CN114477995B - 一种中饱和磁化强度功率型高介电常数石榴石材料及其制备方法 - Google Patents

一种中饱和磁化强度功率型高介电常数石榴石材料及其制备方法 Download PDF

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CN114477995B
CN114477995B CN202210164462.1A CN202210164462A CN114477995B CN 114477995 B CN114477995 B CN 114477995B CN 202210164462 A CN202210164462 A CN 202210164462A CN 114477995 B CN114477995 B CN 114477995B
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鲜聪
孔伟
黄小忠
任仕晶
廖杨
王殿杰
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CETC 9 Research Institute
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Abstract

本发明公开了一种中饱和磁化强度功率型高介电常数石榴石材料，属于微波铁氧体材料领域，其化学式组成为：BiaCabDycY3‑a‑b‑ cFe5‑d‑e‑f‑g‑h‑δZrdVeSnfIngSbhO12，其中1.0≤a≤1.7，1≤b≤2，0≤c≤0.2，0≤d≤0.7，0≤e≤0.7，0≤f≤0.3，0≤g≤0.2，0≤h≤0.1，δ为缺铁量，本发明还公开了其制备方法，本发明的铁氧体材料的介电常数为25～26，且具有中饱和磁化强度、较低的铁磁共振线宽和一定的自旋波线宽，这些性能不仅可以有效降低器件的体积和损耗，还可以使器件承受更高的功率，可用于小型化功率型微波器件中，尤其适用于雷达、5G通信等领域。

Description

一种中饱和磁化强度功率型高介电常数石榴石材料及其制备 方法
技术领域
本发明涉及微波铁氧体材料领域，尤其涉及一种中饱和磁化强度功率型高介电常数石榴石材料及其制备方法。
背景技术
由微波传输理论可知：微波铁氧体的介电常数ε越大，相应微波铁氧体器件尺寸就越小。传统的石榴石旋磁材料由于介电常数较低(其值约13～15)，大大限制了器件的小型化发展。通过极化离子掺杂，石榴石旋磁材料介电常数可以显著的提高，根据理论计算，用介电常数30的石榴石旋磁材料制备的器件尺寸可缩小到原来尺寸的70％以下，这可以实现微波器件的小型化。因此研究高介电常数旋磁材料及其应用技术对解决微波器件的小型化、集成化有着十分现实的意义。
上世纪就有人提出在钇铁石榴石中掺入高极化离子可以提高材料的介电常数。近几年也有许多专利报道了高介电常数钇铁石榴石材料的制备方法，如专利公开号为CN107417266A、CN104478425A、CN107034517A、CN111848149A、CN112390637A和CN112679204A等的中国专利申请。这些专利中材料的介电常数明显提高，并取得了不错的铁磁共振线宽性能，但鲜有自旋波线宽性能的研究。对于功率型铁氧体器件自旋波线宽是非常重要的参数，自旋波线宽越大器件所能承受的功率容量越大，但自旋波线宽越大的材料往往铁磁共振线宽越大，导致器件损耗恶化，因此在实际工程中功率型材料都是在自旋波线宽和铁磁共振线宽之间取平衡。
发明内容
本发明的目的，就在于提供一种中饱和磁化强度功率型高介电常数石榴石材料，以解决上述问题。
为了实现上述目的，本发明采用的技术方案是这样的：一种中饱和磁化强度功率型高介电常数石榴石材料，其化学式组成为：BiaCabDycY3-a-b-cFe5-d-e-f-g-h-δZrdVeSnfIngSbhO12，其中1.0≤a≤1.7，1≤b≤2，0≤c≤0.2，0≤d≤0.7，0≤e≤0.7，0≤f≤0.3，0≤g≤0.2，0≤h≤0.1，δ为缺铁量。
本发明提供的上述材料具有中饱和磁化强度、较高的介电常数、较低的铁磁共振线宽和一定的自旋波线宽，可满足一定功率微波铁氧体器件的应用。
本发明所采用的技术方案是：通过掺杂Zr4+、Sn4+、V5+、Sb5+、In3+、Ca2+等离子来调控材料的铁磁共振线宽和饱和磁化强度；通过Bi3+掺杂来调控材料的介电常数；通过掺杂Dy3+来调控材料的自旋波线宽。
本发明的目的之二，在于提供一种上述材料的制备方法，采用的技术方案为：
包括下述步骤：
(1)一次料的制备：按所述主要成分的含量称取原材料，加入溶剂进行球磨，球磨时间4～12h，然后过滤烘干过筛，在800～900℃进行预烧处理，冷却后，得到一次料；
(2)二次料的制备：将步骤(1)所得的一次料粉碎，加入溶剂球磨4～12h，过滤烘干后，得到二次料；
(3)造粒：将制备的二次料加入一定量的胶合剂，进行造粒过筛；
(4)成型：造粒好的细粉放入模具进行压制，压制压强为50MPa～250MPa，得到材料生坯
(5)烧结；将生坯装入空气气氛或氧化气氛炉中进行烧结，即得样品。
作为优选的技术方案：步骤(a)中的原材料为分析纯，其化学式分别为Fe2O3、Bi2O3、CaCO3、ZrO2、Dy2O3、V2O5、SnO2、In2O3、Sb2O5、Y2O3。
作为优选的技术方案：步骤(1)中，球料比为4:1，球磨时间为4h。
作为优选的技术方案：步骤(1)中，所述球为氧化锆，所述溶剂为去离子水或酒精。
作为优选的技术方案：步骤(1)中，球磨时球料比例为3～4:1，料与溶剂比例为1:0.9～1.1，所述溶剂为去离子水
作为进一步优选的技术方案：步骤(2)中，料与溶剂的比例为1:1，球磨时间为4h。
步骤(1)、(3)中过筛时筛规格大小为20目～60目。
作为优选的技术方案：步骤(3)中，所述胶合剂为聚乙烯醇水溶液，浓度为5wt％～12wt％。
作为优选的技术方案：步骤(5)中，烧结温度为900℃～1100℃，保温6小时以上。
与现有技术相比，本发明的优点在于：本发明的铁氧体材料的介电常数为25～26，且具有中饱和磁化强度、较低的铁磁共振线宽和一定的自旋波线宽，这些性能不仅可以有效的降低器件的体积和损耗，还可以使器件承受更高的功率，可用于小型化功率型微波器件中，尤其适用于雷达、5G通信等领域。
具体实施方式
下面将对本发明作进一步说明。
实施例1：
一种中饱和磁化强度功率型高介电常数石榴石材料，按组成化学式BiaCabDycY3-a-b-cFe5-d-e-f-g-h-δZrdVeSnfIngSbhO12称取Fe2O3、Bi2O3、CaCO3、ZrO2、Dy2O3、V2O5、SnO2、In2O3、Sb2O5、Y2O3,其中a＝1.38，b＝1.615，c＝0.005，d＝0.45，e＝0.43，f＝0.1，g＝0.05，h＝0.1，δ＝0.05。
实施例2：
一种中饱和磁化强度功率型高介电常数石榴石材料，按组成化学式BiaCabDycY3-a-b-cFe5-d-e-f-g-h-δZrdVeSnfIngSbhO12称取Fe2O3、Bi2O3、CaCO3、ZrO2、Dy2O3、V2O5、SnO2、In2O3、Sb2O5、Y2O3,其中a＝1.38，b＝1.61，c＝0.01，d＝0.45，e＝0.43，f＝0.1，g＝0.05，h＝0.1，δ＝0.05。
实施例3：
一种中饱和磁化强度功率型高介电常数石榴石材料，按组成化学式BiaCabDycY3-a-b-cFe5-d-e-f-g-h-δZrdVeSnfIngSbhO12称取Fe2O3、Bi2O3、CaCO3、ZrO2、Dy2O3、V2O5、SnO2、In2O3、Sb2O5、Y2O3,其中a＝1.38，b＝1.6，c＝0.02，d＝0.45，e＝0.43，f＝0.1，g＝0.05，h＝0.1，δ＝0.05。
实施例4：
一种中饱和磁化强度功率型高介电常数石榴石材料，按组成化学式BiaCabDycY3-a-b-cFe5-d-e-f-g-h-δZrdVeSnfIngSbhO12称取Fe2O3、Bi2O3、CaCO3、ZrO2、Dy2O3、V2O5、SnO2、In2O3、Sb2O5、Y2O3,其中a＝1.38，b＝1.59，c＝0.03，d＝0.45，e＝0.43，f＝0.1，g＝0.05，h＝0.1，δ＝0.05。
制备方法：按照实施例1～4称取原材料，原材料都为分析纯；
一次料的制备：将称取好的原材料进行湿法球磨，球：料：稀释剂的比例为4:1:1,(球为氧化锆,稀释剂为去离子水或酒精)，湿法球磨4h，然后过滤烘干过筛，在860℃进行预烧处理，然后自然冷却；
二次料的制备：将制备好的一次敲碎，倒入球磨罐中，进行二次球磨，球：料：稀释剂的比例为4:1:0.8，湿法球磨4h，然后过滤烘干；
造粒：将二次料加入浓度为9wt％的聚乙烯醇水溶液，充分混合后过筛；
成型：将造粒后的颗粒放入模具进行压制，压制压力为100MPa，得到材料生坯；
烧结：将生坯装入空气气氛炉中进行烧结，烧结温度为1000℃左右，保温时间8小时后，自然冷却；
测试：将烧结出的样品进行饱和磁化强度、铁磁共振线宽、自旋波线宽和介电常数的测试，测试结果如表1所示；
表1:实施例1-4的铁氧体的性能
Figure GDA0003579299430000061
对上述性能数据进行分析：
与传统石榴石材料介电常数(其值约13～15)相比，本发明实施例1、2材料介电常数约为25-26，且兼顾较低的铁磁共振线宽(在25Oe以内)和一定的自旋波线宽，可满足工程化对材料损耗和功率的要求
与其它高介电常数石榴石材料相比，本发明实施例2材料介电常数为26.1，铁磁共振线宽为25Oe，且自旋波线宽为4.9Oe，在铁磁共振线宽增加不是很大的基础上增大了材料的自旋波线宽，使得实施例2可承受更高的功率。
对比实施例1-4，材料铁磁共振线宽和自旋波线宽依次明显增大，当实施例2时，材料铁磁共振线宽和自旋波线宽取得最优值。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (10)

1.一种中饱和磁化强度功率型高介电常数石榴石材料，其特征在于：其化学式组成为：
BiaCabDycY3-a-b-cFe5-d-e-f-g-h-δZrdVeSnfIngSbhO12，其中，a=1.38，1.59≤b≤1.615，0.005≤c≤0.03，d=0.45，e=0.43，f=0.1，g=0.05，h=0.1，δ为缺铁量。
2.权利要求1所述的中饱和磁化强度功率型高介电常数石榴石材料的制备方法，其特征在于，包括以下步骤：
（1）一次料的制备：按所述化学式组成称取原材料，加入溶剂进行球磨，球磨时间4～12h，然后过滤烘干过筛，在800～900 ℃进行预烧处理，冷却后，得到一次料；
（2）二次料的制备：将步骤（1）所得的一次料粉碎，加入溶剂球磨4～12 h，过滤烘干后，得到二次料；
（3）造粒：将制备的二次料加入胶合剂，进行造粒过筛；
（4）成型：造粒好的细粉放入模具进行压制，压制压强为50MPa～250MPa，得到材料生坯；
（5）烧结；将生坯装入空气气氛或氧化气氛炉中进行烧结，即得样品。
3.根据权利要求2所述的制备方法，其特征在于：步骤(1)中的原材料为分析纯，其化学式分别为Fe2O3、Bi2O3、CaCO3、ZrO2、Dy2O3、V2O5、SnO2、In2O3、Sb2O5、Y2O3。
4.根据权利要求2所述的制备方法，其特征在于：步骤（1）中，所述球为氧化锆，所述溶剂为去离子水或酒精。
5.根据权利要求2所述的制备方法，其特征在于：步骤（1）中，球磨时球料比例为3～4:1，料与溶剂比例为1: 0.9～1.1，所述溶剂为去离子水。
6.根据权利要求5所述的制备方法，其特征在于：步骤（1）中，球料比为4:1，球磨时间为4h。
7.根据权利要求2所述的制备方法，其特征在于：步骤（2）中，所述一次料与溶剂比例1:0.8～1。
8.根据权利要求7所述的制备方法，其特征在于：所述一次料与溶剂比例为1:1，球磨时间为4h。
9.根据权利要求2所述的制备方法，其特征在于：步骤(3)中，所述胶合剂为聚乙烯醇水溶液，浓度为5wt％～12wt％。
10.根据权利要求2所述的制备方法，其特征在于：步骤(5)中，烧结温度为900℃～1100℃，保温6小时以上。
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