CN107324792A - 一种高磁通软磁铁氧体复合材料 - Google Patents

一种高磁通软磁铁氧体复合材料 Download PDF

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CN107324792A
CN107324792A CN201710370359.1A CN201710370359A CN107324792A CN 107324792 A CN107324792 A CN 107324792A CN 201710370359 A CN201710370359 A CN 201710370359A CN 107324792 A CN107324792 A CN 107324792A
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soft magnetic
magnetic ferrite
composite
magnetic flux
composite powder
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曹庆波
王遵跃
张展胜
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Anhui Dongfang Magnetic Magnet Manufacturing Co Ltd
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Abstract

本发明提出了一种高磁通软磁铁氧体复合材料，包括软磁铁氧体预烧结料和复合粉料，所述复合粉料为软磁铁氧体预烧结料质量的8‑21％，所述复合粉料为气相白炭黑、稀土和多晶莫来石纤维的组合物，本发明通过合理的配方改进，对锰锌铁氧体以Cu、Ni掺杂的同时添加气相白炭黑、稀土和多晶莫来石纤维进行复合改性，有效提高了软磁铁氧体的饱和磁感应强度、居里温度和初始磁导率，大大减轻了功率损耗，综合提升了软磁铁氧体的磁性能，适用范围广。

Description

一种高磁通软磁铁氧体复合材料
技术领域
本发明涉及铁氧体磁性材料技术领域，具体涉及一种高磁通软磁铁氧体复合材料。
背景技术
高电阻率铁氧体磁粉、磁芯是实现程控通讯、数字技术、网络通讯彩电等电子设备中用作电感器、滤波器、脉冲变压器等产品使其小型化、轻量化必不可少的电子材料，不断提高磁性材料中的电阻率，一直是从事该专业的工程技术人员和生产厂商的追求，但材料的性能指标，如损耗、频率特性、居里温度等都不尽人意。当前软磁铁氧体材料的研究重点主要集中在两个方面：一方面研究配方以及添加剂对材料性能的影响，另一方面研究生产工艺的优化及新设备的开发对提高材料性能的作用。大量的研究表明、配方、添加剂、粉体的制备方法、烧结工艺中的各种因素等都会对铁氧体的性能产生很大的影响。其中合理的配方、添加剂对软磁铁氧体的性能有着重要的影响，也是制备高性能铁氧体材料的有效方法之一，配方与添加剂的研究已经逐步成为铁氧体制备中的关键技术。
发明内容
针对上述存在的问题，本发明提出了一种高磁通软磁铁氧体复合材料，通过合理的配方改进，对锰锌铁氧体以Cu、Ni掺杂的同时添加气相白炭黑、稀土和多晶莫来石纤维进行复合改性，有效提高了软磁铁氧体的饱和磁感应强度、居里温度和初始磁导率，大大减轻了功率损耗，综合提升了软磁铁氧体的磁性能，适用范围广。
为了实现上述的目的，本发明采用以下的技术方案：
一种高磁通软磁铁氧体复合材料，包括软磁铁氧体预烧结料和复合粉料，所述复合粉料为软磁铁氧体预烧结料质量的8-21％，所述复合粉料为气相白炭黑、稀土和多晶莫来石纤维的组合物。
优选的，所述软磁铁氧体预烧结料为Cu-Ni掺杂锰锌软磁铁氧体预烧结料。
优选的，所述Cu-Ni掺杂锰锌软磁铁氧体预烧结料包括主料和辅料，所述主料包括以下摩尔百分含量组分：MnO 36.2-38.5％、ZnO 8-9％、NiO 0.05-0.3％、Cu2O 0.015-0.024％、Fe2O3余量。
优选的，所述辅料包括占主料质量百分含量的如下组分：Cr2O3 0.005-0.012％、CaCO3 0.022-0.028％、ZrO2 0.015-0.018％、SnO2 0.01-0.04％。
优选的，所述软磁铁氧体预烧结料制备步骤如下：将主料在球磨机中研磨至粒径为20-30μm，烘干后在900℃条件下预烧结30-40min，然后以2℃/min升温至970℃预烧结20-25min，取出后与辅料共混，进行二次球磨至粒径小于1μm，烘干后即得软磁铁氧体预烧结料。
优选的，所述复合粉料中气相白炭黑、稀土、多晶莫来石纤维的添加质量比为4-6：0.5：0.8。
优选的，所述稀土为质量比1:0.6的氧化镧和氧化钕。
优选的，高磁通软磁铁氧体复合材料，制备步骤如下：按配方比例称取原料，先将复合粉料球磨至纳米级，然后再将软磁铁氧体预烧结料和复合粉料共混，送入球磨机中研磨，烘干后造粒，压制成型，在1100℃条件下烧结1-2h，再升温至1250℃烧结1-2h，最后升温至1300℃烧结2-4h，即得高磁通软磁铁氧体复合材料
由于采用上述的技术方案，本发明的有益效果是：本发明通过合理的配方改进，对锰锌铁氧体以Cu、Ni掺杂的同时添加气相白炭黑、稀土和多晶莫来石纤维进行复合改性，有效提高了软磁铁氧体的饱和磁感应强度、居里温度和初始磁导率，大大减轻了功率损耗，综合提升了软磁铁氧体的磁性能，且一定程度上提高了铁氧体的力学性能，适用范围广。本发明制得的高磁通软磁铁氧体复合材料初始磁导率为8380，饱和磁感应强度为476mT(100℃)，居里温度为287℃，功率损耗为328kw/m3(100℃)(以上数据均为本发明实施例经检测后的平均值)。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述。基于本发明的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1：
一种高磁通软磁铁氧体复合材料，包括软磁铁氧体预烧结料和复合粉料，所述软磁铁氧体预烧结料为Cu-Ni掺杂锰锌软磁铁氧体预烧结料，所述Cu-Ni掺杂锰锌软磁铁氧体预烧结料包括主料和辅料，所述主料包括以下摩尔百分含量组分：MnO 37.5％、ZnO 8.5％、NiO 0.15％、Cu2O 0.02％、Fe2O3余量，所述辅料包括占主料质量百分含量的如下组分：Cr2O30.008％、CaCO3 0.025％、ZrO2 0.017％、SnO2 0.02％，所述复合粉料为软磁铁氧体预烧结料质量的8％，所述复合粉料为气相白炭黑、稀土和多晶莫来石纤维的组合物，所述复合粉料中气相白炭黑、稀土、多晶莫来石纤维的添加质量比为4：0.5：0.8，所述稀土为质量比1:0.6的氧化镧和氧化钕。
高磁通软磁铁氧体复合材料制备方法：
1)软磁铁氧体预烧结料制备：将主料在球磨机中研磨至粒径为20-30μm，烘干后在900℃条件下预烧结30min，然后以2℃/min升温至970℃预烧结20min，取出后与辅料共混，进行二次球磨至粒径小于1μm，烘干后即得软磁铁氧体预烧结料；
2)高磁通软磁铁氧体复合材料制备：按配方比例称取原料，先将复合粉料球磨至纳米级，然后再将软磁铁氧体预烧结料和复合粉料共混，送入球磨机中研磨，烘干后造粒，压制成型，在1100℃条件下烧结1.5h，再升温至1250℃烧结1.5h，最后升温至1300℃烧结2.5h，即得高磁通软磁铁氧体复合材料。
实施例2：
一种高磁通软磁铁氧体复合材料，包括软磁铁氧体预烧结料和复合粉料，所述软磁铁氧体预烧结料为Cu-Ni掺杂锰锌软磁铁氧体预烧结料，所述Cu-Ni掺杂锰锌软磁铁氧体预烧结料包括主料和辅料，所述主料包括以下摩尔百分含量组分：MnO 38％、ZnO 8％、NiO0.05％、Cu2O 0.022％、Fe2O3余量，所述辅料包括占主料质量百分含量的如下组分：Cr2O30.01％、CaCO30.022％、ZrO20.016％、SnO20.04％，所述复合粉料为软磁铁氧体预烧结料质量的15％，所述复合粉料为气相白炭黑、稀土和多晶莫来石纤维的组合物，所述复合粉料中气相白炭黑、稀土、多晶莫来石纤维的添加质量比为5：0.5：0.8，所述稀土为质量比1:0.6的氧化镧和氧化钕。
高磁通软磁铁氧体复合材料制备方法：
1)软磁铁氧体预烧结料制备：将主料在球磨机中研磨至粒径为20-30μm，烘干后在900℃条件下预烧结35min，然后以2℃/min升温至970℃预烧结25min，取出后与辅料共混，进行二次球磨至粒径小于1μm，烘干后即得软磁铁氧体预烧结料；
2)高磁通软磁铁氧体复合材料制备：按配方比例称取原料，先将复合粉料球磨至纳米级，然后再将软磁铁氧体预烧结料和复合粉料共混，送入球磨机中研磨，烘干后造粒，压制成型，在1100℃条件下烧结2h，再升温至1250℃烧结1h，最后升温至1300℃烧结2h，即得高磁通软磁铁氧体复合材料。
实施例3：
一种高磁通软磁铁氧体复合材料，包括软磁铁氧体预烧结料和复合粉料，所述软磁铁氧体预烧结料为Cu-Ni掺杂锰锌软磁铁氧体预烧结料，所述Cu-Ni掺杂锰锌软磁铁氧体预烧结料包括主料和辅料，所述主料包括以下摩尔百分含量组分：MnO 36.7％、ZnO 8.4％、NiO 0.2％、Cu2O 0.024％、Fe2O3余量，所述辅料包括占主料质量百分含量的如下组分：Cr2O30.012％、CaCO3 0.024％、ZrO2 0.018％、SnO2 0.03％，所述复合粉料为软磁铁氧体预烧结料质量的10％，所述复合粉料为气相白炭黑、稀土和多晶莫来石纤维的组合物，所述复合粉料中气相白炭黑、稀土、多晶莫来石纤维的添加质量比为4.5：0.5：0.8，所述稀土为质量比1:0.6的氧化镧和氧化钕。
高磁通软磁铁氧体复合材料制备方法：
1)软磁铁氧体预烧结料制备：将主料在球磨机中研磨至粒径为20-30μm，烘干后在900℃条件下预烧结40min，然后以2℃/min升温至970℃预烧结25min，取出后与辅料共混，进行二次球磨至粒径小于1μm，烘干后即得软磁铁氧体预烧结料；
2)高磁通软磁铁氧体复合材料制备：按配方比例称取原料，先将复合粉料球磨至纳米级，然后再将软磁铁氧体预烧结料和复合粉料共混，送入球磨机中研磨，烘干后造粒，压制成型，在1100℃条件下烧结1h，再升温至1250℃烧结1.5h，最后升温至1300℃烧结3h，即得高磁通软磁铁氧体复合材料。
实施例4：
一种高磁通软磁铁氧体复合材料，包括软磁铁氧体预烧结料和复合粉料，所述软磁铁氧体预烧结料为Cu-Ni掺杂锰锌软磁铁氧体预烧结料，所述Cu-Ni掺杂锰锌软磁铁氧体预烧结料包括主料和辅料，所述主料包括以下摩尔百分含量组分：MnO 36.2％、ZnO 9％、NiO 0.25％、Cu2O 0.017％、Fe2O3余量，所述辅料包括占主料质量百分含量的如下组分：Cr2O3 0.005％、CaCO3 0.028％、ZrO2 0.015％、SnO2 0.02％，所述复合粉料为软磁铁氧体预烧结料质量的21％，所述复合粉料为气相白炭黑、稀土和多晶莫来石纤维的组合物，所述复合粉料中气相白炭黑、稀土、多晶莫来石纤维的添加质量比为6：0.5：0.8，所述稀土为质量比1:0.6的氧化镧和氧化钕。
高磁通软磁铁氧体复合材料制备方法：
1)软磁铁氧体预烧结料制备：将主料在球磨机中研磨至粒径为20-30μm，烘干后在900℃条件下预烧结35min，然后以2℃/min升温至970℃预烧结25min，取出后与辅料共混，进行二次球磨至粒径小于1μm，烘干后即得软磁铁氧体预烧结料；
2)高磁通软磁铁氧体复合材料制备：按配方比例称取原料，先将复合粉料球磨至纳米级，然后再将软磁铁氧体预烧结料和复合粉料共混，送入球磨机中研磨，烘干后造粒，压制成型，在1100℃条件下烧结1h，再升温至1250℃烧结1h，最后升温至1300℃烧结4h，即得高磁通软磁铁氧体复合材料。
实施例5：
一种高磁通软磁铁氧体复合材料，包括软磁铁氧体预烧结料和复合粉料，所述软磁铁氧体预烧结料为Cu-Ni掺杂锰锌软磁铁氧体预烧结料，所述Cu-Ni掺杂锰锌软磁铁氧体预烧结料包括主料和辅料，所述主料包括以下摩尔百分含量组分：MnO 38.5％、ZnO 8.6％、NiO 0.3％、Cu2O 0.015％、Fe2O3余量，所述辅料包括占主料质量百分含量的如下组分：Cr2O30.008％、CaCO3 0.026％、ZrO2 0.016％、SnO2 0.01％，所述复合粉料为软磁铁氧体预烧结料质量的16％，所述复合粉料为气相白炭黑、稀土和多晶莫来石纤维的组合物，所述复合粉料中气相白炭黑、稀土、多晶莫来石纤维的添加质量比为5：0.5：0.8，所述稀土为质量比1:0.6的氧化镧和氧化钕。
高磁通软磁铁氧体复合材料制备方法：
1)软磁铁氧体预烧结料制备：将主料在球磨机中研磨至粒径为20-30μm，烘干后在900℃条件下预烧结35min，然后以2℃/min升温至970℃预烧结20min，取出后与辅料共混，进行二次球磨至粒径小于1μm，烘干后即得软磁铁氧体预烧结料；
2)高磁通软磁铁氧体复合材料制备：按配方比例称取原料，先将复合粉料球磨至纳米级，然后再将软磁铁氧体预烧结料和复合粉料共混，送入球磨机中研磨，烘干后造粒，压制成型，在1100℃条件下烧结2h，再升温至1250℃烧结2h，最后升温至1300℃烧结3.5h，即得高磁通软磁铁氧体复合材料。
以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。

Claims (8)

1.一种高磁通软磁铁氧体复合材料，其特征在于，包括软磁铁氧体预烧结料和复合粉料，所述复合粉料为软磁铁氧体预烧结料质量的8-21％，所述复合粉料为气相白炭黑、稀土和多晶莫来石纤维的组合物。
2.根据权利要求1所述的高磁通软磁铁氧体复合材料，其特征在于：所述软磁铁氧体预烧结料为Cu-Ni掺杂锰锌软磁铁氧体预烧结料。
3.根据权利要求2所述的高磁通软磁铁氧体复合材料，其特征在于：所述Cu-Ni掺杂锰锌软磁铁氧体预烧结料包括主料和辅料，所述主料包括以下摩尔百分含量组分：MnO 36.2-38.5％、ZnO 8-9％、NiO 0.05-0.3％、Cu2O 0.015-0.024％、Fe2O3余量。
4.根据权利要求3所述的高磁通软磁铁氧体复合材料，其特征在于，所述辅料包括占主料质量百分含量的如下组分：Cr2O3 0.005-0.012％、CaCO3 0.022-0.028％、ZrO2 0.015-0.018％、SnO2 0.01-0.04％。
5.根据权利要求2或3所述的高磁通软磁铁氧体复合材料，其特征在于，所述软磁铁氧体预烧结料制备步骤如下：将主料在球磨机中研磨至粒径为20-30μm，烘干后在900℃条件下预烧结30-40min，然后以2℃/min升温至970℃预烧结20-25min，取出后与辅料共混，进行二次球磨至粒径小于1μm，烘干后即得软磁铁氧体预烧结料。
6.根据权利要求1所述的高磁通软磁铁氧体复合材料，其特征在于：所述复合粉料中气相白炭黑、稀土、多晶莫来石纤维的添加质量比为4-6：0.5：0.8。
7.根据权利要求1所述的高磁通软磁铁氧体复合材料，其特征在于：所述稀土为质量比1:0.6的氧化镧和氧化钕。
8.根据权利要求1-7任一项所述的高磁通软磁铁氧体复合材料，其特征在于，制备步骤如下：按配方比例称取原料，先将复合粉料球磨至纳米级，然后再将软磁铁氧体预烧结料和复合粉料共混，送入球磨机中研磨，烘干后造粒，压制成型，在1100℃条件下烧结1-2h，再升温至1250℃烧结1-2h，最后升温至1300℃烧结2-4h，即得高磁通软磁铁氧体复合材料。
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