CN107056269A - 一种高频高电阻率铁氧体软磁材料的制备方法 - Google Patents

一种高频高电阻率铁氧体软磁材料的制备方法 Download PDF

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CN107056269A
CN107056269A CN201710310146.XA CN201710310146A CN107056269A CN 107056269 A CN107056269 A CN 107056269A CN 201710310146 A CN201710310146 A CN 201710310146A CN 107056269 A CN107056269 A CN 107056269A
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李聪
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Abstract

本发明公开了一种高频高电阻率铁氧体软磁材料的制备方法，该高频高电阻率铁氧体软磁材料，由主要原料、辅原料和助剂制成，所述主要原料按重量份包括：60‑65份Fe2O3、4‑4.5份Mn3O4、20‑22份NiO、1‑2.5份PbO、1‑2份SrCO3、1‑2份BaCO3、1‑2份CoO，辅原料按重量份包括：1‑1.5份ZrO2、0.5‑1份Bi2O3、1.5‑1.8份PtO2、0.5‑1.2份BaTiO3、0.2‑0.5份Ce2O3、0.3‑0.5份硼化铬，助剂按重量份包括：5‑8份硫酸钡、3‑6份乳化硅油、3‑6份改性聚乙烯醇；该种高频高电阻率铁氧体软磁材料具有耐高温、高电阻率、高频、高饱和磁通密度和低磁损耗的特点。

Description

一种高频高电阻率铁氧体软磁材料的制备方法
技术领域
本发明涉及一种高频高电阻率铁氧体软磁材料的制备方法。
背景技术
当磁化发生在Hc不大于1000A/m，这样的材料称为软磁体。软磁铁氧体是以Fe2O3为主成分的亚铁磁性氧化物，采用粉末冶金方法生产。40年代到60年代，是科学技术飞速发展的时期，雷达、电视广播、集成电路的发明等，对软磁材料的要求也更高，生产出了软磁合金薄带及软磁铁氧体材料。20世纪50年代是铁氧体蓬勃发展的时期。1952年磁铅石硬磁铁氧体研制成功；1956年又在此晶系中开发出平面型超高频铁氧体，同时发现了合稀土元素的石榴石型铁氧体，从而形成了尖晶石型、磁铅石型和石榴石型三大晶系铁氧体材料体系。进入70年代，随着电讯、自动控制、计算机等行业的发展，研制出了磁头用软磁合金，除了传统的晶态软磁合金外，又兴起了另一类材料-非晶态软磁合金应该说铁氧体的问世是强磁学和磁性材料发展史上的一个重要里程碑。至今铁氧体磁性材料已在众多高技术领域得到了广泛的应用。目前，随着智能手机、物联网等行业的迅猛发展，手机无线充电器、电子标签上的吸波材料得到了迅猛发展，高频、超低损耗Ni-Zn软磁铁氧体材料越来越无法满足需求。
发明内容
有鉴于此，本发明目的是提供一种耐高温、高电阻率、高频、高饱和磁通密度和低磁损耗的高频高电阻率铁氧体软磁材料。
为了解决上述技术问题，本发明的技术方案是：
一种高频高电阻率铁氧体软磁材料，由主要原料、辅原料和助剂制成，所述主要原料按重量份包括：60-65份Fe2O3、4-4.5份Mn3O4、20-22份NiO、1-2.5份PbO、1-2份SrCO3、1-2份BaCO3、1-2份CoO，所述辅原料按重量份包括：1-1.5份ZrO2、0.5-1份Bi2O3、1.5-1.8份PtO2、0.5-1.2份BaTiO3、0.2-0.5份Ce2O3、0.3-0.5份硼化铬，所述助剂按重量份包括：5-8份硫酸钡、3-6份乳化硅油、3-6份改性聚乙烯醇。
进一步的，所述一种高频高电阻率铁氧体软磁材料，由主要原料、辅原料和助剂制成，所述主要原料按重量份包括：65份Fe2O3、4份Mn3O4、20份NiO、1份PbO、1份SrCO3、1份BaCO3、1份CoO，所述辅原料按重量份包括：1份ZrO2、0.5份Bi2O3、1.5份PtO2、0.5份BaTiO3、0.2份Ce2O3、0.3份硼化铬，所述助剂按重量份包括：5份硫酸钡、3份乳化硅油、3份改性聚乙烯醇。
进一步的，所述一种高频高电阻率铁氧体软磁材料，由主要原料、辅原料和助剂制成，所述主要原料按重量份包括：60份Fe2O3、4.5份Mn3O4、22份NiO、2.5份PbO、2份SrCO3、2份BaCO3、2份CoO，所述辅原料按重量份包括：1.5份ZrO2、1份Bi2O3、1.8份PtO2、1.2份BaTiO3、0.5份Ce2O3、0.5份硼化铬，所述助剂按重量份包括：8份硫酸钡、6份乳化硅油、6份改性聚乙烯醇。
进一步的，所述一种高频高电阻率铁氧体软磁材料，由主要原料、辅原料和助剂制成，所述主要原料按重量份包括：63份Fe2O3、4.2份Mn3O4、21份NiO、1.8份PbO、1.5份SrCO3、1.5份BaCO3、1.5份CoO，所述辅原料按重量份包括：1.2份ZrO2、0.8份Bi2O3、1.6份PtO2、0.9份BaTiO3、0.3份Ce2O3、0.4份硼化铬，所述助剂按重量份包括：6.5份硫酸钡、5份乳化硅油、5份改性聚乙烯醇。
本发明要解决的另一技术问题为提供一种高频高电阻率铁氧体软磁材料的制备方法，包括以下步骤：
1)配料混合：取主要原料60-65份Fe2O3、4-4.5份Mn3O4、20-22份NiO、1-2.5份PbO、1-2份SrCO3、1-2份BaCO3、1-2份CoO和辅原料1-1.5份ZrO2、0.5-1份Bi2O3、1.5-1.8份PtO2、0.5-1.2份BaTiO3、0.2-0.5份Ce2O3、0.3-0.5份硼化铬放入搅拌机，以30-40r/min的速度搅拌20-25min，使得配料混合均匀，制得配料混合物，备用；
2)球磨：将步骤1)制得的配料混合物放入球磨机，以7000-7500rpm的速度高速球磨20min，使得配料混合物完全粉碎，制得预混料，备用；
3)烘干过筛：将步骤2)制得的预混料放入烘焙箱内，以60℃热风循环的方式加热30-40min，使得预混料烘干，然后过400-500目筛；
4)一次烧结：将步骤3)过筛后的预混料放入烧结机进行第一次烧结，在烧结过程中，将温度从室温以2-3℃/min的速度升温至760-800℃，烧结1.5h，以3-4℃/min的速度降温至室温，制得预烧料，备用；
5)加助剂粉碎：将步骤4)降温至室温的预烧料放入超微粉碎研磨机中，然后加入助剂5-8份硫酸钡、3-6份乳化硅油、3-6份改性聚乙烯醇，以4500r/min的速度研磨10-15min，使得预烧料和助剂粉碎混合均匀，制得预烧料混合物，备用；
6)入模成型：将步骤5)制得的预烧料混合物浇注入模具，用2.5-3GPa的压力成型；
7)二次烧结：将步骤6)压制成型的模具放入烧结机进行第二次烧结，在烧结过程中，将温度从室温以2-3℃/min的速度升温至900-1000℃，烧结2-3h，以3-4℃/min的速度降温至室温，即得铁氧体软磁。
本发明技术效果主要体现在以下方面：将主要原料Fe2O3、Mn3O4、NiO、PbO、SrCO3、BaCO3、CoO和辅原料ZrO2、Bi2O3、PtO2、BaTiO3、Ce2O3硼化铬经过混合、球磨、烘干过筛和第一次烧结的方式制得预烧料，在预烧料中加入助剂硫酸钡、乳化硅油和改性聚乙烯醇后进行研磨，再将研磨后的预烧料入模成型，然后将成型的模具进行第二次烧结，最后降至室温，制得一种耐高温、高电阻率、高频、高饱和磁通密度和低磁损耗的高频高电阻率铁氧体软磁材料。
具体实施方式
实施例1
一种高频高电阻率铁氧体软磁材料，由主要原料、辅原料和助剂制成，所述主要原料按重量份包括：65份Fe2O3、4份Mn3O4、20份NiO、1份PbO、1份SrCO3、1份BaCO3、1份CoO，所述辅原料按重量份包括：1份ZrO2、0.5份Bi2O3、1.5份PtO2、0.5份BaTiO3、0.2份Ce2O3、0.3份硼化铬，所述助剂按重量份包括：5份硫酸钡、3份乳化硅油、3份改性聚乙烯醇。
一种高频高电阻率铁氧体软磁材料的制备方法，包括以下步骤：
1)配料混合：取主要原料65份Fe2O3、4份Mn3O4、20份NiO、1份PbO、1份SrCO3、1份BaCO3、1份CoO和辅原料1份ZrO2、0.5份Bi2O3、1.5份PtO2、0.5份BaTiO3、0.2份Ce2O3、0.3份硼化铬放入搅拌机，以40r/min的速度搅拌25min，使得配料混合均匀，制得配料混合物，备用；
2)球磨：将步骤1)制得的配料混合物放入球磨机，以7500rpm的速度高速球磨20min，使得配料混合物完全粉碎，制得预混料，备用；
3)烘干过筛：将步骤2)制得的预混料放入烘焙箱内，以60℃热风循环的方式加热40min，使得预混料烘干，然后过500目筛；
4)一次烧结：将步骤3)过筛后的预混料放入烧结机进行第一次烧结，在烧结过程中，将温度从室温以3℃/min的速度升温至800℃，烧结1.5h，以4℃/min的速度降温至室温，制得预烧料，备用；
5)加助剂粉碎：将步骤4)降温至室温的预烧料放入超微粉碎研磨机中，然后加入助剂5份硫酸钡、3份乳化硅油、3份改性聚乙烯醇，以4500r/min的速度研磨15min，使得预烧料和助剂粉碎混合均匀，制得预烧料混合物，备用；
6)入模成型：将步骤5)制得的预烧料混合物浇注入模具，用3GPa的压力成型；
7)二次烧结：将步骤6)压制成型的预烧料混合物模具放入烧结机进行第二次烧结，在烧结过程中，将温度从室温以3℃/min的速度升温至1000℃，烧结3h，以4℃/min的速度降温至室温，即得铁氧体软磁。
实施例2
一种高频高电阻率铁氧体软磁材料，由主要原料、辅原料和助剂制成，所述主要原料按重量份包括：60份Fe2O3、4.5份Mn3O4、22份NiO、2.5份PbO、2份SrCO3、2份BaCO3、2份CoO，所述辅原料按重量份包括：1.5份ZrO2、1份Bi2O3、1.8份PtO2、1.2份BaTiO3、0.5份Ce2O3、0.5份硼化铬，所述助剂按重量份包括：8份硫酸钡、6份乳化硅油、6份改性聚乙烯醇。
一种高频高电阻率铁氧体软磁材料的制备方法，包括以下步骤：
1)配料混合：取主要原料60份Fe2O3、4.5份Mn3O4、22份NiO、2.5份PbO、2份SrCO3、2份BaCO3、2份CoO和辅原料1.5份ZrO2、1份Bi2O3、1.8份PtO2、1.2份BaTiO3、0.5份Ce2O3、0.5份硼化铬放入搅拌机，以30r/min的速度搅拌20min，使得配料混合均匀，制得配料混合物，备用；
2)球磨：将步骤1)制得的配料混合物放入球磨机，以7000rpm的速度高速球磨20min，使得配料混合物完全粉碎，制得预混料，备用；
3)烘干过筛：将步骤2)制得的预混料放入烘焙箱内，以60℃热风循环的方式加热30min，使得预混料烘干，然后过400目筛；
4)一次烧结：将步骤3)过筛后的预混料放入烧结机进行第一次烧结，在烧结过程中，将温度从室温以2℃/min的速度升温至760℃，烧结1.5h，以3℃/min的速度降温至室温，制得预烧料，备用；
5)加助剂粉碎：将步骤4)降温至室温的预烧料放入超微粉碎研磨机中，然后加入助剂8份硫酸钡、6份乳化硅油、6份改性聚乙烯醇，以4500r/min的速度研磨10min，使得预烧料和助剂粉碎混合均匀，制得预烧料混合物，备用；
6)入模成型：将步骤5)制得的预烧料混合物浇注入模具，用2.5GPa的压力成型；
7)二次烧结：将步骤6)压制成型的预烧料混合物模具放入烧结机进行第二次烧结，在烧结过程中，将温度从室温以2℃/min的速度升温至900℃，烧结2h，以3℃/min的速度降温至室温，即得铁氧体软磁。
实施例3
一种高频高电阻率铁氧体软磁材料，由主要原料、辅原料和助剂制成，所述主要原料按重量份包括：63份Fe2O3、4.2份Mn3O4、21份NiO、1.8份PbO、1.5份SrCO3、1.5份BaCO3、1.5份CoO，所述辅原料按重量份包括：1.2份ZrO2、0.8份Bi2O3、1.6份PtO2、0.9份BaTiO3、0.3份Ce2O3、0.4份硼化铬，所述助剂按重量份包括：6.5份硫酸钡、5份乳化硅油、5份改性聚乙烯醇。
一种高频高电阻率铁氧体软磁材料的制备方法，包括以下步骤：
1)配料混合：取主要原料63份Fe2O3、4.2份Mn3O4、21份NiO、1.8份PbO、1.5份SrCO3、1.5份BaCO3、1.5份CoO和辅原料1.2份ZrO2、0.8份Bi2O3、1.6份PtO2、0.9份BaTiO3、0.3份Ce2O3、0.4份硼化铬放入搅拌机，以35r/min的速度搅拌23min，使得配料混合均匀，制得配料混合物，备用；
2)球磨：将步骤1)制得的配料混合物放入球磨机，以7300rpm的速度高速球磨20min，使得配料混合物完全粉碎，制得预混料，备用；
3)烘干过筛：将步骤2)制得的预混料放入烘焙箱内，以60℃热风循环的方式加热35min，使得预混料烘干，然后过450目筛；
4)一次烧结：将步骤3)过筛后的预混料放入烧结机进行第一次烧结，在烧结过程中，将温度从室温以2℃/min的速度升温至800℃，烧结1.5h，以3℃/min的速度降温至室温，制得预烧料，备用；
5)加助剂粉碎：将步骤4)降温至室温的预烧料放入超微粉碎研磨机中，然后加入助剂硫酸钡、5份乳化硅油、5份改性聚乙烯醇，以4500r/min的速度研磨13min，使得预烧料和助剂粉碎混合均匀，制得预烧料混合物，备用；
6)入模成型：将步骤5)制得的预烧料混合物浇注入模具，用2.8GPa的压力成型；
7)二次烧结：将步骤6)压制成型的预烧料混合物模具放入烧结机进行第二次烧结，在烧结过程中，将温度从室温以3℃/min的速度升温至1000℃，烧结3h，以3℃/min的速度降温至室温，即得铁氧体软磁。
本发明中Fe2O3含量过低制品饱和磁通密度小，含量过高则材料的电阻率急剧下降、比损耗增大，Mn3O4的加入，Mn离子在烧结结反应取代2价Fe离子，进而降低三价Fe离子的生成，材料的电阻率进一步增高，当Mn3O4含量较低时材料的电阻率小，通过合理控制Fe2O3、NiO、PbO、SrCO3、BaCO3、CoO及Mn3O4的含量处于一定的范围，七者协同作用，并通过ZrO2、BaTiO3、Ce2O3、PtO21.6份和硼化铬0.4等原料的复合添加，可以大幅度提高软磁铁氧体磁芯材料的电阻率，使得软磁铁氧体磁芯材料在高频和低频下均有很高的阻抗特性，且仍保持较高的磁导率和饱和磁通密度，并加入一定量的助剂改性聚乙烯醇、硫酸钡和乳化硅油，可有效改善性能，产品结晶均匀，并可减少晶粒间、晶界间的气孔，使得产品具有独特的耐高温性能。
实验例
表一为实施例1-3高频高电阻率铁氧体软磁性能测试的平均结果：
表一
试验对象：将本发明高频高电阻率铁氧体软磁做为实验组，普通的铁氧体软磁做为对照组一，特制的铁氧体软磁做为对照组二。
实验方法：对三组铁氧体软磁的起始磁导率、最大磁导率、饱和磁通密度、矫顽力、居里温度和电阻率的测试结果进行对比。
表二为三组铁氧体软磁性能测试的参考环境：
形状和尺寸 环形、R20、直径0.35mm
测试环境温度 23±2℃
测试频率 ≤10KHz
测试要求 远离振源、磁场
表二
表三为三组铁氧体软磁的具体性能测试结果如下表：
表三
通过表三对三组铁氧体软磁的性能测试结果对比，可以看出本发明高频高电阻率铁氧体软磁材料比普通铁氧体软磁和特制铁氧体软磁起始磁导率高、最大磁导率大、矫顽力大、居里温度高和电阻率高。
本发明技术效果主要体现在以下方面：将主要原料Fe2O3、Mn3O4、NiO、PbO、SrCO3、BaCO3、CoO和辅原料ZrO2、Bi2O3、PtO2、BaTiO3、Ce2O3硼化铬经过混合、球磨、烘干过筛和第一次烧结的方式制得预烧料，在预烧料中加入助剂硫酸钡、乳化硅油和改性聚乙烯醇后进行研磨，再将研磨后的预烧料入模成型，然后将成型的模具进行第二次烧结，最后降至室温，制得一种耐高温、高电阻率、高频、高饱和磁通密度和低磁损耗的高频高电阻率铁氧体软磁材料。
当然，以上只是本发明的典型实例，除此之外，本发明还可以有其它多种具体实施方式，凡采用等同替换或等效变换形成的技术方案，均落在本发明要求保护的范围之内。

Claims (4)

1.一种高频高电阻率铁氧体软磁材料，由主要原料、辅原料和助剂制成，其特征在于，所述主要原料按重量份包括：60-65份Fe2O3、4-4.5份Mn3O4、20-22份NiO、1-2.5份PbO、1-2份SrCO3、1-2份BaCO3、1-2份CoO，所述辅原料按重量份包括：1-1.5份ZrO2、0.5-1份Bi2O3、1.5-1.8份PtO2、0.5-1.2份BaTiO3、0.2-0.5份Ce2O3、0.3-0.5份硼化铬，所述助剂按重量份包括：5-8份硫酸钡、3-6份乳化硅油、3-6份改性聚乙烯醇。
2.如权利要求1所述一种高频高电阻率铁氧体软磁材料，由主要原料、辅原料和助剂制成，其特征在于，所述主要原料按重量份包括：65份Fe2O3、4份Mn3O4、20份NiO、1份PbO、1份SrCO3、1份BaCO3、1份CoO，所述辅原料按重量份包括：1份ZrO2、0.5份Bi2O3、1.5份PtO2、0.5份BaTiO3、0.2份Ce2O3、0.3份硼化铬，所述助剂按重量份包括：5份硫酸钡、3份乳化硅油、3份改性聚乙烯醇。
3.如权利要求1所述一种高频高电阻率铁氧体软磁材料，由主要原料、辅原料和助剂制成，其特征在于，所述主要原料按重量份包括：60份Fe2O3、4.5份Mn3O4、22份NiO、2.5份PbO、2份SrCO3、2份BaCO3、2份CoO，所述辅原料按重量份包括：1.5份ZrO2、1份Bi2O3、1.8份PtO2、1.2份BaTiO3、0.5份Ce2O3、0.5份硼化铬，所述助剂按重量份包括：8份硫酸钡、6份乳化硅油、6份改性聚乙烯醇。
4.如权利要求1所述一种高频高电阻率铁氧体软磁材料，由主要原料、辅原料和助剂制成，其特征在于，所述主要原料按重量份包括：63份Fe2O3、4.2份Mn3O4、21份NiO、1.8份PbO、1.5份SrCO3、1.5份BaCO3、1.5份CoO，所述辅原料按重量份包括：1.2份ZrO2、0.8份Bi2O3、1.6份PtO2、0.9份BaTiO3、0.3份Ce2O3、0.4份硼化铬，所述助剂按重量份包括：6.5份硫酸钡、5份乳化硅油、5份改性聚乙烯醇。
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RU2761797C1 (ru) * 2021-05-31 2021-12-13 Федеральное государственное бюджетное образовательное учреждение высшего образования «Тверской государственный университет» Способ изготовления композита титанат бария - феррит бария в алюминийсодержащих тиглях
CN114685153A (zh) * 2022-03-30 2022-07-01 电子科技大学 宽温宽频MnZn功率铁氧体材料及制备方法
CN114716240A (zh) * 2022-03-30 2022-07-08 电子科技大学 高力学性能低损耗MnZn功率铁氧体材料制备方法
CN114835481A (zh) * 2022-03-30 2022-08-02 电子科技大学 高温高频MnZn功率铁氧体材料的制备方法

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Publication number Priority date Publication date Assignee Title
RU2761797C1 (ru) * 2021-05-31 2021-12-13 Федеральное государственное бюджетное образовательное учреждение высшего образования «Тверской государственный университет» Способ изготовления композита титанат бария - феррит бария в алюминийсодержащих тиглях
CN114685153A (zh) * 2022-03-30 2022-07-01 电子科技大学 宽温宽频MnZn功率铁氧体材料及制备方法
CN114716240A (zh) * 2022-03-30 2022-07-08 电子科技大学 高力学性能低损耗MnZn功率铁氧体材料制备方法
CN114835481A (zh) * 2022-03-30 2022-08-02 电子科技大学 高温高频MnZn功率铁氧体材料的制备方法
CN114685153B (zh) * 2022-03-30 2022-12-16 电子科技大学 宽温宽频MnZn功率铁氧体材料及制备方法
CN114835481B (zh) * 2022-03-30 2023-01-03 电子科技大学 高温高频MnZn功率铁氧体材料的制备方法
CN114716240B (zh) * 2022-03-30 2023-01-03 电子科技大学 高力学性能低损耗MnZn功率铁氧体材料制备方法

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