，加入10wt％的聚乙烯醇造粒，然后于10MPa压力下压制成型；
(3.2)将步骤3.1得到的样品置于烧结炉，先在1℃/min的升温速率下达到300℃，在300℃温度下保温2h，再在2℃/min的升温速率下达到1400℃，并保温5h，随后以2℃/min的降温速率下降到1200℃，最后随炉自然冷却至室温取出，即可得到所述YIG材料。
作为优选方式，所述步骤(1.1)中一次球磨的球磨时间为6h。
作为优选方式，所述步骤(1.2)中预烧温度为1200℃，保温时间为4h。
本发明的有益效果为：
1.本发明采用Sn4+离子取代八面体位的Fe3+以降低各向异性常数和铁磁共振线宽。同时，对于缺铁量设置梯度，以降低八面体(a位)和四面体(d位)间的铁离子之间的电子转移，从而降低材料的介电损耗。最终得到了低成本样品且其铁磁共振线宽为127Oe，介电常数为15.6，介电损耗正切为4×10-4。
2.本发明通过Sn4+离子取代八面体位Fe3+离子，增大铁氧体材料的分子磁矩，得到YIG样品饱和磁化强度为1865Gs。
附图说明
图1是本发明实施例磁化曲线图；
具体实施方式
以下通过特定的具体实例说明本发明的实施方式，本领域技术人员可由本说明书所揭露的内容轻易地了解本发明的其他优点与功效。本发明还可以通过另外不同的具体实施方式加以实施或应用，本说明书中的各项细节也可以基于不同观点与应用，在没有背离本发明的精神下进行各种修饰或改变。
一种低损耗的YIG材料，材料结构式为Y2.7Ca0.3Fe(4.7-x)Sn0.3O12，其中，0≤x≤0.325。
采用Sn4+离子取代八面体位的Fe3+以降低各向异性常数和铁磁共振线宽，同时，缺铁以降低八面体a位和四面体d位间的铁离子之间的电子转移，从而控制材料的介电损耗。
实施例提供一种低损耗YIG材料的制备方法，包括以下步骤：
(1)步骤1、预烧料的制备：
(1.1)以氧化铁、氧化钙、氧化钇、氧化锡为原料，按照Y2.7Ca0.3Fe(4.7-x)Sn0.3O12、0≤x≤0.325的比例称取原料，然后置于尼龙罐中以去离子水为介质一次球磨6-9h；优选的，所述步骤(1.1)中一次球磨的球磨时间为6h。
(1.2)将步骤1.1得到的一次球磨料烘干、过筛后，在1200℃下预烧4-5h，随后随炉冷却至室温；优选的，保温时间为4h。
(2)步骤2、二次球磨：
将步骤1得到的预烧料置于尼龙罐中加入去离子水进行二次球磨6-8h，球磨完成后烘干；
(3)步骤3、成型，烧结：
(3.1)将步骤2得到的二次球磨料过筛后，加入10wt％的聚乙烯醇造粒，然后于10MPa压力下压制成型；
(3.2)将步骤3.1得到的样品置于烧结炉，先在1℃/min的升温速率下达到300℃，在300℃温度下保温2h，再在2℃/min的升温速率下达到1400℃，并保温5h，随后以2℃/min的降温速率下降到1200℃，最后随炉自然冷却至室温取出，即可得到所述YIG材料。
(4)步骤4、测试
将步骤3所得样品进行性能测试。
采用阿基米德排水法测量样品表观密度d。
使用X射线衍射仪分析样品相成分。
采用SEM观察样品断面微观形貌。
使用VSM测量静态磁参数。
将样品制成直径1.6mm±0.01mm和长度22mm±0.5mm的圆柱，在谐振腔中测试获得材料介电损耗和介电常数。测试频率为9.3GHz
将样品制成直径为0.6mm-1.0mm的小球，采用波导谐振腔铁磁共振法测量材料铁磁共振线宽。
实施例1
本实施例提供一种低损耗YIG材料的制备方法，包括以下步骤：
(1)步骤1、预烧料的制备：
(1.1)以氧化铁、氧化钙、氧化钇、氧化锡为原料，按照Y2.7Ca0.3Fe(4.7-x)Sn0.3O12,x＝0的比例称取原料，然后置于尼龙罐中以去离子水为介质一次球磨6-9h；转速为260r/min；
(1.2)将步骤1.1得到的一次球磨料烘干、过筛后，在1200℃下预烧4-5h，随后随炉冷却至室温；
(2)步骤2、二次球磨：
将步骤1得到的预烧料置于尼龙罐中加入去离子水进行二次球磨6-8h，转速为260r/min，球磨完成后烘干；
(3)步骤3、成型，烧结：
(3.1)将步骤2得到的二次球磨料过筛后，加入10wt％的聚乙烯醇造粒，然后于10MPa压力下压制成型；
(3.2)将步骤3.1得到的样品置于烧结炉，先在1℃/min的升温速率下达到300℃，在300℃温度下保温2h，再在2℃/min的升温速率下达到1400℃，并保温5h，随后以2℃/min的降温速率下降到1200℃，最后随炉自然冷却至室温取出，即可得到所述YIG材料。
实施例1制备的到的YIG铁氧体材料的性能为：
饱和磁化强度1930Gs，介电常数16.1，介电损耗正切1.2×10-3，铁磁共振线宽47Oe。
实施例2
本实例与实施例1相比，区别在于：步骤1.1中的x＝0.25，其余步骤与实施例1相同。
实施例2制备的YIG铁氧体材料的性能为：
饱和磁化强度1874Gs，介电常数16，介电损耗正切8×10-4，铁磁共振线宽132Oe。
实施例3
本实例与实施例1相比，区别在于：步骤1.1中的x＝0.275，其余步骤与实施例1相同。
实施例3制备的YIG铁氧体材料的性能为：
饱和磁化强度1865Gs，介电常数15.6，介电损耗正切4×10-4，铁磁共振线宽127Oe。
实施例4
本实例与实施例1相比，区别在于：步骤1.1中的x＝0.3，其余步骤与实施例1相同。
实施例4制备的YIG铁氧体材料的性能为：
饱和磁化强度1790Gs，介电常数15.8，介电损耗正切5×10-4，铁磁共振线宽178Oe。
实施例5
本实例与实施例1相比，区别在于：步骤1.1中的x＝0.325，其余步骤与实施例1相同。
实施例4制备的YIG铁氧体材料的性能为：
饱和磁化强度1852Gs，介电常数15.5，介电损耗正切3×10-4，铁磁共振线宽168Oe。
对比例
本对比例与实施例1相比，区别在于：步骤1.1中按照Y3Fe5O12称取原料，其余步骤与实施例1相同。
对比例制备的YIG铁氧体材料的性能为：
饱和磁化强度1710Gs，介电常数14.9，介电损耗正切1.5×10-3，铁磁共振线宽79Oe。
表1对比例与实施例的样品性能对比
Figure BDA0003559350640000051
上述实施例仅例示性说明本发明的原理及其功效，而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下，对上述实施例进行修饰或改变。因此，凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变，仍应由本发明的权利要求所涵盖。

Claims (5)

1.一种低损耗YIG材料，其特征在于：材料结构式为Y2.7Ca0.3Fe(4.7-x)Sn0.3O12，其中，0≤x≤0.325。
2.根据权利要求1所述的一种低损耗YIG材料，其特征在于：采用Sn4+离子取代八面体位的Fe3+以降低各向异性常数和铁磁共振线宽，同时，缺铁以降低八面体a位和四面体d位间的铁离子之间的电子转移，从而控制材料的介电损耗。
3.权利要求1所述的一种低损耗YIG材料的制备方法，其特征在于包括以下步骤：
(1)步骤1、预烧料的制备：
(1.1)以氧化铁、氧化钙、氧化钇、氧化锡为原料，按照Y2.7Ca0.3Fe(4.7-x)Sn0.3O12、0≤x≤0.325的比例称取原料，然后置于尼龙罐中以去离子水为介质一次球磨6-9h；
(1.2)将步骤1.1得到的一次球磨料烘干、过筛后，在1200℃下预烧4-5h，随后随炉冷却至室温；
(2)步骤2、二次球磨：
将步骤1得到的预烧料置于尼龙罐中加入去离子水进行二次球磨6-8h，球磨完成后烘干；
(3)步骤3、成型，烧结：
(3.1)将步骤2得到的二次球磨料过筛后，加入10wt％的聚乙烯醇造粒，然后于10MPa压力下压制成型；
(3.2)将步骤3.1得到的样品置于烧结炉，先在1℃/min的升温速率下达到300℃，在300℃温度下保温2h，再在2℃/min的升温速率下达到1400℃，并保温5h，随后以2℃/min的降温速率下降到1200℃，最后随炉自然冷却至室温取出，即可得到所述YIG材料。
4.根据权利要求3所述的低损耗YIG材料的制备方法，其特征在于：所述步骤(1.1)中一次球磨的球磨时间为6h。
5.根据权利要求3所述的低损耗YIG材料的制备方法，其特征在于：所述步骤(1.2)中预烧温度为1200℃，保温时间为4h。
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