WO2019153309A1 - 一种新型球形铁基非晶合金粉末及非晶磁粉芯的制备方法 - Google Patents

一种新型球形铁基非晶合金粉末及非晶磁粉芯的制备方法 Download PDF

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WO2019153309A1
WO2019153309A1 PCT/CN2018/076354 CN2018076354W WO2019153309A1 WO 2019153309 A1 WO2019153309 A1 WO 2019153309A1 CN 2018076354 W CN2018076354 W CN 2018076354W WO 2019153309 A1 WO2019153309 A1 WO 2019153309A1
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amorphous alloy
powder
alloy powder
magnetic powder
amorphous
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PCT/CN2018/076354
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French (fr)
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郭雄志
张云帆
肖强
徐方胜
周金
刘欢
何恺
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深圳市铂科新材料股份有限公司
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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
    • H01F1/14—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 metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/153—Amorphous metallic alloys, e.g. glassy metals

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  • the invention relates to the field of magnetic materials, in particular to a novel spherical iron-based amorphous alloy powder and a method for preparing an amorphous magnetic powder core.
  • the iron-based amorphous soft magnetic alloy has the advantages of high saturation magnetic induction, high initial magnetic permeability, small coercive force and low loss, and the iron core prepared by the rapid quenching method is appropriately heat-treated. After the excellent soft magnetic properties, it has been widely used in various fields such as transformers, sensors, switching power supplies and so on. However, with the development of the electronic power industry, electronic devices are developing in the direction of miniaturization, high frequency, and high current, and the soft magnetic core with winding and lamination is greatly depleted at high frequency, which limits its high frequency. Applications. At this point, a magnetic powder core is needed to meet the job requirements.
  • the magnetic powder core is made by powder metallurgy process, which is prepared by mixing soft magnetic alloy powder and insulating medium.
  • the traditional magnetic powder core mainly includes iron powder core, iron silicon powder core, iron silicon aluminum powder core, iron nickel powder core and iron nickel molybdenum powder core.
  • the iron powder core is cheap, but the high frequency characteristics and loss characteristics are not good; the iron silicon powder core is moderately priced, the DC superposition performance is excellent, but the high frequency loss is high; the iron silicon aluminum powder core has a wide application range, low loss and good frequency performance. Excellent cost performance, but DC superposition characteristics are not ideal; iron nickel powder core has the best DC bias characteristics, but the price is higher, the loss is also high; iron nickel molybdenum performance is the most superior, but the price is also the most expensive, high price Limit its scope of application.
  • the iron-based amorphous magnetic powder core has the characteristics of constant magnetic permeability, high electrical resistivity, low loss and good temperature stability at high frequency, and also meets the requirements of the national 12th Five-Year Development Plan for energy conservation and emission reduction, and the cost is low. It is an important development direction of magnetic powder core materials, and has gradually become a hot spot of research and application in recent years. Fu Min et al. (Army Materials Science and Engineering, 2014, 37:90) studied the effects of passivating agents, insulating agents and binders on the properties of strip-decomposed FeSiB amorphous magnetic powder cores in the insulation coating process.
  • the effective magnetic permeability of the magnetic powder core decreases with the increase of the content of the insulating coating agent, and the quality factor Q increases with the addition amount.
  • the mass fraction of the passivating agent is 4% to 8%
  • the performance of the magnetic powder core Excellent magnetic permeability reaches 45.
  • Tang Jian et al. (Functional Materials, 2012, 43:96) studied the effect of heat treatment temperature on the properties of Fe 78 Si 9 B 13 amorphous magnetic powder core. The results show that the amorphous state is lower than the initial crystallization temperature. The loss of the magnetic powder core tends to decrease first and then increase with the increase of annealing temperature, while the magnetic permeability shows the opposite trend.
  • the invention patent No. 201310018768.7 discloses a preparation method of a soft magnetic alloy magnetic powder core, which comprises embrittlement treatment of amorphous strip, pulverization into powder, sieving and proportioning, passivation treatment and insulation coating, press molding, The steps of annealing treatment and spraying, the magnetic powder core has excellent high frequency performance.
  • the invention patent No. 201410394382.0 discloses a method for preparing an amorphous metal soft magnetic powder core.
  • the amorphous metal soft magnetic powder is sieved through different sieves to obtain two powders with different particle size distributions to be mixed to obtain powder.
  • the isostatic pressing treatment is performed, and the stress relief annealing treatment is performed at a temperature of 300-450 ° C to obtain an amorphous metal soft magnetic powder core having high density and uniform distribution.
  • the magnetic powders used in the amorphous magnetic powder cores mentioned in the above articles and patents are all prepared by the strip crushing method, and impurities are easily introduced during the ball mill crushing process, resulting in uneven composition of the powder, and at the same time, obtained. Most of the powders are angular sheets, which are difficult to insulate, resulting in high loss of the magnetic powder core and poor resistance to DC bias.
  • the present invention provides a novel method for preparing a spherical iron-based amorphous alloy powder and an amorphous magnetic powder core.
  • the technical scheme of the present invention is as follows: a novel spherical iron-based amorphous alloy powder, wherein the atomic percentage of each element in the iron-based amorphous alloy powder is 7 to 10% Si, 7 to 11% B, and 3 to 6% P, 0 to 3% Nb, 0 to 2% Cu, and the balance is Fe.
  • the invention also provides a method for preparing an amorphous magnetic powder core by using the novel spherical iron-based amorphous alloy powder described above, comprising the following steps:
  • a stress relief annealing treatment is performed.
  • the alloy melt is kept at a temperature of 150 to 300 ° C for 10 to 30 minutes; more preferably, the alloy melt is kept at a temperature of 200 to 250 ° C for 15 to 25 minutes. .
  • the atomization pressure of the gas atomization is 5 to 15 MPa, and the diameter of the melt nozzle is 0.5 to 3 mm; more preferably, the atomization pressure of the gas atomization is 8 to 12 MPa, and the diameter of the melt nozzle It is 1 to 2 mm.
  • the atomizing gas in the step (1) may be an inert gas such as nitrogen, argon or helium, or may be a gas such as air or oxygen.
  • the amorphous alloy powder of the target particle diameter in the step (2) is a powder passing through a 200 mesh sieve, that is, the powder particle diameter is less than 75 ⁇ m; and the amorphous structure of the powder in the step (2) can be determined by an X-ray diffractometer. .
  • the passivating agent in the step (3) is a phosphating solution
  • the insulating agent is mica powder
  • the binder is an epoxy resin or a polyamide resin.
  • the process of treating the amorphous alloy powder in the step (3) is: adding the amorphous alloy powder to the phosphating solution of 1 to 5 wt%, stirring uniformly to dryness, and then phosphating the amorphous alloy powder. It is uniformly mixed with 1 to 5 wt% of mica. Finally, the mixed powder is added to 1 to 5 wt% of an epoxy resin or a polyamide resin in acetone, and stirred until dry.
  • the pressure of press molding in the step (4) is 10 to 26 t/cm 2 , and the pressure holding time is 5 to 120 s.
  • the temperature of the stress relief annealing treatment in the step (4) is 300 to 450 ° C, and the treatment time is 0.5 to 3 h.
  • the atmosphere for stress relief annealing in the step (4) may be a protective atmosphere such as nitrogen or argon or a reducing atmosphere such as hydrogen.
  • the invention has the following beneficial effects: 1.
  • the amorphous forming ability of the alloy is high, and the iron-based amorphous alloy powder is prepared by the gas atomization method, thereby avoiding the impurities mixed in the conventional strip crushing method, and the composition.
  • the problem of unevenness and sharp edges and corners facilitates the insulation coating of the powder, thereby reducing the core loss of the magnetic powder core and improving its resistance to DC bias.
  • the structure is uniform. High-strength, high-density and constant-permeability iron-based amorphous magnetic powder cores are expected to be used as various inductive components for filtering, steady current and energy storage on various switching power supply modules.
  • Example 1 is a SEM appearance top view of a novel spherical iron-based amorphous alloy powder prepared in Example 1.
  • Example 2 is an XRD pattern of a novel spherical iron-based amorphous alloy powder prepared in Example 1.
  • Example 3 is a graph showing the change in magnetic permeability of the amorphous magnetic powder core prepared in Example 1 with frequency.
  • Example 4 is a graph showing the tendency of the loss of the amorphous magnetic powder core core produced in Example 1 with frequency.
  • Fig. 5 is a graph showing the relationship between the magnetic permeability of the amorphous magnetic powder core prepared in Example 1 and the applied magnetic field.
  • the master alloy was heated and melted to 200 ° C above the melting point and held for 10 minutes.
  • the Fe 76 Si 9 B 10 P 5 alloy powder was prepared by gas atomization.
  • the pressure of the gas atomization was 10 MPa, the nozzle diameter was 1 mm, and the mesh was sieved with 200 mesh.
  • the powder was sieved to obtain the target powder, and the morphology of the target powder was analyzed by a scanning electron microscope (SEM).
  • SEM scanning electron microscope
  • Fig. 1 it can be seen that the powder exhibited a spherical shape with a smooth surface and no obvious pores or holes.
  • the defects were measured by X-ray diffractometry (XRD).
  • XRD X-ray diffractometry
  • the amorphous alloy powder is subjected to an insulating coating treatment, and the amorphous alloy powder is added to a 1 wt% epoxy resin and a 1 wt% polyamide resin acetone solution, and stirred at a constant speed until dry. After the insulation coating, the sieve was re-screened through a 100-mesh sieve, and powder particles of 100 mesh or less were collected for press molding.
  • the powder particles were put into a hydroforming machine, and a ring-shaped magnetic powder core having an outer diameter of 20.3 mm, an inner diameter of 12.7 mm, a height of 6.35 mm ( ⁇ 20.3 ⁇ 12.7 ⁇ 6.35 mm), and a dwell time were prepared using a pressure of 18 t/cm 2 .
  • the surface composition of the magnetic powder core after molding is uniform and there are no obvious defects.
  • an iron-based amorphous magnetic powder core was obtained, and the magnetic permeability, loss and DC bias of the magnetic powder core were measured.
  • the magnetic powder core After testing, the magnetic powder core has a magnetic permeability of 69 at a frequency of 1 MHz, and the frequency stability is excellent, as shown in Fig. 3; the loss of the magnetic powder core is very low, and the loss is 707 mW/cm 3 at 50 kHz and 0.1 T. As shown in Fig. 4; under the magnetic field of 100Oe, the magnetic permeability can still be maintained at 61% when no magnetic field is applied. As shown in Fig. 5, it can be seen that the prepared iron-based amorphous magnetic powder core has excellent comprehensive performance.
  • the master alloy was heated and melted to 150 ° C above the melting point and held for 15 minutes.
  • the Fe 76 Si 9 B 10 P 5 alloy powder was prepared by gas atomization. The pressure of the gas atomization was 9 MPa, the nozzle diameter was 1 mm, and the mesh was sieved with 200 mesh. The powder was sieved to obtain the target powder.
  • the SEM image showed that the powder exhibited a spherical shape with a smooth surface and no obvious defects such as pores and holes; the XRD pattern showed that the prepared powder was completely amorphous.
  • the amorphous alloy powder is subjected to an insulating coating treatment, and the amorphous alloy powder is added to a 2 wt% epoxy resin and a 1 wt% polyamide resin acetone solution, and stirred at a constant speed until dry. After the insulation coating, the sieve was re-screened through a 100-mesh sieve, and powder particles of 100 mesh or less were collected for press molding.
  • the powder particles were put into a hydroforming machine, and a ring-shaped magnetic powder core having an outer diameter of 20.3 mm, an inner diameter of 12.7 mm, a height of 6.35 mm ( ⁇ 20.3 ⁇ 12.7 ⁇ 6.35 mm), and a dwell time were prepared using a pressure of 16 t/cm 2 .
  • the surface composition of the magnetic powder core after molding is uniform, and there is no obvious defect.
  • an iron-based amorphous magnetic powder core was obtained, and the magnetic permeability, loss and DC bias of the magnetic powder core were measured.
  • the magnetic powder core After testing, the magnetic powder core has a magnetic permeability of 63 at a frequency of 1 MHz, and at the same time, the frequency stability is excellent; the loss of the magnetic powder core is very low, and the loss is 900 mW/cm 3 at 50 kHz and 0.1 T; at a magnetic field of 100 Oe The magnetic permeability can still be maintained at 63% when no magnetic field is applied. It can be seen that the prepared iron-based amorphous magnetic powder core has excellent comprehensive performance.
  • the master alloy was heated and melted to 200 ° C above the melting point and kept for 20 minutes.
  • the alloy powder (Fe 0.76 Si 0.09 B 0.1 P 0.05 ) 99 Nb 1 was prepared by gas atomization. The pressure of the gas atomization was 9 MPa, and the diameter of the nozzle was 1.3 mm. After drying the alloy powder in a vacuum drying oven, the powder was sieved with a 200 mesh screen to obtain a target powder. The SEM image showed that the powder exhibited a spherical shape with a smooth surface and no obvious defects such as holes and holes; XRD pattern showed The powder prepared is completely amorphous.
  • Passivation and insulation coating treatment of amorphous alloy powder, passivation treatment Pour amorphous alloy powder into 1wt% phosphating solution, stir at a constant speed until dry; Insulation coating: amorphous after passivation treatment The alloy powder was added to a 1 wt% epoxy resin and a 1 wt% polyamide resin acetone solution, and stirred at a constant speed until dry. After the insulation coating, the sieve was re-screened through a 100-mesh sieve, and powder particles of 100 mesh or less were collected for press molding.
  • the powder particles were put into a hydroforming machine, and a ring-shaped magnetic powder core having an outer diameter of 20.3 mm, an inner diameter of 12.7 mm, a height of 6.35 mm ( ⁇ 20.3 ⁇ 12.7 ⁇ 6.35 mm), and a dwell time were prepared using a pressure of 18 t/cm 2 .
  • the surface composition of the magnetic powder core after molding is uniform and there are no obvious defects.
  • the formed magnetic powder core was annealed at 450 ° C for 1 hour, an iron-based amorphous magnetic powder core was obtained, and the magnetic permeability, loss and DC bias of the magnetic powder core were measured.
  • the magnetic powder core After testing, the magnetic powder core has a magnetic permeability of 65 at a frequency of 1 MHz, and at the same time, the frequency stability is excellent; the loss of the magnetic powder core is very low, and the loss is 670 mW/cm 3 at 50 kHz and 0.1 T; at a magnetic field of 100 Oe The magnetic permeability can still be maintained at 63% when no magnetic field is applied. It can be seen that the prepared iron-based amorphous magnetic powder core has excellent comprehensive performance.
  • the master alloy was heated and melted to 250 ° C above the melting point and held for 15 minutes.
  • the alloy powder (Fe 0.76 Si 0.09 B 0.1 P 0.05 ) 99 Nb 1 was prepared by gas atomization.
  • the pressure of the gas atomization was 11 MPa, and the diameter of the nozzle was 1 mm.
  • the powder was sieved with a 200-mesh sieve to obtain a target powder.
  • the SEM image showed that the powder exhibited a spherical shape with a smooth surface and no obvious defects such as pores and holes; the XRD pattern showed that the prepared powder was completely amorphous.
  • the powder particles were put into a hydroforming machine, and a ring-shaped magnetic powder core having an outer diameter of 20.3 mm, an inner diameter of 12.7 mm, a height of 6.35 mm ( ⁇ 20.3 ⁇ 12.7 ⁇ 6.35 mm), and a dwell time were prepared using a pressure of 17 t/cm 2 .
  • the surface composition of the magnetic powder core after molding is uniform, and there is no obvious defect.
  • an iron-based amorphous magnetic powder core was obtained, and the magnetic permeability, loss and DC bias of the magnetic powder core were respectively measured.
  • the magnetic powder core After testing, the magnetic powder core has a magnetic permeability of 63 at a frequency of 1 MHz, and at the same time, the frequency stability is excellent; the loss of the magnetic powder core is very low, and the loss is 680 mW/cm 3 at 50 kHz and 0.1 T; at a magnetic field of 100 Oe The magnetic permeability can still be maintained at 62% when no magnetic field is applied. It can be seen that the prepared iron-based amorphous magnetic powder core has excellent comprehensive performance.
  • the master alloy was heated and melted to 200 ° C above the melting point and held for 15 minutes.
  • the alloy was prepared by gas atomization (Fe 0.76 Si 0.09 B 0.1 P 0.05 ) 98.5 Nb 1 Cu 0.5 alloy powder.
  • the pressure of the gas atomization was 10 MPa, and the nozzle diameter was 1mm, the powder was sieved with a 200 mesh screen to obtain the target powder.
  • the SEM image showed that the powder exhibited a spherical shape with smooth surface and no obvious defects such as holes and holes.
  • the XRD pattern showed that the prepared powder was completely amorphous. .
  • the powder particles were put into a hydroforming machine, and a ring-shaped magnetic powder core having an outer diameter of 20.3 mm, an inner diameter of 12.7 mm, a height of 6.35 mm ( ⁇ 20.3 ⁇ 12.7 ⁇ 6.35 mm), and a dwell time were prepared using a pressure of 20 t/cm 2 .
  • the surface composition of the magnetic powder core after molding is uniform and there are no obvious defects.
  • an iron-based amorphous magnetic powder core was obtained, and the magnetic permeability, loss and DC bias of the magnetic powder core were measured.
  • the magnetic powder core After testing, the magnetic powder core has a magnetic permeability of 65 at 1MHz frequency, and the frequency stability is excellent; the loss of the magnetic powder core is very low, and the loss is 450mW/cm 3 under the condition of 100kHz and 0.05T; under the magnetic field of 100Oe The magnetic permeability can still be maintained at 69% when no magnetic field is applied. It can be seen that the prepared iron-based amorphous magnetic powder core has excellent comprehensive performance.
  • the master alloy was heated and melted to 200 ° C above the melting point and held for 15 minutes.
  • the powder was prepared by gas atomization (Fe 0.76 Si 0.09 B 0.1 P 0.05 ) 98.25 Nb 1 Cu 0.75 alloy powder.
  • the pressure of the gas atomization was 9 MPa, and the nozzle diameter was 1.2mm, the powder was sieved with a 200 mesh screen to obtain the target powder.
  • the SEM image showed that the powder exhibited a spherical shape with smooth surface and no obvious defects such as holes and holes.
  • the XRD pattern showed that the prepared powder was completely amorphous. of.
  • the powder particles were put into a hydroforming machine, and a ring-shaped magnetic powder core having an outer diameter of 20.3 mm, an inner diameter of 12.7 mm, a height of 6.35 mm ( ⁇ 20.3 ⁇ 12.7 ⁇ 6.35 mm), and a dwell time were prepared using a pressure of 18 t/cm 2 .
  • the surface composition of the magnetic powder core after molding is uniform, and there is no obvious defect.
  • an iron-based amorphous magnetic powder core was obtained, and the magnetic permeability, loss and DC bias of the magnetic powder core were respectively measured.
  • the permeability of the magnetic powder core at 1MHz frequency is 73; the loss of the magnetic powder core is very low, the loss is 420mW/cm 3 under the condition of 100kHz and 0.05T, and the magnetic permeability can be maintained under the external magnetic field of 100Oe. 66% when no magnetic field is applied. It can be seen that the prepared iron-based amorphous magnetic powder core has excellent comprehensive performance.

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Abstract

一种球形铁基非晶合金粉末及非晶磁粉芯的制备方法，包括如下步骤：采用气雾化法制备所述球形铁基非晶合金粉末；对所述球形铁基非晶合金粉末进行筛分，获得目标粒径的非晶合金粉末；分别采用钝化剂、绝缘剂和粘结剂对筛分后的非晶合金粉末依次进行钝化和绝缘包覆处理；采用冷压法将处理好的非晶合金粉末压制成型后，进行去应力退火处理。制备的非晶磁粉芯具有稳定的磁导率、低的铁芯损耗和优异的抗直流偏置能力，综合性能优异，有望用做各种开关电源模块上的滤波、稳流和储能等各种电感元件。

Description

一种新型球形铁基非晶合金粉末及非晶磁粉芯的制备方法 技术领域
本发明涉及磁性材料领域，尤其涉及一种新型球形铁基非晶合金粉末及非晶磁粉芯的制备方法。
背景技术
铁基非晶软磁合金具有饱和磁感应强度高、初始磁导率高、矫顽力小、损耗低等优点，用快淬法制备出的非晶带材绕制成的铁芯经适当的热处理后具有优良的软磁性能，在各类变压器、传感器、开关电源等领域得到了广泛的应用。但随着电子电力工业的发展，电子器件向小型化、高频化和大电流方向发展，而带绕、叠片的软磁铁芯在高频工作时损耗很大，限制了其在高频下的应用。此时，需要采用磁粉芯来满足工作需求。磁粉芯是采用粉末冶金工艺，由软磁合金粉末和绝缘介质混合压制而成的。传统的磁粉芯主要有铁粉芯、铁硅粉芯、铁硅铝粉芯、铁镍粉芯和铁镍钼粉芯等。铁粉芯价格低廉，但高频特性和损耗特性不佳；铁硅粉芯价格适中，直流叠加性能优异，但高频损耗高；铁硅铝粉芯应用面广，损耗低，频率性能好，具有优良的性价比，但直流叠加特性不够理想；铁镍粉芯具有最佳的直流偏磁特性，但是价格较高，损耗也高；铁镍钼性能最优越，但是价格也最昂贵，高昂的价格限制了其应用范围。
铁基非晶磁粉芯在高频下具有恒磁导率、高电阻率、低损耗、温度稳定性好等特点，也符合国家节能减排“十二五”发展规划的要求，且成本低廉，是磁粉芯材料的重要发展方向，近年来逐渐成为研究和应用的热点。付敏等(兵器材料科学与工程，2014，37:90)研究了 绝缘包覆工艺中的钝化剂、绝缘剂和粘结剂对带材破碎FeSiB非晶磁粉芯性能的影响，研究结果表明，磁粉芯的有效磁导率随绝缘包覆剂含量的增大而减小，品质因数Q随添加量的增加而增大，钝化剂的质量分数在4％～8％时，磁粉芯性能优异，磁导率达到45。唐坚等(功能材料，2012，43:96)研究了热处理温度对Fe 78Si 9B 13非晶磁粉芯性能的影响规律，结果表明，在低于起始晶化温度的条件下，非晶磁粉芯的损耗随退火温度的提高呈现出先降低后增大的趋势，而磁导率呈现出相反的趋势。在热处理温度过高时，非晶磁粉发生晶化，磁各向异性常数增加，导致磁导率急剧下降，而磁导率在3MHz范围内变化不大，频率稳定性良好。申请号为201310018768.7的发明专利公布了一种软磁合金磁粉芯的制备方法，包括非晶带材脆化处理、粉碎成粉末、筛分和配比、钝化处理和绝缘包覆、压制成型、退火处理和喷涂等步骤，磁粉芯的高频性能优异。申请号为201410394382.0的发明专利公布了一种非晶金属软磁粉芯的制备方法，将非晶金属软磁粉末通过不同筛目的筛子筛分后得到粒径分布不同的两种粉末进行混合达到粉料，在压制成型得到非晶金属软磁粉芯生坯后进行等静压处理，并在温度为300-450℃条件下进行去应力退火处理，得到密度高且分布均匀的非晶金属软磁粉芯。
然而，上述文章及专利中涉及的非晶磁粉芯所采用的磁粉均是通过带材破碎法来制备的，在球磨破碎的过程中容易引入杂质，导致粉末的组分不均匀，同时，所获得的粉末多为带棱角的片状，难以绝缘，导致磁粉芯的损耗较高，抗直流偏置能力较差。
技术问题
为解决现有技术中存在的问题，本发明提出一种新型球形铁基非晶合金粉末及非晶磁粉芯的制备方法。
技术解决方案
本发明技术方案如下：一种新型球形铁基非晶合金粉末，所述铁基非晶合金粉末中各元素的原子百分比为7～10％Si，7～11％B，3～6％P，0～3％Nb，0～2％Cu，余量为Fe。
本发明还提供一种利用上述的新型球形铁基非晶合金粉末制备非晶磁粉芯的方法，包括如下步骤：
(1)采用气雾化法制备所述新型球形铁基非晶合金粉末；
(2)对步骤(1)制得的所述新型球形铁基非晶合金粉末进行筛分，获得目标粒径的非晶合金粉末；
(3)分别采用钝化剂、绝缘剂和粘结剂对经步骤(2)筛分后的非晶合金粉末依次进行钝化和绝缘包覆处理；
(4)采用冷压法将经步骤(3)处理好的非晶合金粉末压制成型后，进行去应力退火处理。
优选的，步骤(1)中，在雾化喷粉前，合金熔体要在熔点以上150～300℃保温10～30min；更优选的，合金熔体在熔点以上200～250℃保温15～25min。
优选的，步骤(1)中，气雾化的雾化压力为5～15MPa，熔体喷嘴直径为0.5～3mm；更优选的，气雾化的雾化压力为8～12MPa，熔体喷嘴直径为1～2mm。
优选的，步骤(1)中的雾化气体可以是氮气、氩气或氦气等惰 性气体，也可以是空气或氧气等气体。
优选的，步骤(2)中目标粒径的非晶合金粉末为通过200目筛网的粉末，即粉末粒径小于75μm；步骤(2)中粉末的非晶态结构可以通过X射线衍射仪测定。
优选的，步骤(3)中所述钝化剂为磷化液，所述绝缘剂为云母粉，所述粘结剂为环氧树脂或聚酰胺树脂。
优选的，步骤(3)中对非晶合金粉末的处理过程为：将非晶合金粉末加入到1～5wt％的磷化液中，搅拌均匀至干燥，随后将磷化后的非晶合金粉末与1～5wt％的云母均匀混合，最后，将混合粉末加入到1～5wt％的环氧树脂或聚酰胺树脂的丙酮溶液中，搅拌均匀至干燥。
优选的，步骤(4)中压制成型的压力为10～26t/cm 2，保压时间为5～120s。
优选的，步骤(4)中去应力退火处理的温度为300～450℃，处理时间为0.5～3h。
优选的，步骤(4)中去应力退火的气氛可以是氮气、氩气等保护性气氛或氢气等还原性气氛。
有益效果
与现有技术相比，本发明具有如下有益效果：1、合金的非晶形成能力高，采用气雾化法制备铁基非晶合金粉末，可避免传统带材破碎法存在的混入杂质，成分不均匀和存在尖锐棱角的问题，利于粉末的绝缘包覆，从而降低磁粉芯的铁芯损耗，提高其抗直流偏置能力；2、通过压制成型和去应力退火处理后，得到了组织均匀、高强度、 高致密度和磁导率恒定的铁基非晶磁粉芯，有望用做各种开关电源模块上的滤波、稳流和储能等各种电感元件。
附图说明
图1是实施例1中制备的新型球形铁基非晶合金粉末的SEM外观形貌图。
图2是实施例1中制备的新型球形铁基非晶合金粉末的XRD图谱。
图3是实施例1中制备的非晶磁粉芯磁导率随频率的变化趋势。
图4是实施例1中制备的非晶磁粉芯铁芯损耗随频率的变化趋势。
图5是实施例1中制备的非晶磁粉芯的磁导率随外加磁场的变化趋势。
本发明的最佳实施方式
为进一步阐释本发明为实现预定目的而采取的技术手段及功效，以下结合具体实施例，对本发明的具体实施方式、结构、特征及功效，详细说明如下；
实施例1：
将母合金加热熔融至熔点以上200℃并保温10分钟，采用气雾化法制备Fe 76Si 9B 10P 5合金粉末，气雾化的压力为10MPa，喷嘴直径为1mm，用200目筛网对粉末进行筛分，获得目标粉末，用扫描电子显微镜(SEM)对目标粉末的形貌进行分析，如图1所示，可以看出，粉末呈现出球形，表面光滑，无明显的孔、洞等缺陷；用X射线衍射仪(XRD)检测其结构，结果如图2所示，可以看出，XRD图谱上没有任何结晶相对应的衍射峰，仅有一个宽的漫散射峰，说明所制备的 粉末是完全非晶态的。
对非晶合金粉末进行绝缘包覆处理，将非晶合金粉末加入到1wt％环氧树脂和1wt％的聚酰胺树脂丙酮溶液中，匀速搅拌至干燥。在绝缘包覆后，经过100目的筛网重新筛分，收集100目以下的粉末颗粒进行压制成型。
将粉末颗粒投入到液压成型机中，使用18t/cm 2的压强压制成外径20.3mm，内径12.7mm，高度为6.35mm(Φ20.3×12.7×6.35mm)的环形磁粉芯，保压时间为30s，成型后磁粉芯的表面组成均匀，无明显缺陷。对所述成型的磁粉芯在400℃下进行1个小时的去应力退火处理后，获得铁基非晶磁粉芯，分别测定磁粉芯的磁导率、损耗和直流偏置等性能。
经测试，磁粉芯在1MHz频率下的磁导率为69，同时，频率稳定性优异，如图3所示；磁粉芯的损耗很低，在50kHz，0.1T条件下，损耗为707mW/cm 3，如图4所示；在100Oe外加磁场下，磁导率仍能保持在未加磁场时的61％，如图5所示，可见，所制备的新型铁基非晶磁粉芯综合性能优异。
实施例2：
将母合金加热熔融至熔点以上150℃并保温15分钟，采用气雾化法制备Fe 76Si 9B 10P 5合金粉末，气雾化的压力为9MPa，喷嘴直径为1mm，用200目筛网对粉末进行筛分，获得目标粉末，SEM图谱显示粉末呈现出球形，表面光滑，无明显的孔、洞等缺陷；XRD图谱显示所制备的粉末是完全非晶态的。
对非晶合金粉末进行绝缘包覆处理，将非晶合金粉末加入到2wt％环氧树脂和1wt％的聚酰胺树脂丙酮溶液中，匀速搅拌至干燥。在绝缘包覆后，经过100目的筛网重新筛分，收集100目以下的粉末颗粒进行压制成型。
将粉末颗粒投入到液压成型机中，使用16t/cm 2的压强压制成外径20.3mm，内径12.7mm，高度为6.35mm(Φ20.3×12.7×6.35mm)的环形磁粉芯，保压时间为20s，成型后磁粉芯的表面组成均匀，无明显缺陷。对所述成型的磁粉芯在400℃下进行1个小时的去应力退火处理后，获得铁基非晶磁粉芯，分别测定磁粉芯的磁导率、损耗和直流偏置等性能。
经测试，磁粉芯在1MHz频率下的磁导率为63，同时，频率稳定性优异；磁粉芯的损耗很低，在50kHz，0.1T条件下，损耗为900mW/cm 3；在100Oe外加磁场下，磁导率仍能保持在未加磁场时的63％。可见，所制备的新型铁基非晶磁粉芯综合性能优异。
实施例3：
将母合金加热熔融至熔点以上200℃并保温20分钟，采用气雾化法制备(Fe 0.76Si 0.09B 0.1P 0.05) 99Nb 1合金粉末，气雾化的压力为9MPa，喷嘴直径为1.3mm，将合金粉末在真空干燥箱中干燥后，用200目筛网对粉末进行筛分，获得目标粉末，SEM图谱显示粉末呈现出球形，表面光滑，无明显的孔、洞等缺陷；XRD图谱显示所制备的粉末是完全非晶态的。
对非晶合金粉末进行钝化和绝缘包覆处理，钝化处理：将非晶合 金粉末倒入1wt％的磷化液中，匀速搅拌直至干燥；绝缘包覆：将钝化处理后的非晶合金粉末加入到1wt％环氧树脂和1wt％的聚酰胺树脂丙酮溶液中，匀速搅拌至干燥。在绝缘包覆后，经过100目的筛网重新筛分，收集100目以下的粉末颗粒进行压制成型。
将粉末颗粒投入到液压成型机中，使用18t/cm 2的压强压制成外径20.3mm，内径12.7mm，高度为6.35mm(Φ20.3×12.7×6.35mm)的环形磁粉芯，保压时间为15s，成型后磁粉芯的表面组成均匀，无明显缺陷。对所述成型的磁粉芯在450℃下进行1个小时的退火处理后，获得铁基非晶磁粉芯，分别测定磁粉芯的磁导率、损耗和直流偏置等性能。
经测试，磁粉芯在1MHz频率下的磁导率为65，同时，频率稳定性优异；磁粉芯的损耗很低，在50kHz，0.1T条件下，损耗为670mW/cm 3；在100Oe外加磁场下，磁导率仍能保持在未加磁场时的63％。可见，所制备的新型铁基非晶磁粉芯综合性能优异。
实施例4：
将母合金加热熔融至熔点以上250℃并保温15分钟，采用气雾化法制备(Fe 0.76Si 0.09B 0.1P 0.05) 99Nb 1合金粉末，气雾化的压力为11MPa，喷嘴直径为1mm，用200目筛网对粉末进行筛分，获得目标粉末，SEM图谱显示粉末呈现出球形，表面光滑，无明显的孔、洞等缺陷；XRD图谱显示所制备的粉末是完全非晶态的。
对非晶合金粉末进行钝化和绝缘包覆处理，钝化处理：将非晶合金粉末倒入1wt％的磷化液中，匀速搅拌直至干燥；绝缘包覆：将磷 化后的非晶合金粉末加入到1wt％的云母均匀混合，再将混合粉末加入到2wt％环氧树脂和1wt％的聚酰胺树脂丙酮溶液中，匀速搅拌至干燥。在绝缘包覆后，经过100目的筛网重新筛分，收集100目以下的粉末颗粒进行压制成型。
将粉末颗粒投入到液压成型机中，使用17t/cm 2的压强压制成外径20.3mm，内径12.7mm，高度为6.35mm(Φ20.3×12.7×6.35mm)的环形磁粉芯，保压时间为10s，成型后磁粉芯的表面组成均匀，无明显缺陷。对所述成型的磁粉芯在420℃下进行1个小时的去应力退火处理后，获得铁基非晶磁粉芯，分别测定磁粉芯的磁导率、损耗和直流偏置等性能。
经测试，磁粉芯在1MHz频率下的磁导率为63，同时，频率稳定性优异；磁粉芯的损耗很低，在50kHz，0.1T条件下，损耗为680mW/cm 3；在100Oe外加磁场下，磁导率仍能保持在未加磁场时的62％。可见，所制备的新型铁基非晶磁粉芯综合性能优异。
实施例5：
将母合金加热熔融至熔点以上200℃并保温15分钟，采用气雾化法制备(Fe 0.76Si 0.09B 0.1P 0.05) 98.5Nb 1Cu 0.5合金粉末，气雾化的压力为10MPa，喷嘴直径为1mm，用200目筛网对粉末进行筛分，获得目标粉末，SEM图谱显示粉末呈现出球形，表面光滑，无明显的孔、洞等缺陷；XRD图谱显示所制备的粉末是完全非晶态的。
对非晶合金粉末进行钝化和绝缘包覆处理，钝化处理：将非晶合金粉末倒入1wt％的磷化液中，匀速搅拌直至干燥；绝缘包覆：将磷 化后的非晶合金粉末加入到3wt％的云母均匀混合，再将混合粉末加入到2wt％环氧树脂丙酮溶液中，匀速搅拌至干燥。在绝缘包覆后，经过100目的筛网重新筛分，收集100目以下的粉末颗粒进行压制成型。
将粉末颗粒投入到液压成型机中，使用20t/cm 2的压强压制成外径20.3mm，内径12.7mm，高度为6.35mm(Φ20.3×12.7×6.35mm)的环形磁粉芯，保压时间为30s，成型后磁粉芯的表面组成均匀，无明显缺陷。对所述成型的磁粉芯在400℃下进行1个小时的去应力退火处理后，获得铁基非晶磁粉芯，分别测定磁粉芯的磁导率、损耗和直流偏置等性能。
经测试，磁粉芯在1MHz频率下的磁导率为65，同时，频率稳定性优异；磁粉芯的损耗很低，在100kHz，0.05T条件下，损耗为450mW/cm 3；在100Oe外加磁场下，磁导率仍能保持在未加磁场时的69％。可见，所制备的新型铁基非晶磁粉芯综合性能优异。
实施例6：
将母合金加热熔融至熔点以上200℃并保温15分钟，采用气雾化法制备(Fe 0.76Si 0.09B 0.1P 0.05) 98.25Nb 1Cu 0.75合金粉末，气雾化的压力为9MPa，喷嘴直径为1.2mm，用200目筛网对粉末进行筛分，获得目标粉末，SEM图谱显示粉末呈现出球形，表面光滑，无明显的孔、洞等缺陷；XRD图谱显示所制备的粉末是完全非晶态的。
对非晶合金粉末进行钝化和绝缘包覆处理，钝化处理：将非晶合金粉末倒入1wt％的磷化液中，匀速搅拌直至干燥；绝缘包覆：将磷 化后的非晶合金粉末加入到5wt％的云母均匀混合，再将混合粉末加入到1wt％环氧树脂和1wt％的聚酰胺树脂丙酮溶液中，匀速搅拌至干燥。在绝缘包覆后，经过100目的筛网重新筛分，收集100目以下的粉末颗粒进行压制成型。将粉末颗粒投入到液压成型机中，使用18t/cm 2的压强压制成外径20.3mm，内径12.7mm，高度为6.35mm(Φ20.3×12.7×6.35mm)的环形磁粉芯，保压时间为10s，成型后磁粉芯的表面组成均匀，无明显缺陷。对所述成型的磁粉芯在420℃下进行1个小时的去应力退火处理后，获得铁基非晶磁粉芯，分别测定磁粉芯的磁导率、损耗和直流偏置等性能。
经测试，磁粉芯在1MHz频率下的磁导率为73；磁粉芯的损耗很低，在100kHz，0.05T条件下，损耗为420mW/cm 3，在100Oe外加磁场下，磁导率仍能保持在未加磁场时的66％。可见，所制备的新型铁基非晶磁粉芯综合性能优异。
对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限为性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。
此外，应当理解，虽然本说明书按照实施方式加以描述，但并非每个实施方式仅包含一个独立的技术方案，说明书的这种叙述方式仅仅是为清楚起见，本领域技术人员应当将说明书作为一个整体，各实 施例中的技术方案也可以经适当组合，形成本领域技术人员可以理解的其他实施方式。

Claims (11)

  1. 一种新型球形铁基非晶合金粉末，其特征在于，所述铁基非晶合金粉末中各元素的原子百分比为7～10％Si，7～11％B，3～6％P，0～3％Nb，0～2％Cu，余量为Fe。
  2. 根据权利要求1所述的新型球形铁基非晶合金粉末制备非晶磁粉芯的方法，其特征在于，包括如下步骤：
    (1)采用气雾化法制备所述新型球形铁基非晶合金粉末；
    (2)对步骤(1)制得的所述新型球形铁基非晶合金粉末进行筛分，获得目标粒径的非晶合金粉末；
    (3)分别采用钝化剂、绝缘剂和粘结剂对经步骤(2)筛分后的非晶合金粉末依次进行钝化和绝缘包覆处理；
    (4)采用冷压法将经步骤(3)处理好的非晶合金粉末压制成型后，进行去应力退火处理。
  3. 根据权利要求2所述的制备非晶磁粉芯的方法，其特征在于，步骤(1)中，在雾化喷粉前，合金熔体要在熔点以上150～300℃保温10～30min。
  4. 根据权利要求2所述的制备非晶磁粉芯的方法，其特征在于，步骤(1)中，气雾化的雾化压力为5～15MPa，熔体喷嘴直径为0.5～3mm。
  5. 根据权利要求2所述的制备非晶磁粉芯的方法，其特征在于，步骤(1)中的雾化气体是氮气、氩气、氦气、空气或氧气。
  6. 根据权利要求2所述的制备非晶磁粉芯的方法，其特征在于，步骤(2)中目标粒径的非晶合金粉末为通过200目筛网的粉末。
  7. 根据权利要求2所述的制备非晶磁粉芯的方法，其特征在于，步骤(3)中所述钝化剂为磷化液，所述绝缘剂为云母粉，所述粘结剂为环氧树脂或聚酰胺树脂。
  8. 根据权利要求2所述的制备非晶磁粉芯的方法，其特征在于，步骤(3)中对非晶合金粉末的处理过程为：将非晶合金粉末加入到1～5wt％的磷化液中，搅拌均匀至干燥，随后将磷化后的非晶合金粉末与1～5wt％的云母均匀混合，最后，将混合粉末加入到1～5wt％的环氧树脂或聚酰胺树脂的丙酮溶液中，搅拌均匀至干燥。
  9. 根据权利要求2所述的制备非晶磁粉芯的方法，其特征在于，步骤(4)中压制成型的压力为10～26t/cm 2，保压时间为5～120s。
  10. 根据权利要求2所述的制备非晶磁粉芯的方法，其特征在于，步骤(4)中去应力退火处理的温度为300～450℃，处理时间为0.5～3h。
  11. 根据权利要求2所述的制备非晶磁粉芯的方法，其特征在于，步骤(4)中去应力退火的气氛是氮气、氩气或氢气。
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