CN107746269A - 低损耗功率旋磁材料及其制备方法 - Google Patents

低损耗功率旋磁材料及其制备方法 Download PDF

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CN107746269A
CN107746269A CN201711044624.3A CN201711044624A CN107746269A CN 107746269 A CN107746269 A CN 107746269A CN 201711044624 A CN201711044624 A CN 201711044624A CN 107746269 A CN107746269 A CN 107746269A
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熊飞
张伟
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SHENZHEN HUAYANG COMMUNICATION TECHNOLOGY Co Ltd
Shenzhen Huayang Technology Development Co Ltd
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Abstract

本发明涉及一种低损耗功率旋磁材料,包括以下重量份原料:Bi203 15‑20份、Y2O3 22‑26份、GeO2 1‑2.5份、CaCO3 2‑5份、Fe2O3 41‑47份、ZrO2 2‑5份、MnCO3 0.2‑1份和CaTiO3 6‑10份。本发明还涉及一种低损耗功率旋磁材料的制备方法。本发明的低损耗功率旋磁材料具有高磁矩、高居里温度、烧结温度低、能耗小及高介电常数高达30的优点。

Description

低损耗功率旋磁材料及其制备方法
技术领域
本发明涉及磁性材料技术,特别涉及一种低损耗功率旋磁材料及其制备方法。
背景技术
磁性材料从应用功能上可分为软磁材料、永磁材料、磁记录-矩磁材料和旋磁材料等种类,其中旋磁材料即为铁氧体材料。目前,随着通信技术飞速发展,环形器隔离器向着小型化、集成化发展。而现有铁氧体的介电常数在12-16之间,在低频环形器隔离器设计时器件尺寸偏大,无法满足小型化、集成化的需求;若提高铁氧体的介电常数到30,可以把隔离器环形器的尺寸缩小30%,达到小型化、集成化的需求。
发明内容
本发明所要解决的技术问题是:提供一种介电常数可达30的低损耗功率旋磁材料及其制备方法。
为了解决上述技术问题,本发明采用的技术方案为:
一种低损耗功率旋磁材料,包括以下重量份原料:Bi20315-20份、Y2O322-26份、GeO21-2.5份、CaCO32-5份、Fe2O341-47份、ZrO22-5份、MnCO30.2-1份和CaTiO36-10份。
本发明还提供一种低损耗功率旋磁材料的制备方法,包括以下步骤:
(1)将Bi203、Y2O3、GeO2、CaCO3、Fe2O3、ZrO2和MnCO3按照权利要求1-3任意一项所述的低损耗功率旋磁材料中的重量份比例进行混合,获得混合原料;
(2)将所述混合原料进行一次球磨,所述一次球磨中原料、水和钢球的重量比为1:1.2-1.5:4.3-4.7;
(3)将一次球磨后的料浆进行烘干,获得烘干料;
(4)将所述烘干料进行预烧,获得预烧料,所述预烧的温度为900-1000℃,然后将所述预烧料进行保温2-6h;
(5)将CaTiO3按照权利要求1-3任意一项所述的低损耗功率旋磁材料中的重量份比例与保温后的预烧料混合,然后进行二次球磨,所述二次球磨中原料、水和钢球的重量比为1:1.1-1.4:3.4-3.9;
(6)将二次球磨后的料浆依次进行烘干、造粒和成型,获得成型样品;
(7)将所述成型样品进行烧结,所述烧结的温度为1150-1250℃,烧结后进行保温6-10h,获得所述低损耗功率旋磁材料。
本发明的有益效果在于:
本发明制备的低损耗功率旋磁材料为一种具有高磁矩、高居里温度等优良性能的高介电常数铁氧体,同时还具有烧结温度低,能耗小的优点。本发明获得的低损耗功率旋磁材料4πMs为1800Gs,介电常数εr为30,通过组装用于频段851-894MHz环形器,插入损耗为0.24dB,隔离25dB,驻波25dB。
具体实施方式
为详细说明本发明的技术内容、所实现目的及效果,以下结合实施方式予以说明。
本发明最关键的构思在于:设计上述原料配比的低损耗功率旋磁材料。
本发明提供一种低损耗功率旋磁材料,包括以下重量份原料:Bi20315-20份、Y2O322-26份、GeO21-2.5份、CaCO32-5份、Fe2O341-47份、ZrO22-5份、MnCO30.2-1份和CaTiO36-10份。
本发明还提供一种低损耗功率旋磁材料的制备方法,包括以下步骤:
(1)将Bi203、Y2O3、GeO2、CaCO3、Fe2O3、ZrO2和MnCO3按照权利要求1-3任意一项所述的低损耗功率旋磁材料中的重量份比例进行混合,获得混合原料;
(2)将所述混合原料进行一次球磨,所述一次球磨中原料、水和钢球的重量比为1:1.2-1.5:4.3-4.7;
(3)将一次球磨后的料浆进行烘干,获得烘干料;
(4)将所述烘干料进行预烧,获得预烧料,所述预烧的温度为900-1000℃,然后将所述预烧料进行保温2-6h;
(5)将CaTiO3按照权利要求1-3任意一项所述的低损耗功率旋磁材料中的重量份比例与保温后的预烧料混合,然后进行二次球磨,所述二次球磨中原料、水和钢球的重量比为1:1.1-1.4:3.4-3.9;
(6)将二次球磨后的料浆依次进行烘干、造粒和成型,获得成型样品;
(7)将所述成型样品进行烧结,所述烧结的温度为1150-1250℃,烧结后进行保温6-10h,获得所述低损耗功率旋磁材料。
从上述描述可知,本发明的有益效果在于:
本发明制备的低损耗功率旋磁材料为一种具有高磁矩、高居里温度等优良性能的高介电常数铁氧体,同时还具有烧结温度低,能耗小的优点。本发明获得的低损耗功率旋磁材料4πMs为1800Gs,介电常数εr为30,通过组装用于频段851-894MHz环形器,插入损耗为0.24dB,隔离25dB,驻波25dB。
本发明的低损耗功率旋磁材料中:
进一步的,包括以下重量份原料:Bi20316-18份、Y2O323-25份、GeO2 1-2份、CaCO32-4份、Fe2O342-46份、ZrO22-4份、MnCO30.2-1份和CaTiO36-9份。
进一步的,包括以下重量份原料:Bi20317份、Y2O323份、GeO21.5份、CaCO33份、Fe2O345份、ZrO23份、MnCO30.5份和CaTiO37份。
由上述描述可知,上述配比均为优选的低损耗功率旋磁材料的原料组分配比设计,具有更好的高磁矩、高居里温度、烧结温度低及能耗小等优点。
本发明的实施例1为:
一种高介电常数旋磁材料,该旋磁材料由下列重量份的组分组成:Bi20317份、Y2O323份、GeO21.5份、CaC033份、Fe2O345份、ZrO23份、MnCO30.5份和CaTiO37份。生产该旋磁材料1000g,各组分的具体用量如下:Bi203170g、Y2O3240g、GeO215g、CaC0330g、Fe2O3440g、ZrO230g、MnCO35g和CaTiO370g。
上述的一种低损耗功率旋磁材料的制备方法,它包括下述步骤:
(1)配料:按照原料各组分的比例进行配料;
(2)一次球磨:按照重量比原料:水:钢球=1:1.3:4.5,具体用量依次为:1000g、1300g、4500g,球磨机转速为70r/Min,球磨时间为20h;
(3)出料烘干:将装有球磨好的料浆进行烘干,烘干温度为140℃,烘干时间为4h;
(4)预烧:将烘干后的料过40目标准分样筛,然后放入箱式电阻炉中预烧,预烧温度为950℃,保温4h;
(5)二次球磨:按照重量比原料:水:钢球=1:1.2:3.6,具体用量为:1000g、1200g和3600g,球磨机转速为100r/Min,球磨时间为34h;
(6)烘干造粒:将装有二次球磨好的料浆进行烘干,烘干温度为120℃,烘干时间为10h,加入浓度为10%、质量比为10%PVA的胶水造粒,过120目标准分样筛;
(7)成型:将过筛好、含水率为3.20%的粉料,进行样品压制,压制压力为6MPa;
(8)烧结:将压制好的样品进行烧结,烧结温度为1200℃,保温时间为8h。
实施例2
一种高介电常数旋磁材料,该旋磁材料由下列重量份的组分组成:Bi20316份、Y2O324份、GeO22份、CaC034份、Fe2O3 44份、ZrO2 3.8份、MnCO3 0.2份和CaTiO3 6份。生产该旋磁材料1000g,各组分的具体用量如下:Bi203 160g、Y2O3230g、GeO2 20g、CaC0340g、Fe2O3430g、ZrO238g、MnCO32g和CaTiO380g。
上述的一种低损耗功率旋磁材料的制备方法,它包括下述步骤:
(1)配料:按照原料各组分的比例进行配料;
(2)一次球磨:按照重量比原料:水:钢球=1:1.5:4.3,具体用量为:1000g、1500g和4300g,球磨机转速为60r/Min,球磨时间为22h;
(3)出料烘干:将装有球磨好的料浆进行烘干,烘干温度为160℃,烘干时间为6h;
(4)预烧:将烘干后的料过60目标准分样筛,然后放入箱式电阻炉中预烧,预烧温度为1000℃,保温2h;
(5)二次球磨:按照重量比原料:水:钢球=1:1.0:3.9,具体用量为:1000g、1000g和3900g,球磨机转速为97r/Min,球磨时间为36h;
(6)烘干造粒:将装有二次球磨好的料浆进行烘干,烘干温度为140℃,烘干时间为8h,加入浓度为11%、质量比为9%PVA的胶水造粒,过120目标准分样筛;
(7)成型:将过筛好、含水率为3.40%的粉料晾干,进行样品压制,压制压力为7MPa;
(8)烧结:将压制好的样品进行烧结,烧结温度为1150℃,保温时间为10h。
实施例3
一种高介电常数旋磁材料,该旋磁材料由下列重量份的组分组成:Bi20318份、Y2O322份,GeO2 1份,CaC032份,Fe2O3 46份,ZrO2 2份,MnCO31份,CaTiO38份。生产该旋磁材料1000g,各组分的具体用量如下:Bi203 170g、Y2O3240g、GeO2 10g、CaC0320g、Fe2O3460g、ZrO210g、MnCO310g和CaTiO360g。
上述的一种高介电常数旋磁材料的制备方法,它包括下述步骤:
(1)配料:按照原料各组分的比例进行配料;
(2)一次球磨:按照重量比原料:7C:钢球=1:1.2:4.7,具体用量为:1000g、1200g和4700g,球磨机转速为80r/Min,球磨时间为18h;
(3)出料烘干:将装有球磨好的料浆进行烘干,烘干温度为120℃,烘干时间为6h;
(4)预烧:将烘干后的料过60目标准分样筛,然后放入箱式电阻炉中预烧,预烧温度为900℃,保温6h;
(5)二次球磨:按照重量比原料:水:钢球=1:1.4:3.4,具体用量为:1000g、1400g和3400g,球磨机转速为103r/Min,球磨时间为36h;
(6)烘干造粒:将装有二次球磨好的料浆进行烘干,烘干温度为100℃,烘干时间为12h,加入浓度为9%、质量比为11%PVA的胶水造粒,过120目标准分样筛;
(7)成型:将过筛好、含水率为3.00%的粉料晾干,进行样品压制,压制压力为5MPa;
(8)烧结:将压制好的样品进行烧结,烧结温度为1250℃,保温时间为6h。
试验测试
将实施例1-3中所得的低损耗功率旋磁材料进行性能测试,对其4πMs、居里温度Tc、线宽△H、介电常数εr和介电损耗角正切Tanδ进行测试。结果如下表1。表1为低损耗功率旋磁材料的饱和磁化强度4πMs、居里温度Tc、线宽△H、介电常数εr和介电损耗角正切Tanδ性能的测试结果表。
表1
性能 测试结果
4πMs(Gs) 1800
Tc(℃) 215
△H(oe) 25
εr 30
Tanδ 5.2×10-4
将实施例1-3中所得的低损耗功率旋磁材料进行性能测试,对其插入损耗、驻波和隔离性能进行测试,测试结果见表2。表2为插入损耗、驻波和隔离性能的测试结果表。
表2
性能 频率(851MHz) 频率(872.5MHz) 频率(894MHz)
插入损耗(dB) 0.21 0.24 0.23
驻波(dB) 27.3 26.1 26.8
隔离(dB) 27.3 27.5 26.2
综上所述,本发明提供的低损耗功率旋磁材料具有高磁矩、高居里温度、烧结温度低、能耗小及高介电常数高达30的优点。
以上所述仅为本发明的实施例,并非因此限制本发明的专利范围,凡是利用本发明说明书内容所作的等同变换,或直接或间接运用在相关的技术领域,均同理包括在本发明的专利保护范围内。

Claims (10)

1.一种低损耗功率旋磁材料,其特征在于,包括以下重量份原料:Bi20315-20份、Y2O322-26份、GeO21-2.5份、CaCO32-5份、Fe2O341-47份、ZrO22-5份、MnCO30.2-1份和CaTiO36-10份。
2.根据权利要求1所述的低损耗功率旋磁材料,其特征在于,包括以下重量份原料:Bi20316-18份、Y2O323-25份、GeO2 1-2份、CaCO32-4份、Fe2O342-46份、ZrO22-4份、MnCO30.2-1份和CaTiO36-9份。
3.根据权利要求1所述的低损耗功率旋磁材料,其特征在于,包括以下重量份原料:Bi20317份、Y2O323份、GeO2 1.5份、CaCO33份、Fe2O345份、ZrO23份、MnCO30.5份和CaTiO37份。
4.一种低损耗功率旋磁材料的制备方法,其特征在于,包括以下步骤:
(1)将Bi203、Y2O3、GeO2、CaCO3、Fe2O3、ZrO2和MnCO3按照权利要求1-3任意一项所述的低损耗功率旋磁材料中的重量份比例进行混合,获得混合原料;
(2)将所述混合原料进行一次球磨,所述一次球磨中原料、水和钢球的重量比为1:1.2-1.5:4.3-4.7;
(3)将一次球磨后的料浆进行烘干,获得烘干料;
(4)将所述烘干料进行预烧,获得预烧料,所述预烧的温度为900-1000℃,然后将所述预烧料进行保温2-6h;
(5)将CaTiO3按照权利要求1-3任意一项所述的低损耗功率旋磁材料中的重量份比例与保温后的预烧料混合,然后进行二次球磨,所述二次球磨中原料、水和钢球的重量比为1:1.1-1.4:3.4-3.9;
(6)将二次球磨后的料浆依次进行烘干、造粒和成型,获得成型样品;
(7)将所述成型样品进行烧结,所述烧结的温度为1050-1150℃,烧结后进行保温6-10h,获得所述低损耗功率旋磁材料。
5.根据权利要求4所述的低损耗功率旋磁材料的制备方法,其特征在于,步骤(2)中,所述一次球磨的球磨转速为60-80r/min,球磨时间为18-22h。
6.根据权利要求4所述的低损耗功率旋磁材料的制备方法,其特征在于,步骤(3)中,所述烘干的温度为120-160℃,时间为6-10h。
7.根据权利要求4所述的低损耗功率旋磁材料的制备方法,其特征在于,步骤(4)中,先将烘干后的混合原料过40目标准分样筛,再进行预烧。
8.根据权利要求4所述的低损耗功率旋磁材料的制备方法,其特征在于,步骤(5)中,所述二次球磨的球磨转速为97-103r/min,球磨时间为32-36h。
9.根据权利要求4所述的低损耗功率旋磁材料的制备方法,其特征在于,步骤(6)中,所述烘干的温度为100-140℃,时间为8-12h。
10.根据权利要求4所述的低损耗功率旋磁材料的制备方法,其特征在于,步骤(6)中,加入浓度为9-11%、质量比为9-11%PVA的胶水进行所述造粒,且造粒后过120目标准分样筛,然后再进行所述成型;所述成型的压制压力为3-7MPa。
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