CN105344993A - Method for preparing iron-silicon-aluminum soft magnetic powder core through warm-pressing - Google Patents

Method for preparing iron-silicon-aluminum soft magnetic powder core through warm-pressing Download PDF

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CN105344993A
CN105344993A CN201510888547.4A CN201510888547A CN105344993A CN 105344993 A CN105344993 A CN 105344993A CN 201510888547 A CN201510888547 A CN 201510888547A CN 105344993 A CN105344993 A CN 105344993A
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soft magnetic
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alloy powder
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CN105344993B (en
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黄钧声
王志远
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GUANGZHOU QIDA MATERIAL TECHNOLOGY Co Ltd
Guangdong University of Technology
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GUANGZHOU QIDA MATERIAL TECHNOLOGY Co Ltd
Guangdong University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • B22F1/145Chemical treatment, e.g. passivation or decarburisation
    • B22F1/0003
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16Metallic particles coated with a non-metal
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets 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
    • H01F1/14Magnets 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 metals or alloys
    • H01F1/147Alloys characterised by their composition
    • H01F1/14766Fe-Si based alloys
    • H01F1/14791Fe-Si-Al based alloys, e.g. Sendust
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets 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
    • H01F1/14Magnets 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 metals or alloys
    • H01F1/20Magnets 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 metals or alloys in the form of particles, e.g. powder
    • H01F1/22Magnets 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 metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
    • H01F1/24Magnets 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 metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02Compacting only
    • B22F2003/023Lubricant mixed with the metal powder

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  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a method for preparing an iron-silicon-aluminum soft magnetic powder core through warm-pressing. The method comprises the following steps that (1) initial soft magnetic alloy powder is subjected to passivating treatment through a passivator, and drying is conducted; (2) the dried soft magnetic alloy powder is evenly mixed with a binder; (3) the mixed powder is dried and sieved, and then an insulator is added for mixing coating; (4) the coated soft magnetic alloy powder is mixed with lubricant, the mixture is put into a die, then pressurization and heating are conducted simultaneously, and warm-pressing forming is conducted; and (5) the warm-pressing formed magnetic powder core is subjected to annealing treatment. The initial soft magnetic alloy powder comprises, by weight, 8.5%-10.5% of silicon, 4.5%-6.5% of aluminum, and the balance iron. The lubricant in the step (4) is the mixture of zinc stearate and polyethylene glycol. According to the method, the density and the magnetic conductivity of the prepared soft magnetic powder core can be effectively improved, and the magnetic loss is significantly reduced.

Description

一种温压制备铁硅铝软磁磁粉芯的方法A method for preparing sendust soft magnetic powder core by warm pressing

技术领域technical field

本发明涉及金属材料粉末冶金制造领域,尤其是一种铁硅铝软磁磁粉芯的制备方法及采用此方法制备得到的软磁磁粉芯。The invention relates to the field of powder metallurgy manufacturing of metal materials, in particular to a method for preparing a sendust soft magnetic powder core and a soft magnetic powder core prepared by the method.

背景技术Background technique

磁粉芯是一种通过粉末冶金工艺,将软磁合金粉末与绝缘介质混合压制而成的、具有磁电转换特种功能的新型软磁功能材料。由于磁粉粒度非常小,且在铁磁性粉末颗粒的表面均匀包覆着一层绝缘介质膜,提高了磁粉芯的电阻率,阻碍了磁粉之间的涡流作用,因而涡流损耗很低,适合于较高频率应用(20kHz以上)。此外,磁粉芯还具有较高的饱和磁感应强度、良好的频率特性、较低矫顽力和恒导磁与温度稳定性等优点,使得磁粉芯作为电感滤波器,遏流线圈广泛应用于电子通讯、雷达、电源开关等领域,已经成为软磁材料重要的组成部分。Magnetic powder core is a new type of soft magnetic functional material with special function of magnetoelectric conversion, which is made by mixing and pressing soft magnetic alloy powder and insulating medium through powder metallurgy process. Because the particle size of the magnetic powder is very small, and the surface of the ferromagnetic powder particles is evenly coated with a layer of insulating dielectric film, which improves the resistivity of the magnetic powder core and hinders the eddy current between the magnetic powder, so the eddy current loss is very low, suitable for relatively High frequency applications (above 20kHz). In addition, the magnetic powder core also has the advantages of high saturation magnetic induction, good frequency characteristics, low coercive force, constant magnetic permeability and temperature stability, etc., making the magnetic powder core as an inductance filter, and the choke coil is widely used in electronic communications. , radar, power switch and other fields, has become an important part of soft magnetic materials.

铁硅铝磁粉芯成分为Fe-(8~13%)Si-(4~7%)Al,是一种具备磁电转换功能的新型软磁材料。因其优越的软磁性能和适当的价格,被广泛应用于脉冲变压器、回归变压器、线路噪音滤波器、储能性电感器等的电子器件中。目前铁硅铝磁粉芯处于大规模应用及进一步开发阶段。The composition of sendust magnetic powder core is Fe-(8~13%)Si-(4~7%)Al, which is a new type of soft magnetic material with magnetoelectric conversion function. Because of its superior soft magnetic properties and appropriate price, it is widely used in electronic devices such as pulse transformers, regression transformers, line noise filters, and energy storage inductors. At present, sendust magnetic powder cores are in the stage of large-scale application and further development.

一般来说,压力愈大,压坯的密度越高,磁粉的磁导率越大。但增大压力,对磁粉芯密度的提高是有极限的,压力过大也会导致绝缘层破裂,从而减低绝缘效果。Generally speaking, the greater the pressure, the higher the density of the compact, and the greater the magnetic permeability of the magnetic powder. However, increasing the pressure has a limit to increase the density of the magnetic powder core. Excessive pressure will also cause the insulation layer to rupture, thereby reducing the insulation effect.

金属粉末温压成形技术是通过改造传统的粉末冶金压机,采用特制的粉末加热、粉末输送和模具的加热系统,将混有温压专用的润滑剂、粘结剂的混合粉末加热到一个特定的温度进行压制,再采用传统工艺进行烧结,以获得较高的密度和性能的产品。目前,温压主要用于制备结构材料改善力学性能,应用于研制粉末磁性材料改善软磁磁粉芯性能的研究还很少见。在已公开的专利方面,仅有浙江大学“一种温压成形制备金属软磁复合材料的方法(申请号CN201410246527.2)”和广东工业大学“一种非晶软磁磁粉芯的制备方法(申请号CN201410013455.7)”。诸涛(诸涛.粉末温压成形复合润滑剂及其在制备Fe-Si软磁材料中的应用研究[D].合肥:合肥理工大学,2012)研究了温压应用于Fe-Si软磁合金对其组织结构和力学性能的作用,采用胺基聚合物、硬脂酸盐和乙二醇基聚合物的混合物作为温压润滑剂。H.Shokrollahi等人(H.Shokrollahi.etal..JournalofMagnetismandMagneticMaterials.2007,313:182-186)研究了室温下压制参数对以纯铁粉为主软磁复合材料磁粉芯磁性能的影响,所用润滑剂为硬脂酸锌,结果表明,随着压制压力的增大,粉芯的密度有所增加,磁导率和磁感应强度提高,但同时压力增大引入的位错等缺陷和内应力也增加,因而矫顽力也有所增加。Metal powder warm pressing forming technology is to transform the traditional powder metallurgy press, adopt special powder heating, powder conveying and mold heating system, and heat the mixed powder mixed with special lubricant and binder for warm pressing to a specific The temperature is pressed, and then sintered by the traditional process to obtain a product with higher density and performance. At present, warm pressing is mainly used to prepare structural materials to improve mechanical properties, and it is rare to apply it to the development of powder magnetic materials to improve the properties of soft magnetic powder cores. In terms of published patents, only Zhejiang University "a method for preparing metal soft magnetic composite materials by warm pressing (application number CN201410246527.2)" and Guangdong University of Technology "a method for preparing amorphous soft magnetic powder cores ( Application number CN201410013455.7)". Zhu Tao (Zhu Tao. Research on powder warm pressing composite lubricant and its application in the preparation of Fe-Si soft magnetic materials [D]. Hefei: Hefei University of Technology, 2012) studied the application of warm pressing to Fe-Si soft magnetic materials. The effect of the alloy on its structure and mechanical properties, using a mixture of amine-based polymers, stearate and glycol-based polymers as a warm-pressure lubricant. H.Shokrollahi et al. (H.Shokrollahi.etal..JournalofMagnetismandMagneticMaterials.2007,313:182-186) studied the impact of pressing parameters at room temperature on the magnetic properties of the magnetic powder core of soft magnetic composite materials based on pure iron powder. The lubricant used is Zinc stearate, the results show that with the increase of the pressing pressure, the density of the powder core increases, the magnetic permeability and the magnetic induction intensity increase, but at the same time, the defects such as dislocations and internal stress introduced by the pressure increase also increase, so The coercive force also increased.

软磁材料在电力电子领域得到了广泛应用,目前合金的应用产品大都用冷淬薄带卷绕成磁芯后退火处理。但高频段的损耗特性限制了薄带卷芯应用场合,且经过热处理后的薄带脆性大,在工业领域中,多数情况下需要用此种材料制成满足各种需要的特殊形状。在不损害这种材料优异软磁性能这一优点的前提下,应当明显地降低磁芯的损耗值,将合金带材破碎成磁粉,压制成磁粉芯便可以实现这一目的。目前采用温压制备FeSiAl软磁磁粉芯还未见报道。Soft magnetic materials have been widely used in the field of power electronics. At present, most of the alloy application products are wound into magnetic cores with cold-quenched thin strips and then annealed. However, the loss characteristics of the high-frequency band limit the application of the thin strip core, and the thin strip after heat treatment is brittle. In the industrial field, in most cases, it is necessary to use this material to make special shapes to meet various needs. On the premise of not compromising the excellent soft magnetic properties of this material, the loss value of the magnetic core should be significantly reduced. This goal can be achieved by crushing the alloy strip into magnetic powder and pressing it into a magnetic powder core. At present, there is no report on the preparation of FeSiAl soft magnetic powder cores by warm pressing.

发明内容Contents of the invention

本发明的目的在于基于上述背景而提供一种采用温压成形工艺制备软磁磁粉芯的方法;同时,本发明还提供了采用所述方法制备得到的软磁磁粉芯,所述软磁磁粉芯具有较高的磁导率和较低的磁损耗。The purpose of the present invention is to provide a method for preparing a soft magnetic powder core by using a warm pressing process based on the above background; at the same time, the present invention also provides a soft magnetic powder core prepared by the method, the soft magnetic powder core It has high magnetic permeability and low magnetic loss.

为实现上述目的,本发明采取的技术方案为:一种温压制备铁硅铝软磁磁粉芯的方法,包括以下步骤:In order to achieve the above object, the technical solution adopted by the present invention is: a method for preparing sendust soft magnetic powder core by warm pressing, comprising the following steps:

(1)利用钝化剂对初始软磁合金粉末进行钝化处理,干燥;(1) Utilize passivating agent to carry out passivation treatment to initial soft magnetic alloy powder, dry;

(2)将步骤(1)干燥后的软磁合金粉末与粘结剂均匀混合;(2) uniformly mixing the dried soft magnetic alloy powder and binder in step (1);

(3)将步骤(2)得到的混合粉末干燥过筛,然后添加绝缘剂混合包覆;(3) Dry and sieve the mixed powder obtained in step (2), and then add an insulating agent to mix and coat;

(4)将步骤(3)中包覆好的软磁合金粉末与润滑剂混合,并装入模具内,然后在加压的同时进行加热,温压压制成形;(4) Mix the soft magnetic alloy powder coated in step (3) with a lubricant, and put it into a mould, then heat while pressurizing, and press to form under warm pressure;

(5)对步骤(4)中温压压制成形的磁粉芯进行退火处理;(5) carrying out annealing treatment to the magnetic powder core formed by warm pressing in step (4);

所述初始软磁合金粉末的重量百分含量为:硅8.5~10.5%、铝4.5~6.5%、余量为铁;The weight percent content of the initial soft magnetic alloy powder is: 8.5-10.5% of silicon, 4.5-6.5% of aluminum, and the balance is iron;

所述步骤(4)中的润滑剂为硬脂酸锌和聚乙二醇的混合物。The lubricant in the step (4) is a mixture of zinc stearate and polyethylene glycol.

本发明所述温压制备铁硅铝软磁磁粉芯的方法中,采用特殊润滑剂温压,可以大大改善制备所得磁粉芯的磁导率、磁损耗等软磁性能,进一步提高软磁磁粉芯的性价比,有望在短期内取得可观的经济效益。In the method for preparing sendust soft magnetic powder cores by warm pressing in the present invention, special lubricants are used for warm pressing, which can greatly improve the magnetic permeability, magnetic loss and other soft magnetic properties of the prepared magnetic powder cores, and further improve the soft magnetic powder cores. It is expected to achieve considerable economic benefits in the short term.

作为本发明所述温压制备铁硅铝软磁磁粉芯的方法的优选实施方式,所述初始软磁合金粉末的重量百分含量为:硅9.9%、铝5.5%、余量为铁,采用此成分的初始软磁合金粉末时,制备得到的为FeSiAl软磁磁粉芯,其具有较高的磁导率和较高的性价比。本发明所述软磁合金粉末可采用现有技术手段获得,可直接从市场购买等。本发明中软磁合金粉末优选但不限于上述所述成分的软磁合金粉末,上述成分的软磁合金粉末获得来源广泛,而且具有较高的性价比。As a preferred embodiment of the method for preparing sendust soft magnetic powder cores by warm pressing in the present invention, the weight percent content of the initial soft magnetic alloy powder is: 9.9% of silicon, 5.5% of aluminum, and the balance is iron. When the initial soft magnetic alloy powder of this composition is used, the FeSiAl soft magnetic powder core is prepared, which has higher magnetic permeability and higher cost performance. The soft magnetic alloy powder of the present invention can be obtained by means of existing technologies, and can be purchased directly from the market. In the present invention, the soft magnetic alloy powder is preferably but not limited to the soft magnetic alloy powder of the above-mentioned composition, and the soft magnetic alloy powder of the above-mentioned composition can be obtained from a wide range of sources and has relatively high cost performance.

作为本发明所述温压制备铁硅铝软磁磁粉芯的方法的优选实施方式,所述步骤(4)的润滑剂中,硬脂酸锌和聚乙二醇的质量比为(0.02~5):1。作为本发明所述温压制备铁硅铝软磁磁粉芯的方法的更优选实施方式,所述步骤(4)的润滑剂中,硬脂酸锌和聚乙二醇的质量比为(3~1):2。作为本发明所述温压制备铁硅铝软磁磁粉芯的方法的最优选实施方式,所述步骤(4)的润滑剂中,硬脂酸锌和聚乙二醇的质量比为2:3。本发明所述温压制备铁硅铝软磁磁粉芯的方法,采用特殊的润滑剂,即所述润滑剂由两种物质组成,分别为硬脂酸锌和聚乙二醇,而且二者的质量比为(0.02~5):1。本申请发明人经过大量研究发现,当所述润滑剂采用所述特定配比的硬脂酸锌和聚乙二醇时,采用本发明所述方法制备得到的铁硅铝软磁磁粉芯具有较高的磁导率和很低的磁损耗。尤其是当所述润滑剂中,硬脂酸锌和聚乙二醇的质量比为2:3时,所得到的铁硅铝软磁磁粉芯具有最高的磁导率和最低的磁损耗。As a preferred embodiment of the method for preparing sendust soft magnetic powder cores by warm pressing in the present invention, in the lubricant in the step (4), the mass ratio of zinc stearate to polyethylene glycol is (0.02~5 ):1. As a more preferred embodiment of the method for preparing sendust soft magnetic powder cores by warm pressing in the present invention, in the lubricant of the step (4), the mass ratio of zinc stearate to polyethylene glycol is (3~ 1): 2. As the most preferred embodiment of the method for preparing sendust soft magnetic powder cores by warm pressing in the present invention, in the lubricant of the step (4), the mass ratio of zinc stearate to polyethylene glycol is 2:3 . The method for preparing sendust soft magnetic powder cores by warm pressing in the present invention adopts a special lubricant, that is, the lubricant is composed of two substances, namely zinc stearate and polyethylene glycol, and their The mass ratio is (0.02~5):1. The inventors of the present application have found through a lot of research that when the lubricant uses the specific ratio of zinc stearate and polyethylene glycol, the sendust soft magnetic powder core prepared by the method of the present invention has a relatively high High magnetic permeability and very low magnetic loss. Especially when the mass ratio of zinc stearate to polyethylene glycol in the lubricant is 2:3, the obtained sendust soft magnetic powder core has the highest magnetic permeability and the lowest magnetic loss.

作为本发明所述温压制备铁硅铝软磁磁粉芯的方法的优选实施方式,所述步骤(4)中润滑剂与初始软磁合金粉末的质量比为0.4~2%。作为本发明所述温压制备铁硅铝软磁磁粉芯的方法的更优选实施方式,所述步骤(4)中润滑剂与初始软磁合金粉末的质量比为0.5~1.5%。本申请发明人经过研究发现,本申请中所得软磁磁粉芯的性能不仅与所述润滑剂中硬脂酸锌和聚乙二醇的比例有关,而且还与润滑剂的添加量有关,本申请发明人经过试验发现,当所述润滑剂与初始软磁合金粉末的质量比为0.4~2%时,所得软磁磁粉芯具有较高的密度、磁导率和较低的磁损耗;尤其是当所述润滑剂与初始软磁磁粉芯的质量比为0.5~1.5%时,所得软磁磁粉芯具有更好的密度、磁导率和更低的磁损耗。As a preferred embodiment of the method for preparing sendust soft magnetic powder cores by warm pressing in the present invention, the mass ratio of the lubricant to the initial soft magnetic alloy powder in the step (4) is 0.4-2%. As a more preferred embodiment of the method for preparing sendust soft magnetic powder cores by warm pressing in the present invention, the mass ratio of the lubricant to the initial soft magnetic alloy powder in the step (4) is 0.5-1.5%. The inventors of the present application have found through research that the performance of the soft magnetic powder core obtained in this application is not only related to the ratio of zinc stearate and polyethylene glycol in the lubricant, but also related to the amount of lubricant added. The inventors have found through experiments that when the mass ratio of the lubricant to the initial soft magnetic alloy powder is 0.4 to 2%, the resulting soft magnetic powder core has higher density, magnetic permeability and lower magnetic loss; especially When the mass ratio of the lubricant to the initial soft magnetic powder core is 0.5-1.5%, the obtained soft magnetic powder core has better density, magnetic permeability and lower magnetic loss.

作为本发明温压制备铁硅铝所述软磁磁粉芯的方法的优选实施方式,所述步骤(2)中的粘结剂为硅酸钠、耐高温有机硅树脂的混合物;所述步骤(3)中的绝缘剂为纳米二氧化硅。As a preferred embodiment of the method for preparing the soft magnetic powder core of sendust by warm pressing in the present invention, the binding agent in the step (2) is a mixture of sodium silicate and high temperature resistant organic silicon resin; the step ( 3) The insulating agent in is nano silicon dioxide.

作为本发明所述温压制备铁硅铝软磁磁粉芯的方法的优选实施方式,所述步骤(2)的粘结剂中,硅酸钠和耐高温有机硅树脂的质量比为(4~1):2。作为本发明所述温压制备铁硅铝软磁磁粉芯的方法的更优选实施方式,所述步骤(2)的粘结剂中,硅酸钠和耐高温有机硅树脂的质量比为3:2。本发明所述铁硅铝软磁磁粉芯的制备方法中,所述粘结剂采用特定的两种物质组成,即硅酸钠和耐高温有机硅酸树脂,并且二者的质量比为(4~1):2,本申请发明人经过大量研究发现,当所述粘结剂采用特定配比的硅酸钠和耐高温有机硅树脂组成时,配合所述特定配比的润滑剂及工艺条件,能够得到较高磁导率和很低磁损耗的铁硅铝软磁磁粉芯。As a preferred embodiment of the method for preparing sendust soft magnetic powder cores by warm pressing in the present invention, in the binder of the step (2), the mass ratio of sodium silicate and high temperature resistant organic silicon resin is (4~ 1): 2. As a more preferred embodiment of the method for preparing sendust soft magnetic powder core by warm pressing according to the present invention, in the binder of the step (2), the mass ratio of sodium silicate and high temperature resistant silicone resin is 3: 2. In the preparation method of the sendust soft magnetic powder core of the present invention, the binder is composed of two specific substances, i.e. sodium silicate and high temperature resistant organic silicic acid resin, and the mass ratio of the two is (4 ~1): 2. The inventors of the present application have found through a lot of research that when the binder is composed of sodium silicate and high temperature resistant silicone resin in a specific ratio, the lubricant and process conditions in combination with the specific ratio , can obtain the sendust soft magnetic powder core with high magnetic permeability and very low magnetic loss.

作为本发明所述温压制备铁硅铝软磁磁粉芯的方法的优选实施方式,所述步骤(2)中的粘结剂与初始软磁合金粉末的质量比为1~2%;所述步骤(3)中绝缘剂与初始软磁合金粉末的质量比为0~0.4%。作为本发明所述温压制备铁硅铝软磁磁粉芯的方法的更优选实施方式,所述步骤(2)中的粘结剂与初始软磁合金粉末的质量比为1.5%;所述步骤(3)中绝缘剂与初始软磁合金粉末的质量比为0.1~0.4%。作为本发明所述温压制备铁硅铝软磁磁粉芯的方法的更优选实施方式,所述步骤(3)中绝缘剂与初始软磁合金粉末的质量比为0.2%。As a preferred embodiment of the method for preparing sendust soft magnetic powder cores by warm pressing in the present invention, the mass ratio of the binder in the step (2) to the initial soft magnetic alloy powder is 1 to 2%; In step (3), the mass ratio of the insulating agent to the initial soft magnetic alloy powder is 0-0.4%. As a more preferred embodiment of the method for preparing sendust soft magnetic powder core by warm pressing in the present invention, the mass ratio of the binder in the step (2) to the initial soft magnetic alloy powder is 1.5%; the step (3) The mass ratio of the insulating agent to the initial soft magnetic alloy powder is 0.1-0.4%. As a more preferred embodiment of the method for preparing sendust soft magnetic powder cores by warm pressing in the present invention, the mass ratio of the insulating agent to the initial soft magnetic alloy powder in the step (3) is 0.2%.

作为本发明所述温压制备铁硅铝软磁磁粉芯的方法的优选实施方式,所述步骤(1)中采用的钝化剂为磷酸溶液,所述磷酸溶液的质量百分浓度为0.4~3%(其余为水),所述磷酸溶液与初始软磁合金粉末的质量比为(0.5~1.5):1。当磷酸溶液钝化剂浓度很低时,在粉末颗粒表面生成的磷化膜的厚度很薄,钝化效果不太完全。随着钝化剂浓度的增加和钝化程度的加深,粉末颗粒表面可生成完整、均匀覆盖的磷化膜。但是磷酸溶液钝化剂浓度过高时,磷化膜厚度过大又容易造成其开裂及脱落。作为本发明所述温压制备铁硅铝软磁磁粉芯的方法的更优选实施方式,所述步骤(1)中采用的钝化剂为磷酸溶液,所述磷酸溶液的质量百分浓度为0.7%。当所述磷酸溶液钝化剂的质量百分浓度为0.7%时,能够达到最佳的成膜状态。As a preferred embodiment of the method for preparing sendust soft magnetic powder cores by warm pressing in the present invention, the passivating agent used in the step (1) is a phosphoric acid solution, and the mass percent concentration of the phosphoric acid solution is 0.4- 3% (the rest is water), the mass ratio of the phosphoric acid solution to the initial soft magnetic alloy powder is (0.5-1.5):1. When the concentration of the passivating agent in the phosphoric acid solution is very low, the thickness of the phosphating film formed on the surface of the powder particles is very thin, and the passivation effect is not complete. With the increase of passivating agent concentration and the deepening of passivation degree, a complete and uniform phosphating film can be formed on the surface of powder particles. However, when the concentration of the passivating agent in the phosphoric acid solution is too high, the thickness of the phosphating film is too large and it is easy to cause cracking and falling off. As a more preferred embodiment of the method for preparing sendust soft magnetic powder cores by warm pressing in the present invention, the passivating agent adopted in the step (1) is a phosphoric acid solution, and the mass percent concentration of the phosphoric acid solution is 0.7 %. When the mass percent concentration of the phosphoric acid solution passivator is 0.7%, the best film-forming state can be achieved.

作为本发明所述温压制备铁硅铝软磁磁粉芯的方法的优选实施方式,所述步骤(4)中温压压制成形的压制压力为500~1200MPa,压制温度为60~150℃。压制压力过小时,磁粉芯密度不够高、性能不好,压制压力过大时,模具容易损坏。压制温度过低时,固体润滑剂尚未熔化造成温压密度提高效果不明显;温压温度过高时,润滑膜粘度降低,造成粉末颗粒间直接接触,导致密度反而下降,而且内应力高,不利于改善软磁性能。本发明所述软磁磁粉芯的制备方法,所述温压压制过程中,采用所述的压制压力和压制温度,能够在温压温度下以较小的压制压力获得较高的密度,而且所得的磁粉芯内应力低,有利于获得较高的磁导率和较低的损耗,另外可以降低压制压力,较少模具损耗,经济效应显著。As a preferred embodiment of the method for preparing sendust soft magnetic powder cores by warm pressing in the present invention, the pressing pressure of warm pressing in step (4) is 500-1200 MPa, and the pressing temperature is 60-150°C. If the pressing pressure is too small, the density of the magnetic powder core is not high enough and the performance is not good. When the pressing pressure is too high, the mold is easily damaged. When the pressing temperature is too low, the solid lubricant has not yet melted, so the effect of increasing the temperature and pressure density is not obvious; when the temperature and pressure temperature is too high, the viscosity of the lubricating film decreases, resulting in direct contact between powder particles, resulting in a decrease in density, and high internal stress. It is beneficial to improve the soft magnetic properties. In the preparation method of the soft magnetic powder core of the present invention, in the warm-pressing process, the pressing pressure and the pressing temperature are used to obtain a higher density at a lower pressing pressure at the warm-pressing temperature, and the obtained The internal stress of the magnetic powder core is low, which is beneficial to obtain higher magnetic permeability and lower loss. In addition, it can reduce the pressing pressure, reduce the mold loss, and the economic effect is remarkable.

作为本发明所述温压制备铁硅铝软磁磁粉芯的方法的优选实施方式,所述步骤(5)中退火处理的退火温度为550~750℃,退火时间为0.5~1.5小时。退火温度较低、时间较短,则消除内应力效果不明显,不利于改善磁性能;退火温度过高,则磁粉芯易于氧化变质、耗费能源,而且还可能造成粉末颗粒之间绝缘层破坏,恶化磁性能。As a preferred embodiment of the method for preparing sendust soft magnetic powder cores by warm pressing in the present invention, the annealing temperature of the annealing treatment in the step (5) is 550-750° C., and the annealing time is 0.5-1.5 hours. If the annealing temperature is low and the time is short, the effect of eliminating internal stress is not obvious, which is not conducive to improving the magnetic properties; if the annealing temperature is too high, the magnetic powder core is easy to oxidize and deteriorate, consumes energy, and may also cause damage to the insulating layer between powder particles. Deterioration of magnetic properties.

同时,本发明还提供一种具有较高磁导率和较低磁损耗的铁硅铝软磁磁粉芯,为实现此目的,本发明采取的技术方案为:一种铁硅铝软磁磁粉芯,其采用如上所述方法制备得到。At the same time, the present invention also provides a sendust soft magnetic powder core with higher magnetic permeability and lower magnetic loss. To achieve this purpose, the technical solution adopted by the present invention is: a sendust soft magnetic powder core , which was prepared as described above.

本发明所述铁硅铝软磁磁粉芯的制备方法,将粉末冶金温压新技术应用于非晶软磁磁粉芯的制备,通过大量试验摸索,最终选择所述特定的润滑剂和其他加料选择及加料顺序、压制压力、压制温度等的结合,这些整体结合组成的方法技术方案,制备出的非晶软磁磁粉芯具有较高的密度和较低的内应力,所得磁粉芯具有较高的磁导率和很低的磁损耗。本发明所述软磁磁粉芯的制备方法,与现有的软磁磁粉芯制备技术相比,本发明方法能在温压温度下以较小的压制压力获得较高的密度,而且磁粉芯内应力低,从而有利于磁畴壁移动和磁畴转动,有利获得较高的磁导率和较低的损耗。而且本发明的方法可降低压制压力,减少模具损耗,具有较显著的经济效应。The preparation method of the sendust soft magnetic powder core of the present invention applies the new technology of powder metallurgy warm pressing to the preparation of amorphous soft magnetic powder core, and finally selects the specific lubricant and other feeding options through a large number of experiments And the combination of feeding sequence, pressing pressure, pressing temperature, etc., the method technical scheme composed of these overall combination, the prepared amorphous soft magnetic magnetic powder core has higher density and lower internal stress, and the obtained magnetic powder core has higher Magnetic permeability and very low magnetic loss. The preparation method of the soft magnetic magnetic powder core of the present invention, compared with the existing soft magnetic magnetic powder core preparation technology, the inventive method can obtain higher density with a smaller pressing pressure under the warm-pressing temperature, and the magnetic powder core The stress is low, which is conducive to the movement of the magnetic domain wall and the rotation of the magnetic domain, and is beneficial to obtain higher magnetic permeability and lower loss. Moreover, the method of the invention can reduce pressing pressure, reduce mold loss, and has significant economic effect.

具体实施方式detailed description

为更好的说明本发明的目的、技术方案和优点,下面将结合具体实施例对本发明作进一步说明。In order to better illustrate the purpose, technical solutions and advantages of the present invention, the present invention will be further described below in conjunction with specific examples.

以下实施例中,所述初始软磁合金粉末的重量百分含量均为:硅8.5~10.5%、铝4.5~6.5%、余量为铁。更佳地,以下实施例中,所述初始软磁合金粉末的重量百分含量均为:硅9.9%、铝5.5%、余量为铁。In the following examples, the weight percentages of the initial soft magnetic alloy powder are: 8.5-10.5% silicon, 4.5-6.5% aluminum, and iron as the balance. More preferably, in the following examples, the weight percentages of the initial soft magnetic alloy powder are: 9.9% silicon, 5.5% aluminum, and iron as the balance.

实施例1Example 1

本发明温压制备铁硅铝软磁磁粉芯的方法的一种实施例,本实施例所述软磁磁粉芯的制备方法包括以下步骤:An embodiment of the method for preparing sendust soft magnetic powder core by warm pressing in the present invention, the preparation method of the soft magnetic powder core described in this embodiment comprises the following steps:

(1)利用质量百分浓度为0.4%的磷酸溶液对初始软磁合金粉末进行钝化处理,干燥;所述磷酸溶液与初始软磁合金粉末的质量比为0.5:1;(1) Passivate the initial soft magnetic alloy powder with a phosphoric acid solution with a mass percent concentration of 0.4%, and dry it; the mass ratio of the phosphoric acid solution to the initial soft magnetic alloy powder is 0.5:1;

(2)将步骤(1)干燥后的软磁合金粉末与粘结剂均匀混合,所述粘结剂与初始软磁合金粉末的质量比为2%,所述粘结剂为硅酸钠、耐高温有机硅树脂的混合物,且所述硅酸钠、耐高温有机硅树脂的质量比为2:1;(2) The soft magnetic alloy powder after step (1) is dried is mixed evenly with binding agent, and the mass ratio of described binding agent and initial soft magnetic alloy powder is 2%, and described binding agent is sodium silicate, A mixture of high temperature resistant silicone resin, and the mass ratio of the sodium silicate and high temperature resistant silicone resin is 2:1;

(3)将步骤(2)得到的混合粉末干燥过筛,然后添加纳米二氧化硅混合包覆,所述纳米二氧化硅与初始软磁合金粉末的质量比为0.1%;(3) Dry and sieve the mixed powder obtained in step (2), then add nano silicon dioxide to mix and coat, the mass ratio of the nano silicon dioxide to the initial soft magnetic alloy powder is 0.1%;

(4)将步骤(3)中包覆好的软磁合金粉末与润滑剂混合,并装入模具内,然后在加压的同时进行加热,在压力为500MPa、温度为150℃下温压压制成形;所述润滑剂与初始软磁合金粉末的质量比为1%,所述润滑剂为硬脂酸锌和聚乙二醇的混合物,且所述硬脂酸锌和聚乙二醇的质量比为0.02:1;(4) Mix the soft magnetic alloy powder coated in step (3) with a lubricant, put it into a mold, and then heat it while pressurizing, and press it under warm pressure at a pressure of 500MPa and a temperature of 150°C Forming; the mass ratio of the lubricant to the initial soft magnetic alloy powder is 1%, the lubricant is a mixture of zinc stearate and polyethylene glycol, and the mass ratio of the zinc stearate and polyethylene glycol The ratio is 0.02:1;

(5)对步骤(4)中温压压制成形的磁粉芯进行退火处理,退火温度为550℃,退火时间为0.5h。(5) Perform annealing treatment on the magnetic powder core formed by warm pressing in step (4), the annealing temperature is 550°C, and the annealing time is 0.5h.

实施例2Example 2

本发明温压制备铁硅铝软磁磁粉芯的方法的一种实施例,本实施例所述软磁磁粉芯的制备方法包括以下步骤:An embodiment of the method for preparing sendust soft magnetic powder core by warm pressing in the present invention, the preparation method of the soft magnetic powder core described in this embodiment comprises the following steps:

(1)利用质量百分浓度为1%的磷酸溶液对初始软磁合金粉末进行钝化处理,干燥;所述磷酸溶液与初始软磁合金粉末的质量比为0.6:1;(1) Passivate the initial soft magnetic alloy powder with a phosphoric acid solution with a mass percent concentration of 1%, and dry it; the mass ratio of the phosphoric acid solution to the initial soft magnetic alloy powder is 0.6:1;

(2)将步骤(1)干燥后的软磁合金粉末与粘结剂均匀混合,所述粘结剂与初始软磁合金粉末的质量比为1.8%,所述粘结剂为硅酸钠、耐高温有机硅树脂的混合物,且所述硅酸钠、耐高温有机硅树脂的质量比为3:2;(2) The soft magnetic alloy powder after step (1) is dried is mixed evenly with binding agent, and the mass ratio of described binding agent and initial soft magnetic alloy powder is 1.8%, and described binding agent is sodium silicate, A mixture of high temperature resistant silicone resin, and the mass ratio of the sodium silicate and high temperature resistant silicone resin is 3:2;

(3)将步骤(2)得到的混合粉末干燥过筛,然后添加纳米二氧化硅混合包覆,所述纳米二氧化硅与初始软磁合金粉末的质量比为0.15%;(3) Dry and sieve the mixed powder obtained in step (2), then add nano silicon dioxide to mix and coat, the mass ratio of the nano silicon dioxide to the initial soft magnetic alloy powder is 0.15%;

(4)将步骤(3)中包覆好的软磁合金粉末与润滑剂混合,并装入模具内,然后在加压的同时进行加热,在压力为800MPa、温度为90℃下温压压制成形;所述润滑剂与初始软磁合金粉末的质量比为2%,所述润滑剂为硬脂酸锌和聚乙二醇的混合物,且所述硬脂酸锌和聚乙二醇的质量比为0.4:1;(4) Mix the soft magnetic alloy powder coated in step (3) with lubricant, and put it into the mold, then heat it while pressurizing, and press it under warm pressure at a pressure of 800MPa and a temperature of 90°C Shaping; the mass ratio of the lubricant to the initial soft magnetic alloy powder is 2%, the lubricant is a mixture of zinc stearate and polyethylene glycol, and the mass ratio of the zinc stearate and polyethylene glycol The ratio is 0.4:1;

(5)对步骤(4)中温压压制成形的磁粉芯进行退火处理,退火温度为600℃,退火时间为0.6h。(5) Perform annealing treatment on the magnetic powder core formed by warm pressing in step (4), the annealing temperature is 600°C, and the annealing time is 0.6h.

实施例3Example 3

本发明温压制备铁硅铝软磁磁粉芯的方法的一种实施例,本实施例所述软磁磁粉芯的制备方法包括以下步骤:An embodiment of the method for preparing sendust soft magnetic powder core by warm pressing in the present invention, the preparation method of the soft magnetic powder core described in this embodiment comprises the following steps:

(1)利用质量百分浓度为2%的磷酸溶液对初始软磁合金粉末进行钝化处理,干燥;所述磷酸溶液与初始软磁合金粉末的质量比为0.8:1;(1) Passivate the initial soft magnetic alloy powder with a phosphoric acid solution with a mass percent concentration of 2%, and dry it; the mass ratio of the phosphoric acid solution to the initial soft magnetic alloy powder is 0.8:1;

(2)将步骤(1)干燥后的软磁合金粉末与粘结剂均匀混合,所述粘结剂与初始软磁合金粉末的质量比为1.6%,所述粘结剂为硅酸钠、耐高温有机硅树脂的混合物,且所述硅酸钠、耐高温有机硅树脂的质量比为3:2;(2) The soft magnetic alloy powder after step (1) is dried is mixed evenly with binder, and the mass ratio of described binder and initial soft magnetic alloy powder is 1.6%, and described binder is sodium silicate, A mixture of high temperature resistant silicone resin, and the mass ratio of the sodium silicate and high temperature resistant silicone resin is 3:2;

(3)将步骤(2)得到的混合粉末干燥过筛,然后添加纳米二氧化硅混合包覆,所述纳米二氧化硅与初始软磁合金粉末的质量比为0.2%;(3) Dry and sieve the mixed powder obtained in step (2), then add nano silicon dioxide to mix and coat, the mass ratio of the nano silicon dioxide to the initial soft magnetic alloy powder is 0.2%;

(4)将步骤(3)中包覆好的软磁合金粉末与润滑剂混合,并装入模具内,然后在加压的同时进行加热,在压力为600MPa、温度为120℃下温压压制成形;所述润滑剂与初始软磁合金粉末的质量比为0.5%,所述润滑剂为硬脂酸锌和聚乙二醇的混合物,且所述硬脂酸锌和聚乙二醇的质量比为1:2;(4) Mix the soft magnetic alloy powder coated in step (3) with lubricant, and put it into the mold, then heat it while pressurizing, and press it under warm pressure at a pressure of 600MPa and a temperature of 120°C Forming; the mass ratio of the lubricant to the initial soft magnetic alloy powder is 0.5%, the lubricant is a mixture of zinc stearate and polyethylene glycol, and the mass ratio of the zinc stearate and polyethylene glycol The ratio is 1:2;

(5)对步骤(4)中温压压制成形的磁粉芯进行退火处理,退火温度为630℃,退火时间为1h。(5) Perform annealing treatment on the magnetic powder core formed by warm pressing in step (4), the annealing temperature is 630° C., and the annealing time is 1 h.

实施例4Example 4

本发明温压制备铁硅铝软磁磁粉芯的方法的一种实施例,本实施例所述软磁磁粉芯的制备方法包括以下步骤:An embodiment of the method for preparing sendust soft magnetic powder core by warm pressing in the present invention, the preparation method of the soft magnetic powder core described in this embodiment comprises the following steps:

(1)利用质量百分浓度为0.7%的磷酸溶液对初始软磁合金粉末进行钝化处理,干燥;所述磷酸溶液与初始软磁合金粉末的质量比为1:1;(1) Passivate the initial soft magnetic alloy powder with a phosphoric acid solution with a mass percent concentration of 0.7%, and dry it; the mass ratio of the phosphoric acid solution to the initial soft magnetic alloy powder is 1:1;

(2)将步骤(1)干燥后的软磁合金粉末与粘结剂均匀混合,所述粘结剂与初始软磁合金粉末的质量比为1.5%,所述粘结剂为硅酸钠、耐高温有机硅树脂的混合物,且所述硅酸钠、耐高温有机硅树脂的质量比为3:2;(2) The soft magnetic alloy powder after step (1) is dried is mixed evenly with binding agent, and the mass ratio of described binding agent and initial soft magnetic alloy powder is 1.5%, and described binding agent is sodium silicate, A mixture of high temperature resistant silicone resin, and the mass ratio of the sodium silicate and high temperature resistant silicone resin is 3:2;

(3)将步骤(2)得到的混合粉末干燥过筛,然后添加纳米二氧化硅混合包覆,所述纳米二氧化硅与初始软磁合金粉末的质量比为0.2%;(3) Dry and sieve the mixed powder obtained in step (2), then add nano silicon dioxide to mix and coat, the mass ratio of the nano silicon dioxide to the initial soft magnetic alloy powder is 0.2%;

(4)将步骤(3)中包覆好的软磁合金粉末与润滑剂混合,并装入模具内,然后在加压的同时进行加热,在压力为1100MPa、温度为100℃下温压压制成形;所述润滑剂与初始软磁合金粉末的质量比为1.3%,所述润滑剂为硬脂酸锌和聚乙二醇的混合物,且所述硬脂酸锌和聚乙二醇的质量比为2:3;(4) Mix the soft magnetic alloy powder coated in step (3) with lubricant, and put it into the mold, then heat it while pressurizing, and press it under warm pressure at a pressure of 1100MPa and a temperature of 100°C Forming; the mass ratio of the lubricant to the initial soft magnetic alloy powder is 1.3%, the lubricant is a mixture of zinc stearate and polyethylene glycol, and the mass ratio of the zinc stearate and polyethylene glycol The ratio is 2:3;

(5)对步骤(4)中温压压制成形的磁粉芯进行退火处理,退火温度为680℃,退火时间为1h。(5) Perform annealing treatment on the magnetic powder core formed by warm pressing in step (4), the annealing temperature is 680° C., and the annealing time is 1 h.

实施例5Example 5

本发明温压制备铁硅铝软磁磁粉芯的方法的一种实施例,本实施例所述软磁磁粉芯的制备方法包括以下步骤:An embodiment of the method for preparing sendust soft magnetic powder core by warm pressing in the present invention, the preparation method of the soft magnetic powder core described in this embodiment comprises the following steps:

(1)利用质量百分浓度为3%的磷酸溶液对初始软磁合金粉末进行钝化处理,干燥;所述磷酸溶液与初始软磁合金粉末的质量比为1.2:1;(1) Passivate the initial soft magnetic alloy powder with a phosphoric acid solution with a mass percent concentration of 3%, and dry it; the mass ratio of the phosphoric acid solution to the initial soft magnetic alloy powder is 1.2:1;

(2)将步骤(1)干燥后的软磁合金粉末与粘结剂均匀混合,所述粘结剂与初始软磁合金粉末的质量比为1.2%,所述粘结剂为硅酸钠、耐高温有机硅树脂的混合物,且所述硅酸钠、耐高温有机硅树脂的质量比为2:3;(2) The soft magnetic alloy powder after step (1) is dried is mixed evenly with binder, and the mass ratio of described binder and initial soft magnetic alloy powder is 1.2%, and described binder is sodium silicate, A mixture of high temperature resistant silicone resin, and the mass ratio of the sodium silicate and high temperature resistant silicone resin is 2:3;

(3)将步骤(2)得到的混合粉末干燥过筛,然后添加纳米二氧化硅混合包覆,所述纳米二氧化硅与初始软磁合金粉末的质量比为0.3%;(3) Dry and sieve the mixed powder obtained in step (2), then add nano silicon dioxide to mix and coat, the mass ratio of the nano silicon dioxide to the initial soft magnetic alloy powder is 0.3%;

(4)将步骤(3)中包覆好的软磁合金粉末与润滑剂混合,并装入模具内,然后在加压的同时进行加热,在压力为1000MPa、温度为80℃下温压压制成形;所述润滑剂与初始软磁合金粉末的质量比为1.5%,所述润滑剂为硬脂酸锌和聚乙二醇的混合物,且所述硬脂酸锌和聚乙二醇的质量比为3:2;(4) Mix the soft magnetic alloy powder coated in step (3) with a lubricant, put it into a mold, and then heat it while pressurizing, and press it under warm pressure at a pressure of 1000MPa and a temperature of 80°C Forming; the mass ratio of the lubricant to the initial soft magnetic alloy powder is 1.5%, the lubricant is a mixture of zinc stearate and polyethylene glycol, and the mass ratio of the zinc stearate and polyethylene glycol The ratio is 3:2;

(5)对步骤(4)中温压压制成形的磁粉芯进行退火处理,退火温度为700℃,退火时间为1.3h。(5) Perform annealing treatment on the magnetic powder core formed by warm pressing in step (4), the annealing temperature is 700°C, and the annealing time is 1.3h.

实施例6Example 6

本发明温压制备铁硅铝软磁磁粉芯的方法的一种实施例,本实施例所述软磁磁粉芯的制备方法包括以下步骤:An embodiment of the method for preparing sendust soft magnetic powder core by warm pressing in the present invention, the preparation method of the soft magnetic powder core described in this embodiment comprises the following steps:

(1)利用质量百分浓度为1.5%的磷酸溶液对初始软磁合金粉末进行钝化处理,干燥;所述磷酸溶液与初始软磁合金粉末的质量比为1.5:1;(1) Passivate the initial soft magnetic alloy powder with a phosphoric acid solution with a mass percent concentration of 1.5%, and dry it; the mass ratio of the phosphoric acid solution to the initial soft magnetic alloy powder is 1.5:1;

(2)将步骤(1)干燥后的软磁合金粉末与粘结剂均匀混合,所述粘结剂与初始软磁合金粉末的质量比为1%,所述粘结剂为硅酸钠、耐高温有机硅树脂的混合物,且所述硅酸钠、耐高温有机硅树脂的质量比为1:2;(2) The soft magnetic alloy powder after step (1) is dried is mixed evenly with binding agent, and the mass ratio of described binding agent and initial soft magnetic alloy powder is 1%, and described binding agent is sodium silicate, A mixture of high temperature resistant silicone resin, and the mass ratio of the sodium silicate and high temperature resistant silicone resin is 1:2;

(3)将步骤(2)得到的混合粉末干燥过筛,然后添加纳米二氧化硅混合包覆,所述纳米二氧化硅与初始软磁合金粉末的质量比为0.4%;(3) Dry and sieve the mixed powder obtained in step (2), then add nano silicon dioxide to mix and coat, the mass ratio of the nano silicon dioxide to the initial soft magnetic alloy powder is 0.4%;

(4)将步骤(3)中包覆好的软磁合金粉末与润滑剂混合,并装入模具内,然后在加压的同时进行加热,在压力为1200MPa、温度为60℃下温压压制成形;所述润滑剂与初始软磁合金粉末的质量比为0.4%,所述润滑剂为硬脂酸锌和聚乙二醇的混合物,且所述硬脂酸锌和聚乙二醇的质量比为5:1;(4) Mix the soft magnetic alloy powder coated in step (3) with lubricant, and put it into the mold, then heat it while pressurizing, and press it under warm pressure at a pressure of 1200MPa and a temperature of 60°C Shaping; the mass ratio of the lubricant to the initial soft magnetic alloy powder is 0.4%, the lubricant is a mixture of zinc stearate and polyethylene glycol, and the mass ratio of the zinc stearate and polyethylene glycol The ratio is 5:1;

(5)对步骤(4)中温压压制成形的磁粉芯进行退火处理,退火温度为750℃,退火时间为1.5h。(5) Perform annealing treatment on the magnetic powder core formed by warm pressing in step (4), the annealing temperature is 750°C, and the annealing time is 1.5h.

实施例7Example 7

本发明所述方法制备得到的铁硅铝软磁磁粉芯的性能试验Performance test of the sendust soft magnetic powder core prepared by the method of the present invention

分别对实施例1~6制备得到的铁硅铝软磁磁粉芯的性能进行测试,分别测试每组所得铁硅铝软磁磁粉芯的密度、磁导率(50kHz时和1000kHz时)、磁损耗(50kHz/0.05T),测试结果见表1。The properties of the sendust soft magnetic powder cores prepared in Examples 1 to 6 are tested respectively, and the density, magnetic permeability (when 50kHz and 1000kHz), magnetic loss of each group of gained sendust soft magnetic powder cores are tested respectively (50kHz/0.05T), the test results are shown in Table 1.

表1铁硅铝软磁磁粉芯的性能结果Table 1 Performance results of sendust soft magnetic powder core

由上述结果可看出,上述实施例1~6制备得到的铁硅铝软磁磁粉芯,具有较高的密度、较高的磁导率和较低的磁损耗,尤其是实施例4制备得到的铁硅铝软磁磁粉芯,具有特别高的磁导率和很低的磁损耗。It can be seen from the above results that the sendust soft magnetic powder cores prepared in Examples 1 to 6 above have higher density, higher magnetic permeability and lower magnetic loss, especially those prepared in Example 4. Sensitive soft magnetic powder core has particularly high magnetic permeability and low magnetic loss.

实施例8Example 8

本发明所述制备方法中,润滑剂中硬脂酸锌和聚乙二醇的质量比对所得铁硅铝软磁磁粉芯的性能影响试验In the preparation method of the present invention, the mass ratio of zinc stearate and polyethylene glycol in the lubricant affects the performance of the obtained sendust soft magnetic powder core

本实施例试验共设9组,每组的润滑剂中,硬脂酸锌与聚乙二醇的质量比见表2所示。There are 9 groups in the test of this embodiment. In the lubricant of each group, the mass ratio of zinc stearate to polyethylene glycol is shown in Table 2.

表2硬脂酸锌与聚乙二醇的质量比The mass ratio of zinc stearate and polyethylene glycol of table 2

组别group 硬脂酸锌:聚乙二醇Zinc stearate: polyethylene glycol 试验组1Test group 1 0.02:10.02:1

试验组2Test group 2 0.1:10.1:1 试验组3Test group 3 1:51:5 试验组4Test group 4 2:32:3 试验组5Test group 5 1:11:1 试验组6Test group 6 3:23:2 试验组7Test group 7 3:13:1 试验组8Test group 8 4:14:1 试验组9Test group 9 5:15:1

本实施例中,试验组1~9均采用本发明所述方法制备铁硅铝软磁磁粉芯,试验组1~9中,除润滑剂中硬脂酸锌、聚乙二醇的质量比不同外,其余条件均相同。In this embodiment, test groups 1 to 9 all adopt the method of the present invention to prepare sendust soft magnetic powder cores. In test groups 1 to 9, the mass ratios of zinc stearate and polyethylene glycol in the lubricant are different. Other than that, the other conditions are the same.

分别测试试验组1~9制备得到的铁硅铝软磁磁粉芯的密度、磁导率(50kHz时和1000kHz时)、磁损耗(50kHz/0.05T),测试结果见表3所示。The density, permeability (at 50kHz and 1000kHz), and magnetic loss (50kHz/0.05T) of the sendust soft magnetic powder cores prepared by test groups 1 to 9 were tested respectively. The test results are shown in Table 3.

表3铁硅铝软磁磁粉芯的性能测试结果Table 3 Performance test results of sendust soft magnetic powder core

由表3结果可看出,本发明所述铁硅铝软磁磁粉芯的制备方法中,润滑剂中硬脂酸锌与聚乙二醇的质量比对所得软磁磁粉芯的密度、磁导率和磁损耗有直接的影响。当所述润滑剂中,硬脂酸锌和聚乙二醇的质量比为(3~1):2时,所得铁硅铝软磁磁粉芯具有较高的密度、较高的磁导率和较低的磁损耗。尤其是当所述润滑剂中,硬脂酸锌和聚乙二醇的质量比为2:3时,所得铁硅铝软磁磁粉芯具有更高的密度、更高的磁导率和更低的磁损耗。As can be seen from the results in Table 3, in the preparation method of the sendust soft magnetic powder core of the present invention, the mass ratio of zinc stearate and polyethylene glycol in the lubricant to the density and permeability of the obtained soft magnetic powder core rate and magnetic loss have a direct impact. When in the lubricant, the mass ratio of zinc stearate to polyethylene glycol is (3~1):2, the obtained sendust soft magnetic powder core has higher density, higher magnetic permeability and Lower magnetic loss. Especially when in the lubricant, the mass ratio of zinc stearate and polyethylene glycol is 2:3, the gained sendust soft magnetic powder core has higher density, higher magnetic permeability and lower magnetic loss.

实施例9Example 9

本发明所述制备方法中,润滑剂的含量对所得铁硅铝软磁磁粉芯的性能影响试验In the preparation method of the present invention, the test of the influence of the content of the lubricant on the performance of the obtained sendust soft magnetic powder core

本实施例试验共设7组,每组的润滑剂中,硬脂酸锌与聚乙二醇的质量比均为2:3。本实施例中,试验组1~7均采用本发明所述方法制备铁硅铝软磁磁粉芯,试验组1~7中,除润滑剂与初始软磁合金粉末的质量比不同外,其余条件均相同。每组中润滑剂与初始软磁合金粉末的质量比见表4所示。There are 7 groups in the test of this embodiment, and in the lubricant of each group, the mass ratio of zinc stearate to polyethylene glycol is 2:3. In this embodiment, test groups 1 to 7 all adopt the method of the present invention to prepare sendust soft magnetic powder cores. In test groups 1 to 7, except that the mass ratio of the lubricant to the initial soft magnetic alloy powder is different, the remaining conditions are the same. The mass ratio of lubricant to initial soft magnetic alloy powder in each group is shown in Table 4.

表4润滑剂与初始软磁合金粉末的质量比Table 4 Mass ratio of lubricant to initial soft magnetic alloy powder

组别group 润滑剂:初始软磁合金粉末Lubricant: primary soft magnetic alloy powder 试验组1Test group 1 0.4%0.4% 试验组2Test group 2 0.6%0.6% 试验组3Test group 3 0.8%0.8% 试验组4Test group 4 1%1% 试验组5Test group 5 1.3%1.3% 试验组6Test group 6 1.6%1.6% 试验组7Test group 7 2%2%

分别测试试验组1~7制备得到的软磁磁粉芯的密度、磁导率(50kHz时和1000kHz时)、磁损耗(50kHz/0.05T),测试结果见表5所示.The density, permeability (at 50kHz and 1000kHz), and magnetic loss (50kHz/0.05T) of the soft magnetic powder cores prepared by test groups 1 to 7 were tested respectively. The test results are shown in Table 5.

表5软磁磁粉芯的性能测试结果Table 5 Performance test results of soft magnetic powder cores

由表5结果可看出,本发明所述软磁磁粉芯的制备方法中,润滑剂的用量也对软磁磁粉芯的密度、磁导率和磁损耗有直接的影响。当所述润滑剂与初始软磁合金粉末的质量比为0.5~1.5%时,所得软磁磁粉芯具有较高的密度、磁导率和较低的磁损耗。尤其是当所述润滑剂与初始软磁合金粉末的质量比为1.3%时,所得软磁磁粉芯具有更高的密度、磁导率和更低的磁损耗。It can be seen from the results in Table 5 that in the preparation method of the soft magnetic powder core of the present invention, the amount of lubricant also has a direct impact on the density, permeability and magnetic loss of the soft magnetic powder core. When the mass ratio of the lubricant to the initial soft magnetic alloy powder is 0.5-1.5%, the obtained soft magnetic powder core has higher density, magnetic permeability and lower magnetic loss. Especially when the mass ratio of the lubricant to the initial soft magnetic alloy powder is 1.3%, the obtained soft magnetic powder core has higher density, magnetic permeability and lower magnetic loss.

最后所应当说明的是,以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制,尽管参照较佳实施例对本发明作了详细说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的实质和范围。Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than limit the protection scope of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that The technical solution of the present invention can be modified or equivalently replaced without departing from the spirit and scope of the technical solution of the present invention.

Claims (10)

1.一种温压制备铁硅铝软磁磁粉芯的方法,其特征在于,包括以下步骤:1. A method for preparing sendust soft magnetic powder core by warm pressing, is characterized in that, comprises the following steps: (1)利用钝化剂对初始软磁合金粉末进行钝化处理,干燥;(1) Utilize passivating agent to carry out passivation treatment to initial soft magnetic alloy powder, dry; (2)将步骤(1)干燥后的软磁合金粉末与粘结剂均匀混合;(2) uniformly mixing the dried soft magnetic alloy powder and binder in step (1); (3)将步骤(2)得到的混合粉末干燥过筛,然后添加绝缘剂混合包覆;(3) Dry and sieve the mixed powder obtained in step (2), and then add an insulating agent to mix and coat; (4)将步骤(3)中包覆好的软磁合金粉末与润滑剂混合,并装入模具内,然后在加压的同时进行加热,温压压制成形;(4) Mix the soft magnetic alloy powder coated in step (3) with a lubricant, and put it into a mould, then heat while pressurizing, and press to form under warm pressure; (5)对步骤(4)中温压压制成形的磁粉芯进行退火处理;(5) carrying out annealing treatment to the magnetic powder core formed by warm pressing in step (4); 所述初始软磁合金粉末的重量百分含量为:硅8.5~10.5%、铝4.5~6.5%、余量为铁;The weight percent content of the initial soft magnetic alloy powder is: 8.5-10.5% of silicon, 4.5-6.5% of aluminum, and the balance is iron; 所述步骤(4)中的润滑剂为硬脂酸锌和聚乙二醇的混合物。The lubricant in the step (4) is a mixture of zinc stearate and polyethylene glycol. 2.如权利要求1所述的温压制备铁硅铝软磁磁粉芯的方法,其特征在于,所述步骤(4)的润滑剂中,硬脂酸锌和聚乙二醇的质量比为(0.02~5):1;优选地,所述步骤(4)的润滑剂中,硬脂酸锌和聚乙二醇的质量比为(3~1):2;更优选地,所述步骤(4)的润滑剂中,硬脂酸锌和聚乙二醇的质量比为2:3。2. warm pressing as claimed in claim 1 prepares the method for sendust soft magnetic powder core, it is characterized in that, in the lubricant of described step (4), the mass ratio of zinc stearate and polyethylene glycol is (0.02~5): 1; Preferably, in the lubricant of described step (4), the mass ratio of zinc stearate and polyethylene glycol is (3~1): 2; More preferably, described step In the lubricant of (4), the mass ratio of zinc stearate and polyethylene glycol is 2:3. 3.如权利要求1或2所述的温压制备铁硅铝软磁磁粉芯的方法,其特征在于,所述步骤(4)中润滑剂与初始软磁合金粉末的质量比为0.4~2%;优选地,所述步骤(4)中润滑剂与初始软磁合金粉末的质量比为0.5~1.5%。3. the method for preparing sendust soft magnetic powder core by warm pressing as claimed in claim 1 or 2, is characterized in that, in the described step (4), the mass ratio of lubricant and initial soft magnetic alloy powder is 0.4~2 %; Preferably, the mass ratio of the lubricant to the initial soft magnetic alloy powder in the step (4) is 0.5-1.5%. 4.如权利要求1所述的温压制备铁硅铝软磁磁粉芯的方法,其特征在于,所述步骤(2)中的粘结剂为硅酸钠、耐高温有机硅树脂的混合物;所述步骤(3)中的绝缘剂为纳米二氧化硅。4. the method for preparing sendust soft magnetic powder core by warm pressing as claimed in claim 1, is characterized in that, the binding agent in the described step (2) is the mixture of sodium silicate, high temperature resistant organic silicon resin; The insulating agent in the step (3) is nano silicon dioxide. 5.如权利要求4所述的温压制备铁硅铝软磁磁粉芯的方法,其特征在于,所述步骤(2)的粘结剂中,硅酸钠和耐高温有机硅树脂的质量比为(4~1):2;优选地,所述步骤(2)的粘结剂中,硅酸钠和耐高温有机硅树脂的质量比为3:2。5. the method for preparing sendust soft magnetic powder core by warm pressing as claimed in claim 4, is characterized in that, in the binding agent of described step (2), the mass ratio of sodium silicate and high temperature-resistant silicone resin It is (4-1): 2; preferably, in the binder in the step (2), the mass ratio of sodium silicate and high temperature resistant silicone resin is 3:2. 6.如权利要求1所述的温压制备铁硅铝软磁磁粉芯的方法,其特征在于,所述步骤(2)中的粘结剂与初始软磁合金粉末的质量比为1~2%;所述步骤(3)中绝缘剂与初始软磁合金粉末的质量比为0~0.4%。6. the method for preparing sendust soft magnetic powder core by warm pressing as claimed in claim 1, is characterized in that, the mass ratio of binder in the described step (2) and initial soft magnetic alloy powder is 1~2 %; the mass ratio of the insulating agent to the initial soft magnetic alloy powder in the step (3) is 0-0.4%. 7.如权利要求6所述的温压制备铁硅铝软磁磁粉芯的方法,其特征在于,所述步骤(2)中的粘结剂与初始软磁合金粉末的质量比为1.5%;所述步骤(3)中绝缘剂与初始软磁合金粉末的质量比为0.1~0.4%。7. the method for preparing sendust soft magnetic powder core by warm pressing as claimed in claim 6, is characterized in that, the mass ratio of binding agent in described step (2) and initial soft magnetic alloy powder is 1.5%; In the step (3), the mass ratio of the insulating agent to the initial soft magnetic alloy powder is 0.1-0.4%. 8.如权利要求1所述的温压制备铁硅铝软磁磁粉芯的方法,其特征在于,所述步骤(1)中采用的钝化剂为磷酸溶液,所述磷酸溶液的质量百分浓度为0.4~3%,所述磷酸溶液与初始软磁合金粉末的质量比为(0.5~1.5):1。8. the method for preparing sendust soft magnetic powder core by warm pressing as claimed in claim 1, is characterized in that, the passivating agent that adopts in described step (1) is phosphoric acid solution, and the mass percent of described phosphoric acid solution The concentration is 0.4-3%, and the mass ratio of the phosphoric acid solution to the initial soft magnetic alloy powder is (0.5-1.5):1. 9.如权利要求1所述的温压制备铁硅铝软磁磁粉芯的方法,其特征在于,所述步骤(4)中温压压制成形的压制压力为500~1200MPa,压制温度为60~150℃;所述步骤(5)中退火处理的退火温度为550~750℃,退火时间为0.5~1.5小时。9. The method for preparing sendust soft magnetic powder cores by warm pressing as claimed in claim 1, characterized in that, in the step (4), the pressing pressure of warm pressing and forming is 500-1200 MPa, and the pressing temperature is 60-150 ° C; the annealing temperature of the annealing treatment in the step (5) is 550-750 ° C, and the annealing time is 0.5-1.5 hours. 10.一种采用如权利要求1~9任一所述方法制备得到的铁硅铝软磁磁粉芯。10. A sendust soft magnetic powder core prepared by the method according to any one of claims 1-9.
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