CN109456049A - 一种高性能软磁材料的制备方法 - Google Patents
一种高性能软磁材料的制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000696 magnetic material Substances 0.000 title claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 29
- 238000005245 sintering Methods 0.000 claims abstract description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000005253 cladding Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 230000003647 oxidation Effects 0.000 claims abstract description 9
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims abstract description 8
- 230000002378 acidificating effect Effects 0.000 claims abstract description 7
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004615 ingredient Substances 0.000 claims description 18
- 238000000465 moulding Methods 0.000 claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 4
- 238000000748 compression moulding Methods 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 2
- 239000005751 Copper oxide Substances 0.000 claims description 2
- 229910000431 copper oxide Inorganic materials 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 230000005291 magnetic effect Effects 0.000 abstract description 14
- 229910052802 copper Inorganic materials 0.000 abstract description 5
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 abstract description 3
- 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 abstract description 3
- 239000003989 dielectric material Substances 0.000 abstract description 3
- 230000004907 flux Effects 0.000 abstract description 3
- 229910052759 nickel Inorganic materials 0.000 abstract description 3
- 238000001694 spray drying Methods 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 2
- 239000003595 mist Substances 0.000 abstract description 2
- 239000010949 copper Substances 0.000 description 4
- 239000000956 alloy Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000006247 magnetic powder Substances 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- DCXXMTOCNZCJGO-UHFFFAOYSA-N tristearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 description 2
- 229910000976 Electrical steel Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000006353 environmental stress Effects 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
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Abstract
本发明公开了一种高性能软磁材料的制备方法，包括了混合、喷雾干燥、预烧、粉碎、喷雾造粒、压制和烧结等工艺，通过合理的配方改进，并对锰锌铁氧体以Cu、Ni掺杂；本发明还采用纳米的酸性硅溶胶和纳米级MgO介电材料包覆处理粉料在氩气保护下进行粉料包覆，防止粉料的氧化，降低材料的涡流损耗，具有优异的软磁性能及高磁感应强度。
Description
所属技术领域
本发明涉及磁性材料制造领域，具体涉及一种高性能软磁材料的制备方法。
背景技术
软磁复合材料是通过在铁磁颗粒表面包覆电绝缘薄膜而获得的一类电磁应用材料；与传统的叠片钢磁芯相比，采用粉末冶金工艺制备的SMC磁芯具有一系列独特的性能，包括三维各向同性磁性能、非常低的涡流损耗、中高频率下相对低的总损耗和灵活的磁芯结构设计等，适用于复杂形和磁路的电机，能大幅降低磁芯的重量和体积。
铁基纳米晶软磁合金材料自问世以来，因具有高饱和磁感应强度、高磁导率、低损耗、低矫顽力等特点而得到极大的重视和深入的研究，并广泛应用于开关电源和电磁传感器等领域。
软磁合金的最大优点是具有较高的饱和磁通密度(Bs)，具有直流叠加特性好的特点。但软磁合金材料的绝缘电阻较低，损耗高。
目前的常规软磁复合材料包覆方法，主要是对铁粉颗粒表面磷酸化，使其颗粒表面形成一层磷酸盐的绝缘层，来提升电阻率，但含P或S的包覆层对环境污染严重。采用无机绝缘层和磁粉的热膨胀系数相差较大且无机绝缘层的本身的热膨胀系数不可变化，在温差较大的环境或是在长时间使用过程中会在磁粉内产生热应力，导致无机物包覆层的软磁复合材料无法具有优良的磁性能。这些问题都制约着软磁复合材料的发展和应用。
当发明内容
本发明提供一种高性能软磁材料的制备方法，包括了混合、喷雾干燥、预烧、粉碎、喷雾造粒、压制和烧结等工艺，通过合理的配方改进，并对锰锌铁氧体以Cu、Ni掺杂；本发明还采用纳米的酸性硅溶胶和纳米级MgO介电材料包覆处理粉料在氩气保护下进行粉料包覆，防止粉料的氧化，降低材料的涡流损耗，具有优异的软磁性能及高磁感应强度。
为了实现上述目的，实现上述目的，本发明提供了一种高性能软磁材料的制备方法，该方法包括如下步骤：
（1）制备主料粉末
所述主料包括以下质量百分含量组分：氧化锰 32-35％、氧化镍 5-7％、氧化铬 0.1-0.3％、氧化铜 0.03-0.05％、氧化铁余量；
将主料在球磨机中研磨至粒径为10-20μm，烘干后在900℃条件下预烧结35-45min，然后以2℃/min升温至950℃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，烘干后即得主料粉末；
（2）包覆处理
将混合均匀后的所述主料粉末与酸性硅溶胶、纳米级MgO按按照质量比(97-98)：(0.5-1)：(0.6-0.8)的比例在氩气的保护下进行混 合均匀，再向包覆好的粉末中加入质量比为0.3-0.5的硬脂酸锌；
（3）将上述包覆好的粉末置入成型设备模具型腔中，进行浮动压制成型，成型压力控制700-800Mpa，成型压制总时间为5-8s/pcs；成型设备采用的是200t液压机进行压制，在压制8-10s后不再加压，进行保压3-5s，产品再脱模，得到坯件；坯件的压制密度控制在3.5-3.65g/cm3；在保护气氛箱式电阻炉中进行烧结，烧结温度控制在1100℃-1150℃，保温120-180min，烧结气氛为氮气保护，氧含量控制为1%-1.5%，烧结结束后随炉冷却至室温。
本发明具备以下优点：
（1）制备方法报了混合、喷雾干燥、预烧、粉碎、喷雾造粒、压制和烧结等工艺；本发明制备的磁芯通过合理的配方改进，对锰锌铁氧体以Cu、Ni掺杂的同时；
（2）本发明还采用纳米的酸性硅溶胶和纳米级MgO介电材料包覆处理粉料在氩气保护下进行粉料包覆，防止粉料的氧化，降低材料的涡流损耗，，具有优异的软磁性能及高磁感应强度。
具体实施方式
实施例一
所述主料包括以下质量百分含量组分：氧化锰 32％、氧化镍 5％、氧化铬 0.1％、氧化铜 0.03％、氧化铁余量；将主料在球磨机中研磨至粒径为10-20μm，烘干后在900℃条件下预烧结35min，然后以2℃/min升温至950℃预烧结20min，取出后与辅料共混，进行二次球磨至粒径小于1μm，烘干后即得主料粉末。
将混合均匀后的所述主料粉末与酸性硅溶胶、纳米级MgO按按照质量比97：0.5：0.6的比例在氩气的保护下进行混 合均匀，再向包覆好的粉末中加入质量比为0.3的硬脂酸锌。
将上述包覆好的粉末置入成型设备模具型腔中，进行浮动压制成型，成型压力控制700Mpa，成型压制总时间为5s/pcs；成型设备采用的是200t液压机进行压制，在压制8s后不再加压，进行保压3s，产品再脱模，得到坯件；坯件的压制密度控制在3.5g/cm3；在保护气氛箱式电阻炉中进行烧结，烧结温度控制在1100℃，保温120min，烧结气氛为氮气保护，氧含量控制为1%%，烧结结束后随炉冷却至室温。
实施例二
所述主料包括以下质量百分含量组分：氧化锰 35％、氧化镍 7％、氧化铬 0.3％、氧化铜 0.05％、氧化铁余量；将主料在球磨机中研磨至粒径为10-20μm，烘干后在900℃条件下预烧结45min，然后以2℃/min升温至950℃预烧结25min，取出后与辅料共混，进行二次球磨至粒径小于1μm，烘干后即得主料粉末。
将混合均匀后的所述主料粉末与酸性硅溶胶、纳米级MgO按按照质量比98：1：0.8的比例在氩气的保护下进行混合均匀，再向包覆好的粉末中加入质量比为0.5的硬脂酸锌。
将上述包覆好的粉末置入成型设备模具型腔中，进行浮动压制成型，成型压力控制800Mpa，成型压制总时间为8s/pcs；成型设备采用的是200t液压机进行压制，在压制10s后不再加压，进行保压5s，产品再脱模，得到坯件；坯件的压制密度控制在3.65g/cm3；在保护气氛箱式电阻炉中进行烧结，烧结温度控制在1150℃，保温180min，烧结气氛为氮气保护，氧含量控制为1.5%，烧结结束后随炉冷却至室温。
Claims (1)
1.一种高性能软磁材料的制备方法，该方法包括如下步骤：
（1）制备主料粉末
所述主料包括以下质量百分含量组分：氧化锰 32-35％、氧化镍 5-7％、氧化铬 0.1-0.3％、氧化铜 0.03-0.05％、氧化铁余量；
将主料在球磨机中研磨至粒径为10-20μm，烘干后在900℃条件下预烧结35-45min，然后以2℃/min升温至950℃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，烘干后即得主料粉末；
（2）包覆处理
即将混合均匀后的所述主料粉末与酸性硅溶胶、纳米级MgO按按照质量比(97-98)：(0.5-1)：(0.6-0.8)的比例在氩气的保护下进行混 合均匀，再向包覆好的粉末中加入质量比为0.3-0.5的硬脂酸锌；
（3）将上述包覆好的粉末置入成型设备模具型腔中，进行浮动压制成型，成型压力控制700-800Mpa，成型压制总时间为5-8s/pcs；成型设备采用的是200t液压机进行压制，在压制8-10s后不再加压，进行保压3-5s，产品再脱模，得到坯件；坯件的压制密度控制在3.5-3.65g/cm3；在保护气氛箱式电阻炉中进行烧结，烧结温度控制在1100℃-1150℃，保温120-180min，烧结气氛为氮气保护，氧含量控制为1%-1.5%，烧结结束后随炉冷却至室温。
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| CN108818884A (zh) * | 2018-06-13 | 2018-11-16 | 苏州诺弘添恒材料科技有限公司 | 一种具有防腐涂层的软磁材料的制备方法 |
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| CN108818884A (zh) * | 2018-06-13 | 2018-11-16 | 苏州诺弘添恒材料科技有限公司 | 一种具有防腐涂层的软磁材料的制备方法 |
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