WO2020083281A1 - 一种铁硅磁粉芯材料及其制备方法 - Google Patents

一种铁硅磁粉芯材料及其制备方法 Download PDF

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WO2020083281A1
WO2020083281A1 PCT/CN2019/112528 CN2019112528W WO2020083281A1 WO 2020083281 A1 WO2020083281 A1 WO 2020083281A1 CN 2019112528 W CN2019112528 W CN 2019112528W WO 2020083281 A1 WO2020083281 A1 WO 2020083281A1
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powder
iron
silicon
magnetic
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严彪
刘川木
严鹏飞
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Tongji University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/33—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials mixtures of metallic and non-metallic particles; metallic particles having oxide skin
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties

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  • the invention belongs to the technical field of composite soft magnetic materials, in particular to an iron-silicon magnetic powder core material containing Fe 3 O 4 and a preparation method thereof.
  • the soft magnetic composite material (also known as magnetic powder core) is a soft magnetic material that uses magnetic particles as raw materials, coats the particles with an insulating medium, and then uses powder metallurgy to press the powder into the desired shape and heat-anneal it.
  • the iron-silicon magnetic powder core is made of alloy powder of 94% Fe and 6% Si.
  • the iron-silicon magnetic powder core has a high saturation magnetic induction intensity of 1.5T, an effective magnetic permeability range of 26 to 90, and excellent DC bias characteristics, which is still as high as 70% at 100 Oe.
  • the iron loss of the iron-silicon magnetic powder core is higher than that of the traditional iron-silicon-aluminum magnetic powder core (Xianbei alloy). This is because silicon as a semiconductor element has a low resistivity.
  • the purpose of the present invention is to provide an iron-based magnetic powder core material containing Fe 3 O 4 and a preparation method in order to overcome the above-mentioned defects in the prior art.
  • the present invention chooses to add Fe 3 O 4 with higher magnetic properties and higher resistivity as a supplement.
  • Fe 3 O 4 has a relatively low price and a high cost performance.
  • Mn-Zn ferrite particles are added.
  • the iron-based magnetic powder core material containing Fe 3 O 4 has good processing performance, high magnetic performance and low production cost.
  • An iron-silicon magnetic powder core material which is a composite material, includes iron powder, and silicon-containing components, Fe 3 O 4 particles, and Mn-Zn ferrite particles coated on the surface of the iron powder, wherein,
  • the weight percentage of iron powder is ⁇ 90wt%
  • the weight percentage of Fe 3 O 4 particles is 3wt% -5wt%
  • the weight percentage content of Mn-Zn ferrite particles is 2wt%
  • the silicon content in the preferred composite material is not higher than 5 wt% to obtain the best matching of magnetic properties.
  • the iron-silicon magnetic powder core material has a core-shell structure, and the iron powder is a core.
  • the silicon-containing component, Fe 3 O 4 particles, and Mn-Zn ferrite particles are coated on the iron powder to form a shell.
  • the silicon-containing component is pure silicon or a silicon-containing iron-based component.
  • the content of the silicon-containing iron-based component is not less than 75% by weight.
  • the iron powder is ultrafine spherical iron powder, and the iron powder has a trace amount of oxygen / nitride doping, wherein the oxygen / nitride does not exceed 1 wt%.
  • the Fe 3 O 4 particles are powder particles with a particle size of less than 30 ⁇ m.
  • the Fe 3 O 4 particles are resistant to high temperature and are ferromagnetic discontinuous nano-scale particles.
  • the invention forms a coating in the obtained composite material and improves the magnetic properties of the material; the ultra-fine Fe 3 O 4 has high resistivity and better magnetic properties, and can better improve the performance of the traditional iron-silicon magnetic powder core.
  • a preparation method of iron-silicon magnetic powder core material includes the following steps:
  • step (2) The mixed powder obtained in step (1) and the binder are kneaded and granulated on a ball mill to obtain a soft magnetic alloy powder, and the binder accounts for 10% by mass of the mixed powder obtained in step (1);
  • the soft magnetic powder obtained in step (3) and the binder are uniformly mixed, the soft magnetic powder is prepared by ball milling in a planetary ball mill.
  • the mass ratio of the soft magnetic alloy powder obtained in step (3) to the binder is 22: 5;
  • the coated magnetic powder is cold-pressed by a press to form a magnetic ring
  • the magnetic ring is annealed, using argon as a protective atmosphere, and then cooled to room temperature with the furnace.
  • the binder is in powder form and sieved with a 30-mesh sieve.
  • the binder is zinc stearate.
  • the mixing time is 1h and the mixing speed is 30r / min;
  • the mixing time is 1h and the mixing speed is 30r / min;
  • step (4) in a planetary ball mill, with a ball-to-material ratio of 50: 1, a rotation speed of 200 rpm, and ball milling under an argon atmosphere for 2 hours;
  • the pressing pressure is 160kN and the pressing time is 5min;
  • the magnetic powder core is annealed, argon is used as the protective atmosphere, the heating rate is 5K / min, heated to 1000 ° C, kept for 2 hours, and then cooled to room temperature with the furnace.
  • the invention can uniformly coat Fe powder through a mechanical ball milling process to form a core-shell structure magnetic powder with controllable thickness.
  • powders are subjected to vacuum mixing treatment to ensure that no Fe powder is oxidized during the mixing process.
  • Powder forming must go through pressing, degreasing and sintering, densification, heat treatment and other processes. To achieve better performance, certain guidance, filling process and field action are required.
  • the heat treatment process needs to be carried out under the protection of inert gas or inert + reducing atmosphere, the general role is to eliminate stress.
  • the prepared magnetic powder core has the characteristics of high density, uniform internal structure, good DC bias performance and relatively low power consumption.
  • the feature of the invention is that the high-density iron-silicon magnetic powder core prepared by the new technology shows extremely excellent soft magnetic performance.
  • the present invention has the following advantages and beneficial effects:
  • the density of the prepared magnetic powder core is above 7g / cm 3 and the density is as high as over 90%;
  • FIG. 1 is a hysteresis curve diagram of the magnetic ring obtained in Example 1;
  • FIG. 2 is the result of the magnetic ring hysteresis data obtained in Example 1;
  • FIG. 3 is an xps map of the magnetic ring obtained in Example 1;
  • Example 4 is the CSONH component analysis result 1 of the magnetic ring obtained in Example 1;
  • Example 5 is the second CSONH component analysis result of the magnetic ring obtained in Example 1;
  • FIG. 6 is the third CSONH component analysis result of the magnetic ring obtained in Example 1.
  • the raw material powder is reduced iron powder, the binder zinc stearate is made into powder, and sieved with a 30-mesh sieve.
  • 19g of reduced iron powder, 0.4g of nano-Mn-Zn ferrite particles and 0.6g of nano-silica powder are dry mixed in a vacuum glove box, the mixing time is 1h, and the mixing speed is 30r / min.
  • step (2) The mixed powder obtained in step (1) and the binder are kneaded and granulated on a ball mill to obtain a soft magnetic alloy powder.
  • the binder accounts for 10% by mass of the mixed powder obtained in step (1).
  • the planetary ball mill Medium ball milling at 50: 1 ball-to-material ratio, 200 rpm rotation speed, and argon protective atmosphere for 2 hours;
  • step (2) Add the soft magnetic alloy powder obtained in step (2) and nano Fe 3 O 4 to the vacuum glove box to mix uniformly, and mix uniformly for 1 hour at 30 r / min;
  • the coated magnetic powder is cold pressed by a press to form a magnetic ring, the pressing pressure is 160kN, and the pressing time is 5min;
  • the magnetic powder core is annealed, using argon gas as the protective atmosphere, with a heating rate of 5K / min, heated to 1000 ° C, kept for 2 hours, and then cooled to room temperature with the furnace.
  • a total of 15 magnetic rings were prepared according to the above method, of which the fifth performance is more outstanding. Its performance is as follows:
  • the density of the obtained magnetic ring is 7.285g / cm 3.
  • Hs 3000A / m
  • the maximum permeability is 25.92mH / m
  • the saturation magnetic induction intensity is 1.949T
  • the coercive force is 22.4A / m. 1 shown.
  • Figure 2 shows these performance measurements.
  • Fig. 4 Fig. 5 and Fig. 6, the 5 of the sample identifier and the sample name represents the product prepared in this example.

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

一种铁硅磁粉芯材料及其制备方法，该复合材料为将铁粉、少量硅粉、超细Fe 3O 4、Mn-Zn铁氧体颗粒与合适的粘结剂混合均匀，采用新型粉末冶金技术制备出环形材料，将粘结剂脱除后高温退火烧结，得到高致密、高性能的软磁材料。该材料以铁粉为主体，加入的纳米级颗粒在不影响铁粉磁性能的前提下，对材料磁性能进一步提升。该铁硅磁粉芯材料具有加工灵活、磁学性能高、产品致密度高等优点。

Description

一种铁硅磁粉芯材料及其制备方法 技术领域
本发明属于复合软磁材料技术领域，尤其是涉及一种含Fe 3O 4的铁硅磁粉芯材料及其制备方法。
背景技术
软磁复合材料(又称磁粉芯)是一种以磁性颗粒为原料，在颗粒表面包覆绝缘介质后采用粉末冶金工艺将粉末压制成所需形状，并通过热处理退火而得到的软磁性材料。铁硅磁粉芯是由94％Fe和6％Si的合金粉末制成。铁硅磁粉芯具有高迖1.5T的饱和磁感应强度，有效磁导率范围26～90，直流偏置特性优异，在100Oe时仍高达70％。
但是铁硅磁粉芯的铁损高于传统的铁硅铝磁粉芯(仙贝合金)，这是由于硅作为一种半导体元素，其电阻率较低。
发明内容
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种含Fe 3O 4的铁基磁粉芯材料及制备方法。
为了提高其电阻率，本发明选择加入磁性能和电阻率较高的Fe 3O 4作为补充物，Fe 3O 4价格较为低廉，性价比高。为了提高其交流稳定性并降低磁损耗，而加入Mn-Zn铁氧体颗粒。
本发明含Fe 3O 4的铁基磁粉芯材料加工性能好、磁性能高、生产成本低。
本发明的目的可以通过以下技术方案来实现：
一种铁硅磁粉芯材料，为复合材料，包括铁粉，以及在铁粉表面包覆的含硅组分、Fe 3O 4颗粒及Mn-Zn铁氧体颗粒，其中，
铁粉的重量百分含量为≥90wt％，
Fe 3O 4颗粒的重量百分含量为3wt％-5wt％，
Mn-Zn铁氧体颗粒的重量百分含量为2wt％，
由于超细Fe 3O 4的作用，优选的复合材料中硅含量不高于5wt％，以获得最佳的磁性能匹配。
所述铁硅磁粉芯材料为核壳结构，铁粉为核，所述含硅组分、Fe 3O 4颗粒及Mn-Zn铁氧体颗粒包覆在铁粉外面形成壳。
所述含硅组分为纯硅或含硅铁基的组分，含硅铁基的组分中硅铁含量不低于75wt％。
所述铁粉为超细球形铁粉，而且所述铁粉具有微量的氧/氮化物掺杂，其中氧/氮化物不超过1wt％。
所述Fe 3O 4颗粒为粒度小于30μm的粉末颗粒，所述Fe 3O 4颗粒耐高温，为亚铁磁性非连续的纳米级颗粒。
本发明在所得复合材料中形成包覆，提高材料的磁性能；超细Fe 3O 4电阻率高，且有较好的磁性能，可对传统的铁硅磁粉芯性能进行较好的改进。
一种铁硅磁粉芯材料的制备方法，包括以下步骤：
(1)将还原铁粉和纳米Mn-Zn铁氧体颗粒、含硅组分在真空手套箱内干混均匀，得到混合粉末，还原铁粉和纳米Mn-Zn铁氧体颗粒、含硅组分的质量比为19:0.4:0.6；
(2)将步骤(1)所得混合粉末与粘结剂在球磨机上混炼制粒，得到软磁合金粉末，粘结剂占步骤(1)所得混合粉末的质量百分比为10％；
(3)将软磁合金粉末与纳米Fe 3O 4颗粒加入真空手套箱中均匀混料，软磁合金粉末与纳米Fe 3O 4颗粒的质量比为10:1，
(4)将步骤(3)所得软磁合金粉末与粘结剂均匀混合后，在行星球磨机中球磨制备软磁粉末，步骤(3)所得软磁合金粉末与粘结剂的质量比为22:5；
(5)将包覆好的磁粉利用压机冷压压制成磁环；
(6)在真空热处理炉中，对磁环进行退火处理，采用氩气作为保护气氛，然后随炉冷却到室温。
所述粘结剂为粉末状，并用30目的筛子过筛。
所述粘结剂为硬脂酸锌。
所述步骤(1)中，混料时间为1h，混料速度为30r/min；
所述步骤(3)中，混料时间为1h，混料速度为30r/min；
所述步骤(4)中，在行星球磨机中，以50：1的球料比，200rpm的转速，氩气保护气氛条件下球磨2h；
所述步骤(5)中，压制压力为160kN,压制时间为5min；
所述步骤(6)中，对磁粉芯进行退火处理，采用氩气作为保护气氛，升温速率为5K/min，加热到1000℃，保温2h，然后随炉冷却到室温。
本发明通过机械球磨工艺可均匀包覆Fe粉，形成厚度可控的核壳结构磁性粉体。
本发明中，将不同粉末进行真空混料处理，保证混料过程中无Fe粉氧化。粉末成形必须要经过压制，脱脂烧结，致密化、热处理等过程，欲达到更优的性能，还需有一定的导向，填充过程以及场的作用。热处理过程需在惰性气体或惰性+还原气氛保护下进行，一般作用为消除应力。
所制备的磁粉芯具有致密度高、内部组织均匀、直流偏磁性能好和功耗相对较低的特点。
本发明制备过程中，需要采用合理的润滑剂辅助成形，根据工艺情况的不同，可以使用针对性的润滑剂。
本发明特点是利用新型技术制备出的高致密性铁硅磁粉芯表现出极为优秀的软磁性能。
与现有技术相比，本发明具有以下优点及有益效果：
(1)制备的磁粉芯密度在7g/cm 3以上，致密度高达90％以上；
(2)加入的Si、Fe 3O 4、Mn-Zn铁氧体经合适配比后，Fe的软磁性能进一步提高了；
(3)所选取材料价格较为便宜，生产成本较低。
附图说明
图1为实施例1所得磁环磁滞曲线图；
图2为实施例1所得磁环磁滞数据结果；
图3为实施例1所得磁环的xps图谱；
图4为实施例1所得磁环的CSONH成分分析结果一；
图5为实施例1所得磁环的CSONH成分分析结果二；
图6为实施例1所得磁环的CSONH成分分析结果三。
具体实施方式
下面结合附图和具体实施例对本发明进行详细说明。
实施例1
(1)原料粉末为还原铁粉，将粘结剂硬脂酸锌制成粉末状，并用30目的筛子过筛。将还原铁粉19g和纳米Mn-Zn铁氧体颗粒0.4g、纳米硅粉0.6g在真空手套箱内干混均匀，混料时间为1h，混料速度为30r/min，
(2)将步骤(1)所得混合粉末与粘结剂在球磨机上混炼制粒，得到软磁合金粉末，粘结剂占步骤(1)所得混合粉末的质量百分比为10％，在行星球磨机中，以50：1的球料比，200rpm的转速，氩气保护气氛条件下球磨2h；
(3)选取纳米Fe 3O 4粉末，球磨成粒度小于30μm的粉末颗粒；
(4)将步骤(2)所得软磁合金粉末与纳米Fe 3O 4加入真空手套箱中均匀混料，在30r/min状态下均匀混合1h；
(5)将步骤(4)所得软磁合金粉末22g与粘结剂5g均匀混合后，在行星球磨机中，以50：1的球料比，200rpm的转速，氩气保护气氛条件下球磨2h，制备软磁粉末；
(6)将包覆好的磁粉利用压机冷压压制成磁环，压制压力为160kN，压制时间为5min；
(7)在真空热处理炉中，对磁粉芯进行退火处理，采用氩气作为保护气氛，升温速率为5K/min，加热到1000℃，保温2h，然后随炉冷却到室温。
按上述方法共制备15个磁环，其中第5个性能更加突出。其性能如下：
所得磁环密度为7.285g/cm 3,在外加磁场Hs取3000A/m时，最大磁导率25.92mH/m，饱和磁感应强度1.949T,矫顽力22.4A/m，其磁滞曲线如图1所示。图2显示的就是这些性能测量结果。
对其做xps图谱分析，结果如图3所示。
对该样品进行CSONH成分分析，所得结果如图4、图5、图6所示。
图4、图5、图6中，样品标识与样品名称的5均表示本实施例所制备的产品。
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和使用发明。熟悉本领域技术的人员显然可以容易地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揭示，不脱离本发明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 (9)

  1. 一种铁硅磁粉芯材料，其特征在于，为复合材料，包括铁粉，以及在铁粉表面包覆的含硅组分、Fe 3O 4颗粒及Mn-Zn铁氧体颗粒，其中，
    铁粉的重量百分含量为≥90wt％，
    Fe 3O 4颗粒的重量百分含量为3wt％-5wt％，
    Mn-Zn铁氧体颗粒的重量百分含量为2wt％，
    复合材料中硅含量不高于5wt％。
  2. 根据权利要求1所述一种铁硅磁粉芯材料，其特征在于，所述铁硅磁粉芯材料为核壳结构，铁粉为核，所述含硅组分、Fe 3O 4颗粒及Mn-Zn铁氧体颗粒包覆在铁粉外面形成壳。
  3. 根据权利要求1所述一种铁硅磁粉芯材料，其特征在于，所述含硅组分为纯硅或含硅铁基的组分，含硅铁基的组分中硅铁含量不低于75wt％。
  4. 根据权利要求1所述一种铁硅磁粉芯材料，其特征在于，所述铁粉为超细球形铁粉，而且所述铁粉具有微量的氧/氮化物掺杂，其中氧/氮化物不超过1wt％。
  5. 根据权利要求1所述一种铁硅磁粉芯材料，其特征在于，所述Fe 3O 4颗粒为粒度小于30μm的粉末颗粒，所述Fe 3O 4颗粒耐高温，为亚铁磁性非连续的纳米级颗粒。
  6. 一种如根据权利要求1-5中任一项所述铁硅磁粉芯材料的制备方法，其特征在于，包括以下步骤：
    (1)将还原铁粉和纳米Mn-Zn铁氧体颗粒、含硅组分在真空手套箱内干混均匀，得到混合粉末，还原铁粉和纳米Mn-Zn铁氧体颗粒、含硅组分的质量比为19:0.4:0.6；
    (2)将步骤(1)所得混合粉末与粘结剂在球磨机上混炼制粒，得到软磁合金粉末，粘结剂占步骤(1)所得混合粉末的质量百分比为10％；
    (3)将软磁合金粉末与纳米Fe 3O 4颗粒加入真空手套箱中均匀混料，软磁合金粉末与纳米Fe 3O 4颗粒的质量比为10:1，
    (4)将步骤(3)所得软磁合金粉末与粘结剂均匀混合后，在行星球磨机中球磨制备软磁粉末，步骤(3)所得软磁合金粉末与粘结剂的质量比为22:5；
    (5)将包覆好的磁粉利用压机冷压压制成磁环；
    (6)在真空热处理炉中，对磁环进行退火处理，采用氩气作为保护气氛，然后随炉冷却到室温。
  7. 根据权利要求6所述一种铁硅磁粉芯材料的制备方法，其特征在于，所述粘结剂为粉末状，并用30目的筛子过筛。
  8. 根据权利要求6所述一种铁硅磁粉芯材料的制备方法，其特征在于，所述粘结剂为硬脂酸锌。
  9. 根据权利要求6所述一种铁硅磁粉芯材料的制备方法，其特征在于，所述步骤(1)中，混料时间为1h，混料速度为30r/min；
    所述步骤(3)中，混料时间为1h，混料速度为30r/min；
    所述步骤(4)中，在行星球磨机中，以50：1的球料比，200rpm的转速，氩气保护气氛条件下球磨2h；
    所述步骤(5)中，压制压力为160kN,压制时间为5min；
    所述步骤(6)中，对磁粉芯进行退火处理，采用氩气作为保护气氛，升温速率为5K/min，加热到1000℃，保温2h，然后随炉冷却到室温。
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