CN117303883A - 一种贫铁高阻抗锰锌铁氧体材料及其制备方法和应用 - Google Patents
一种贫铁高阻抗锰锌铁氧体材料及其制备方法和应用 Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000000463 material Substances 0.000 title claims abstract description 47
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 27
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title claims abstract description 21
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 9
- 229910020599 Co 3 O 4 Inorganic materials 0.000 claims abstract description 8
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 6
- 230000002950 deficient Effects 0.000 claims abstract description 5
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
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- 239000008187 granular material Substances 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 4
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- 239000011572 manganese Substances 0.000 claims description 3
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- 229910000859 α-Fe Inorganic materials 0.000 description 19
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- 150000002500 ions Chemical class 0.000 description 3
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- 229910003962 NiZn Inorganic materials 0.000 description 2
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Abstract
本发明公开了一种贫铁高阻抗锰锌铁氧体材料及其制备方法和应用，该材料包括主成分和辅助成分，主成分包括Fe2O3、ZnO和MnO，辅助成分选自SiO2、CaCO3、Nb2O5、ZrO2、Co3O4、TiO2中的至少一种，按比例调节主成分和辅助成分制成的生坯样品在1260‑1380℃的烧结温度下烧结，并保温4‑8小时，缓慢降温并冷却至180℃出炉，得到的贫铁高阻抗锰锌铁氧体具有高直流电阻率、高居里温度和高饱和磁感应强度特性，并且在宽频范围具有高阻抗特性，可以作为一种抗电磁干扰材料满足5G通讯、汽车电子、抗EMI等电子产品的市场需求。
Description
技术领域
本发明属于磁性材料技术领域，具体涉及一种贫铁高阻抗锰锌铁氧体材料及其制备方法和应用。
背景技术
随着信号延时的减小及信号频率的提高，电子产品的电磁干扰问题越来越受到重视，解决或降低电磁污染以及提高电子设备抗电磁干扰能力的有效办法是采用电磁兼容设计，其中需要用到大量抗电磁干扰(EMI)材料。常用的抗EMI材料有MnZn铁氧体和NiZn铁氧体材料，与NiZn铁氧体相比，MnZn铁氧体的电阻率相对较低，但如果主配方中Fe2O3摩尔百分含量不超过50％，就能抑制Fe2+离子生成，从而提高电阻率，使用频率得到大幅提高。
现有技术中，具有阻抗特性的MnZn铁氧体材料一般主配方采用较高比例的ZnO，虽有利于提高低频的阻抗，却使居里温度下降，或者在主配方中添加CuO、NiO等成分提高使用频率，但会导致低频阻抗低、成本高，例如公开号为CN101857426A的专利文献提供一种贫铁高阻抗MnZn铁氧体材料，采用贫铁配方，其在主配方中ZnO比例为16-21mol％，较高的ZnO比例有利于提高低频的阻抗，但居里温度只有115℃，不能用于5G通讯、汽车电子等温度要求高的工作环境。公开号为CN104261812A的专利文献提供一种抗EMI用铁氧体材料，采用贫铁配方，其电阻率只有100Ω·m，仅在1-100M频率段具有优异的阻抗特性。公开号为CN101805173A的专利文献提供一种贫铁配方的MnZn铁氧体材料，采用贫铁配方辅助成分必须添加ZrO2和SnO2，其电阻率只有50Ω·m，低损耗特性，与高阻抗方向截然相反。总之，类似上述贫铁MnZn铁氧体材料的主配方通过高比例的ZnO提高低频的阻抗，或辅助成分添加CuO、NiO等成分提高使用频率，但会导致居里温度低，或低频阻抗低、成本高。
综上所述，现有技术中铁氧体材料的组成及制备方法难以同时协调获得兼具有高直流电阻率、高居里温度和高饱和磁感应强度特性，并且在宽频范围具有高阻抗特性的MnZn铁氧体材料，难以满足特定领域下的使用要求。
发明内容
为了解决上述技术问题，本发明的主要目的是提供一种贫铁高阻抗锰锌铁氧体材料，其具有高直流电阻率、高居里温度和高饱和磁感应强度特性，并且在宽频范围具有高阻抗特性。
本发明的另一目的是提供所述贫铁高阻抗锰锌铁氧体材料的制备方法。
本发明的再一目的是提供所述贫铁高阻抗锰锌铁氧体材料的应用，用于制备抗电磁干扰(EMI)器件，满足5G通讯、汽车电子、抗EMI等电子产品的市场需求。
为实现上述目的，本发明采用的技术方案是：
本发明提供一种贫铁高阻抗锰锌铁氧体材料，包括主成分和辅助成分，所述主成分包括Fe2O3、ZnO和MnO；所述辅助成分选自SiO2、CaCO3、Nb2O5、ZrO2、Co3O4、TiO2中的至少一种。
作为优选，所述主成分按照摩尔百分含量为100％计，包括47-49.5mol％的Fe2O3和10-21mol％的ZnO，余量为MnO，其中Fe2O3摩尔百分含量不超过50％，有效地抑制Fe2+离子生成，减少了Fe2+-Fe3+间的电子迁移，从而提高材料的电阻率，使得材料使用频率得到大幅提高，且主成分中较低摩尔百分含量的ZnO可以保证高居里温度和高饱和磁感应强度特性。
作为优选，以所述主成分的总重量为100％计，所述辅助成分为SiO2、CaCO3、Nb2O5、ZrO2、Co3O4、TiO2，添加量包括：SiO2：0.004-0.008wt％，CaCO3：0.02-0.10wt％，Nb2O5：0.01-0.05wt％，ZrO2：0.01-0.04wt％，Co3O4：0.01-1.20wt％，TiO2：0.01-0.30wt％；其中CaCO3具有优化晶界、细化晶粒，改善材料损耗的作用，Ca2+向晶界的偏析，能使得晶粒均匀，晶界明显。在铁氧体烧结过程中，CaCO3与SiO2发生反应，Ca2+和Si4+向晶界处扩散，在晶界层形成1-10nm厚的CaSiO3绝缘层，提高材料的电阻率，起到改善宽频阻抗特性的作用；Nb2O5存在于晶界，起到阻止晶粒长大的作用，晶粒生长的阻碍作用从而形成晶粒细小均匀的显微结构，晶粒变得均匀致密，气孔率降低，畴壁位移和磁化矢量转动的阻力下降，材料起始磁导率不降反升，有利于提高宽频的阻抗；Co3O4和TiO2不仅起到改善磁导率温度特性，其对K1值的贡献提高常温的起始磁导率，改善宽频范围的阻抗特性。添加Co3O4可以生成K1正值很大的CoFe2O4，由于Co2+的K1值很大，综合利用Fe2+和Co2+对K1的补偿作用，K1值可能有多个补偿点，对应的磁导率温度曲线在较宽的温度范围较平坦，由此获得良好的宽温特性。Ti4+倾向于占据B位，迫使部分磁性离子Fe3+由B位转移至A位，使得B位中Fe3+/Fe2+间电子跃迁的几率降低，提高材料的电阻率。
作为优选，所述贫铁高阻抗锰锌铁氧体材料的居里温度符合公式：Tc＝6.475×(x-2z/3)-104，其中Tc表示居里温度，x表示Fe2O3的摩尔含量，z表示ZnO的摩尔含量。
本发明还提供一种贫铁高阻抗锰锌铁氧体材料的制备方法，该方法包括以下步骤：
1)Fe2O3、Mn3O4和ZnO各主成分按所述比例混合均匀并烘干；
2)步骤1)所得的粉料在800-950℃下预烧2-3小时，然后自然冷却降温；
3)步骤2)所得的粉料按比例添加所述辅助成分进行球磨；
4)基于步骤3)所得的粉料的总重量，向其中添加5-15wt％的有机粘合剂水溶液，混合均匀造粒，得到颗粒料；
5)步骤4)所得的颗粒料压制成生坯样品；
6)步骤5)所得的生坯样品在1260-1380℃的烧结温度下高温烧结，并保温4-8小时，然后缓慢降温并冷却至180℃出炉，即得；其中保温段氧分压为2-10％，降温过程采用平衡氧分压。
本发明还提供所述贫铁高阻抗锰锌铁氧体材料在制备抗电磁干扰器件中的应用。
与现有技术相比，本发明的有益效果是：
1、本发明的贫铁高阻抗锰锌铁氧体材料包括主成分和辅助成分，主成分中Fe2O3的摩尔百分含量不超过50％，配合较低摩尔百分含量的ZnO以及合理的辅助成分，得到的MnZn铁氧体具有高直流电阻率、高居里温度和高饱和磁感应强度特性，并且在宽频范围具有高阻抗特性。
2、本发明的贫铁高阻抗锰锌铁氧体材料不含高比例的贵金属，例如避免使用价格较高的原材料NiO，具有成本低，工艺简单的特点，制备的产品可满足5G通讯、汽车电子、抗EMI等电子产品的良好运行，从而更好地满足市场需求。
具体实施方式
下面结合具体实施例对本发明进行详细说明。
以下实施例1-4和比较例1为以Fe2O3、Mn3O4、ZnO作为主成分，各主成分添加量不同获得的铁氧体材料，置于球磨机中混合0.5小时后取出烘干；用箱式电阻炉将所得粉料在900℃下预烧1小时，然后将预烧后的粉料放入球磨机中，基于所述主成分的总重量向所得粉料中添加以下辅助成分：0.005wt％的SiO2、0.04wt％的CaCO3、0.025wt％的Nb2O5、0.02wt％的ZrO2、0.90wt％的Co3O4和0.1wt％的TiO2，将此粉料球磨至平均粒度为1.0±0.2μm左右；基于球磨后的粉料总重量，向该粉料中添加10wt％的聚乙烯醇溶液，混合均匀造粒，并将颗粒料压制成25×8×15mm的环形样品。最后在用计算机程序控制的钟罩炉内，在1350℃的温度下保温5小时，然后缓慢降温并冷却至180℃出炉，其中保温段氧分压为5.0％，降温过程采用平衡氧分压。
表1
注：*表示主成分范围已超出本发明的范围。
实施例1-4及比较例1的电磁物理性能检测结果数据见表2。
表2
从表2可以看出，实施例1-4符合本发明的配方要求，其起始磁导率大于2000，具有较高的居里温度和贫铁高阻抗特性。比较例1中，常规主成分的铁氧体材料中Fe2O3、ZnO含量超出本发明的配方含量，所制备的材料无法获得优异的宽频阻抗特性，在25MHz时阻抗跌落到2Ω，更高频则不具有阻抗特性；同时，比较例1的材料也不具备较高的居里温度，其居里温度不能用本发明的贫铁公式进行计算。
实施例5-8以及比较例2-3将主成分固定为48.5mol％的Fe2O3、19.5mol％的ZnO，余量为MnO，基于所述主成分的总重量向所得粉料中添加辅助成分参见表3。
表3
注：*表示辅助成分范围已超出本发明的范围。
实施例5-8以及比较例2-3的电磁物理性能检测结果数据见表4。
表4
从表4可以看出，实施例5-8的辅助成分含量符合本发明的配方范围，其起始磁导率大于2000，具有贫铁高阻抗特性。比较例2-3表明，所添加的辅助成分超出本发明的配方要求，引起晶粒不连续生长、晶粒结构异常变化，所获得材料的磁导率和常温饱和磁感应强度低，低频阻抗特性变差，综合性能低下，同时由于没有加入Co和Ti，使得材料的截止频率大幅度下降，其高频阻抗变差。
从表2和4可以看出，在本发明主成分和辅助成分含量范围内的MnZn铁氧体具有大于140℃的居里温度和大于420mT的常温饱和磁感应强度及大于2000的起始磁导率，同时还具有0.01-700MHz宽频范围的高阻抗特性，其中1MHz、25MHz、100MHz和500MHz的阻抗分别大于8Ω、50Ω、110Ω和1300Ω。而在比较例2和3中，主成分或辅助成分超出本发明中铁氧体材料的配方范围，其直流电阻率、常温饱和磁感应强度、起始磁导率以及阻抗特性发生显著的变化，电磁物理性能检测结果超出本发明的设计指标范围。
上述对实施例的描述是为了便于该技术领域的普通技术人员能理解和使用本发明。熟悉本领域技术人员显然可以容易的对这些实施例做出各种修改，并把在此说明的一般原理应用到其他实施例中，而不必经过创造性的劳动。因此，本发明不限于上述实施例。本领域技术人员根据本发明的原理，不脱离本发明的范畴所做出的改进和修改都应该在本发明的保护范围之内。
Claims (6)
1.一种贫铁高阻抗锰锌铁氧体材料，其特征在于，包括主成分和辅助成分，所述主成分包括Fe2O3、ZnO和MnO；所述辅助成分选自SiO2、CaCO3、Nb2O5、ZrO2、Co3O4、TiO2中的至少一种。
2.根据权利要求1所述的贫铁高阻抗锰锌铁氧体材料，其特征在于，所述主成分按照摩尔百分含量为100％计，包括47-49.5mol％的Fe2O3和10-21mol％的ZnO，余量为MnO。
3.根据权利要求1所述的贫铁高阻抗锰锌铁氧体材料，其特征在于，所述辅助成分为SiO2、CaCO3、Nb2O5、ZrO2、Co3O4和TiO2，以所述主成分的总重量为100％计，各辅助成分的添加量如下：
SiO2：0.004-0.008wt％，CaCO3：0.02-0.10wt％，Nb2O5：0.01-0.05wt％，ZrO2：0.01-0.04wt％，Co3O4：0.01-1.20wt％，TiO2：0.01-0.30wt％。
4.根据权利要求1所述的贫铁高阻抗锰锌铁氧体材料，其特征在于，所述贫铁高阻抗锰锌铁氧体材料的居里温度符合如下公式：
Tc＝6.475×(x-2z/3)-104
其中，Tc表示居里温度，x表示Fe2O3的摩尔含量，z表示ZnO的摩尔含量。
5.权利要求1至4任一项所述贫铁高阻抗锰锌铁氧体材料的制备方法，其特征在于，包括以下步骤：
1)Fe2O3、Mn3O4和ZnO各主成分按所述比例混合均匀并烘干；
2)步骤1)所得的粉料在800-950℃下预烧2-3小时，然后自然冷却降温；
3)步骤2)所得的粉料按比例添加所述辅助成分进行球磨；
4)基于步骤3)所得的粉料的总重量，向其中添加5-15wt％的有机粘合剂水溶液，混合均匀造粒，得到颗粒料；
5)步骤4)所得的颗粒料压制成生坯样品；
6)步骤5)所得的生坯样品在1260-1380℃的烧结温度下高温烧结，并保温4-8小时，然后缓慢降温并冷却至180℃出炉即得，其中保温段氧分压为2-10％，降温过程采用平衡氧分压。
6.权利要求1至4任一项所述贫铁高阻抗锰锌铁氧体材料在制备抗电磁干扰器件中的应用。
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