CN114512323A - 一种MnO-SiO2绝缘包覆的金属软磁粉芯制备方法 - Google Patents
一种MnO-SiO2绝缘包覆的金属软磁粉芯制备方法 Download PDFInfo
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Abstract
本发明适用于金属软磁粉芯领域,提供了一种MnO‑SiO2绝缘包覆的金属软磁粉芯制备方法,所述方法包括以下步骤:向MnO2粉末中加入硅烷偶联剂,对MnO2粉末进行改性,使其富羟基化;向所得改性后的MnO2混合液中加入金属磁粉及乙醇,搅拌后干燥,得到MnO2绝缘包覆的金属磁粉;将所得MnO2绝缘包覆的金属磁粉过筛,进行筛分造粒,加压制成生坯;将所得生坯进行升温退火,得到MnO‑SiO2绝缘包覆的金属软磁粉芯成品。通过高温退火使MnO2包覆层转变为MnO‑SiO2包覆层,金属磁粉中的Si与MnO2原位反应生成的MnO‑SiO2包覆绝缘层比较均匀、致密,MnO‑SiO2包覆层耐高温,不易分解脱落,有效解决了磷酸钝化层高温下易分解的问题。
Description
技术领域
本发明属于金属软磁粉芯领域,特别涉及一种MnO-SiO2绝缘包覆的金属软磁粉芯制备方法。
背景技术
金属软磁粉芯由于具有高的饱和磁感应强度、良好的频率稳定性、优异的直流偏置性能以及低的涡流损耗,被作为开关电源中重要的功能材料,广泛应用于通讯电源、电动汽车、逆变器、变频空调等领域。
制备金属软磁粉芯主要通过对金属磁粉进行绝缘包覆来增大颗粒间的退磁场及降低涡流损耗,提高其抗饱和能力,从而提高其应用频率范围。因此高电阻率、耐高温、均匀的绝缘包覆层成为制备高性能金属软磁粉芯的关键。
目前,金属软磁粉芯的包覆方式主要分为有机包覆和无机包覆,有机包覆方式包覆层较为均匀但存在易老化、不耐高温等缺点;无机包覆方式可分为磷酸钝化和氧化物包覆方式两大类,磷酸钝化层在600℃左右会发生分解,存在同有机包覆方式相似的问题,氧化物包覆方式由于包覆层具有高电阻率、耐高温等优点成为目前金属软磁粉芯包覆方式的优选,但氧化物包覆方式仍存在包覆不均匀、包覆层易脱落等问题。
发明内容
针对上述问题,一方面,本发明公开了一种MnO-SiO2绝缘包覆的金属软磁粉芯制备方法,所述方法包括以下步骤:
向MnO2粉末中加入硅烷偶联剂和H2O的混合液,对MnO2粉末进行改性,使其富羟基化;
向所得改性后的MnO2混合液中加入金属磁粉及乙醇,搅拌后干燥,得到MnO2绝缘包覆的金属磁粉;
将所得MnO2绝缘包覆的金属磁粉过筛,进行筛分造粒,加压制成生坯;
将所得生坯进行升温退火,得到MnO-SiO2绝缘包覆的金属软磁粉芯成品。
进一步地,在所述向MnO2粉末中加入硅烷偶联剂之后,对硅烷偶联剂进行超声分散。
进一步地,所述硅烷偶联剂为KH550。
进一步地,所述向MnO2粉末中加入硅烷偶联剂时,所述MnO2、硅烷偶联剂与H2O的质量比为1:(0.009~0.011):(0.4~0.6)。
进一步地,所述干燥温度为120℃,并保温1h干燥。
进一步地,所述金属磁粉为铁硅铝粉、铁硅粉中的任意一种。
进一步地,所述向所得改性后的MnO2混合液中加入金属磁粉及乙醇时,各组份之间的组份比分别为:金属磁粉100份、MnO2混合液6~16份、乙醇2~5份。
进一步地,所述进行筛分造粒,加压制成生坯具体包括:
称取筛分造粒后的金属磁粉;
向金属磁粉中加入树脂粘结剂和硬脂酸锌,并混合均匀;
用油压机加压压制,制成生坯。
进一步地,所述MnO2绝缘包覆的金属磁粉与树脂粘结剂、硬脂酸锌的质量比为100:(0.25~0.35):(0.35~0.45)。
进一步地,所述油压机采用双向浮动压制方式进行压制。
进一步地,所述压制时的压强为1600-1900MPa,所述生坯密度为5.5~7.0g/cm3。
所述将所得生坯进行升温退火,得到MnO-SiO2绝缘包覆的金属软磁粉芯成品的步骤具体包括:
将生坯置于退火炉中,在氮气保护下将退火炉从室温以5℃/min升温速率升温至200℃,保温1h;
随后以5℃/min升温速率升温至900℃,保温3h;
然后随炉冷却至室温,得到MnO-SiO2绝缘包覆的金属软磁粉芯成品。
与现有技术相比,本发明具有以下有益效果:
(1)本发明通过高温退火使MnO2包覆层转变为MnO-SiO2包覆层,MnO-SiO2包覆绝缘层较MnO2绝缘层具有更高的电阻率,有效提高了金属软磁粉芯的抗饱和能力,降低其涡流损耗,提高其应用频率范围,符合磁性元件高频化的趋势。
(2)相对于传统的氧化物包覆方式,通过金属磁粉中的Si与MnO2原位反应生成的MnO-SiO2包覆绝缘层比较均匀、致密;而相对于同样进行原位包覆的磷酸钝化方式,MnO-SiO2包覆层耐高温,不易分解脱落,有效解决了磷酸钝化层高温下易分解的问题。
(3)本发明制备方法中,未加入有机包覆剂且在高温退火时完全分解了树脂粘结剂和硬脂酸锌,并驰豫了压制内应力,最终实现了全无机绝缘层,有效避免了有机绝缘层的老化问题,且MnO2添加量影响MnO-SiO2包覆层厚度,因此通过控制MnO2添加量可以调节软磁粉芯的直流偏置性能和损耗。
(4)本发明制备方法生产成本低、工艺流程简单。
本发明的其它特征和优点将在随后的说明书中阐述,并且,部分地从说明书中变得显而易见,或者通过实施本发明而了解。本发明的目的和其他优点可通过在说明书、权利要求书以及附图中所指出的结构来实现和获得。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作一简单地介绍,显而易见地,下面描述中的附图是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1是实施例1中制备的铁硅铝软磁粉芯的断面微观形貌图;
图2是实施例2中制备的铁硅铝软磁粉芯的断面微观形貌图;
图3是实施例3中制备的铁硅软磁粉芯的断面微观形貌图。
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中的附图,对本发明实施例中的技术方案进行清楚、完整地说明,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做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
(1)将12gMnO2加入0.12gKH550及6gH2O的混合液中,并机械搅拌1h,得到改性后的MnO2混合液;
(2)向步骤(1)中的混合液中加入300g铁硅铝磁粉及6g乙醇,机械搅拌1h,然后在120℃保温1h进行干燥,得到MnO2绝缘包覆后的铁硅铝粉末;
(3)将步骤(2)所得MnO2绝缘包覆后的铁硅铝粉末过200目筛网,进行筛分造粒,然后称取200g造粒后粉末,并加入0.6g树脂粘结剂和0.8g硬脂酸锌混合均匀,然后用油压机在1860MPa的压强下进行双向浮动压制,制成密度为5.73g/cm3的生坯;
(4)退火处理:将步骤(3)得到的生坯置于退火炉中,并通入氮气,将炉内空气排干净,在氮气的保护下,按照从室温以5℃/min升温速率升温至200℃保温1h,然后以5℃/min升温速率升温至900℃保温3h,之后随炉冷却至室温的热处理工艺进行退火处理,制成铁硅铝软磁粉芯成品。
本实施例制备的铁硅铝软磁粉芯的断面微观形貌如图1所示。可见,粉芯内部结构致密,铁硅铝磁粉间隙均匀包覆有绝缘材料。
本实施例制备的铁硅铝软磁粉芯经绕线测试后得到的磁性能指标如下:
(1)测试频率100kHz及测试电压1V条件下,磁导率μ=28.58;
(2)直流偏置性能:测试频率100kHz,直流偏置磁场100Oe下,磁导率百分比%μ=87.08%;测试频率100kHz,直流偏置磁场200Oe时,磁导率百分比%μ=66.03%;
(3)损耗:测试频率100kHz,测试磁通密度500Gs时,单位体积损耗Pcv=142.07mW/cm3。
实施例2
(1)将24gMnO2加入0.24gKH550及12gH2O的混合液中,并机械搅拌1h,得到改性后的MnO2混合液;
(2)向步骤(1)中的混合液中加入300g铁硅铝磁粉及12g乙醇,机械搅拌1h,然后在120℃保温1h进行干燥,得到MnO2绝缘包覆后的铁硅铝粉末;
(3)将步骤(2)所得MnO2绝缘包覆后的铁硅铝粉末过200目筛网,进行筛分造粒,然后称取200g造粒后粉末,并加入0.6g树脂粘结剂和0.8g硬脂酸锌混合均匀,然后用油压机在1860MPa的压强下进行双向浮动压制,制成密度为5.58g/cm3的生坯;
(4)退火处理:将步骤(3)得到的生坯置于退火炉中,并通入氮气,将炉内空气排干净,在氮气的保护下,按照从室温以5℃/min升温速率升温至200℃保温1h,然后以5℃/min升温速率升温至900℃保温3h,之后随炉冷却至室温的热处理工艺进行退火处理,制成铁硅铝软磁粉芯成品。
本实施例制备的铁硅铝软磁粉芯的断面微观形貌如图1所示。可见,粉芯内部结构致密,铁硅铝磁粉间隙均匀包覆有绝缘材料。
本实施例制备的铁硅铝软磁粉芯经绕线测试后得到的磁性能指标如下:
(1)测试频率100kHz及测试电压1V条件下,磁导率μ=22.04;
(2)直流偏置性能:测试频率100kHz,直流偏置磁场100Oe下,磁导率百分比%μ=90.1%;测试频率100kHz,直流偏置磁场200Oe时,磁导率百分比%μ=73.08%;
(3)损耗:测试频率100kHz,测试磁通密度500Gs时,单位体积损耗Pcv=251.04mW/cm3。
实施例3
(1)将30gMnO2加入0.3gKH550及15gH2O的混合液中,并机械搅拌1h,得到改性后的MnO2混合液;
(2)向步骤(1)中的混合液中加入300g铁硅磁粉及15g乙醇,机械搅拌1h,然后在120℃保温1h进行干燥,得到MnO2绝缘包覆后的铁硅粉末;
(3)将步骤(2)所得MnO2绝缘包覆后的铁硅铝粉末过200目筛网,进行筛分造粒,然后称取200g造粒后粉末,并加入0.6g树脂粘结剂和0.8g硬脂酸锌混合均匀,然后用油压机在1860MPa的压强下进行双向浮动压制,制成密度为6.08g/cm3的生坯;
(4)退火处理:将步骤(3)得到的生坯置于退火炉中,并通入氮气,将炉内空气排干净,在氮气的保护下,按照从室温以5℃/min升温速率升温至200℃保温1h,然后以5℃/min升温速率升温至900℃保温3h,之后随炉冷却至室温的热处理工艺进行退火处理,制成铁硅软磁粉芯成品。
本实施例制备的铁硅软磁粉芯的断面微观形貌如图1所示。可见,粉芯内部结构致密,铁硅磁粉间隙均匀包覆有绝缘材料。
本实施例制备的铁硅软磁粉芯经绕线测试后得到的磁性能指标如下:
(1)测试频率100kHz及测试电压1V条件下,磁导率μ=19.07;
(2)直流偏置性能:测试频率100kHz,直流偏置磁场100Oe下,磁导率百分比%μ=92.2%;测试频率100kHz,直流偏置磁场200Oe时,磁导率百分比%μ=83.69%;
(3)损耗:测试频率100kHz,测试磁通密度500Gs时,单位体积损耗Pcv=511.84mW/cm3。
通过上述制备方法得到MnO-SiO2绝缘包覆的金属软磁粉芯,具备以下优势:
(1)本发明通过高温退火使MnO2包覆层转变为MnO-SiO2包覆层,MnO-SiO2包覆绝缘层较MnO2绝缘层具有更高的电阻率,有效提高了金属软磁粉芯的抗饱和能力,降低其涡流损耗,提高其应用频率范围,符合磁性元件高频化的趋势。
(2)相对于传统的氧化物包覆方式,通过金属磁粉中的Si与MnO2原位反应生成的MnO-SiO2包覆绝缘层比较均匀、致密;而相对于同样进行原位包覆的磷酸钝化方式,MnO-SiO2包覆层耐高温,不易分解脱落,有效解决了磷酸钝化层高温下易分解的问题。
(3)本发明制备方法中,未加入有机包覆剂且在高温退火时完全分解了树脂粘结剂和硬脂酸锌,并驰豫了压制内应力,最终实现了全无机绝缘层,有效避免了有机绝缘层的老化问题,且MnO2添加量影响MnO-SiO2包覆层厚度,因此通过控制MnO2添加量可以调节软磁粉芯的直流偏置性能和损耗。
(4)本发明制备方法生产成本低、工艺流程简单。
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 (12)
1.一种MnO-SiO2绝缘包覆的金属软磁粉芯制备方法,其特征在于,所述方法包括以下步骤:
向MnO2粉末中加入硅烷偶联剂和H2O的混合液,对MnO2粉末进行改性,使其富羟基化;
向所得改性后的MnO2混合液中加入金属磁粉及乙醇,搅拌后干燥,得到MnO2绝缘包覆的金属磁粉;
将所得MnO2绝缘包覆的金属磁粉过筛,进行筛分造粒,加压制成生坯;
将所得生坯进行升温退火,得到MnO-SiO2绝缘包覆的金属软磁粉芯成品。
2.根据权利要求1所述的MnO-SiO2绝缘包覆的金属软磁粉芯制备方法,其特征在于,在所述向MnO2粉末中加入硅烷偶联剂之后,对硅烷偶联剂进行超声分散。
3.根据权利要求1所述的MnO-SiO2绝缘包覆的金属软磁粉芯制备方法,其特征在于,所述硅烷偶联剂为KH550。
4.根据权利要求1所述的MnO-SiO2绝缘包覆的金属软磁粉芯制备方法,其特征在于,所述向MnO2粉末中加入硅烷偶联剂时,所述MnO2、硅烷偶联剂与H2O的质量比为1:0.009~0.011:0.4~0.6。
5.根据权利要求1所述的MnO-SiO2绝缘包覆的金属软磁粉芯制备方法,其特征在于,所述干燥温度为120℃,并保温1h干燥。
6.根据权利要求1所述的MnO-SiO2绝缘包覆的金属软磁粉芯制备方法,其特征在于,所述金属磁粉为铁硅铝粉、铁硅粉中的任意一种。
7.根据权利要求1所述的MnO-SiO2绝缘包覆的金属软磁粉芯制备方法,其特征在于,所述向所得改性后的MnO2混合液中加入金属磁粉及乙醇时,各组份之间的组份比分别为:金属磁粉100份、MnO2混合液6~16份、乙醇2~5份。
8.根据权利要求1所述的MnO-SiO2绝缘包覆的金属软磁粉芯制备方法,其特征在于,所述进行筛分造粒,加压制成生坯具体包括:
称取筛分造粒后的金属磁粉;
向金属磁粉中加入树脂粘结剂和硬脂酸锌,并混合均匀;
用油压机加压压制,制成生坯。
9.根据权利要求8所述的MnO-SiO2绝缘包覆的金属软磁粉芯制备方法,其特征在于,所述MnO2绝缘包覆的金属磁粉与树脂粘结剂、硬脂酸锌的质量比为100:0.25~0.35:0.35~0.45。
10.根据权利要求8所述的MnO-SiO2绝缘包覆的金属软磁粉芯制备方法,其特征在于,所述油压机采用双向浮动压制方式进行压制。
11.根据权利要求8所述的MnO-SiO2绝缘包覆的金属软磁粉芯制备方法,其特征在于,所述压制时的压强为1600-1900MPa,所述生坯密度为5.5~7.0g/cm3。
12.根据权利要求1-11任一所述的MnO-SiO2绝缘包覆的金属软磁粉芯制备方法,其特征在于,所述将所得生坯进行升温退火,得到MnO-SiO2绝缘包覆的金属软磁粉芯成品的步骤具体包括:
将生坯置于退火炉中,在氮气保护下将退火炉从室温以5℃/min升温速率升温至200℃,保温1h;
随后以5℃/min升温速率升温至900℃,保温3h;
然后随炉冷却至室温,得到MnO-SiO2绝缘包覆的金属软磁粉芯成品。
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