WO2017193384A1 - 复合软磁材料及其制备方法 - Google Patents

复合软磁材料及其制备方法 Download PDF

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WO2017193384A1
WO2017193384A1 PCT/CN2016/082075 CN2016082075W WO2017193384A1 WO 2017193384 A1 WO2017193384 A1 WO 2017193384A1 CN 2016082075 W CN2016082075 W CN 2016082075W WO 2017193384 A1 WO2017193384 A1 WO 2017193384A1
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soft magnetic
magnetic material
composite soft
fesicr
zno
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French (fr)
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谈敏
聂敏
李有云
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Shenzhen Sunlord Electronics Co Ltd
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Shenzhen Sunlord Electronics Co Ltd
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Priority to PCT/CN2016/082075 priority Critical patent/WO2017193384A1/zh
Priority to CN201680000414.1A priority patent/CN105993053B/zh
Publication of WO2017193384A1 publication Critical patent/WO2017193384A1/zh
Priority to US15/865,200 priority patent/US10679780B2/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/103—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • 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
    • H01F1/20—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 in the form of particles, e.g. powder
    • H01F1/22—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 in the form of particles, e.g. powder pressed, sintered, or bound together
    • 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
    • H01F1/34—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 non-metallic substances, e.g. ferrites
    • H01F1/36—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 non-metallic substances, e.g. ferrites in the form of particles
    • 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
    • H01F41/02—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 for manufacturing cores, coils, or magnets
    • 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
    • H01F41/02—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 for manufacturing cores, coils, or magnets
    • H01F41/0206—Manufacturing of magnetic cores by mechanical means
    • H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/02—Nitrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2202/00—Treatment under specific physical conditions
    • B22F2202/01—Use of vibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2202/00—Physical properties
    • C22C2202/02—Magnetic

Definitions

  • the invention relates to the field of soft magnetic materials, in particular to a composite soft magnetic material and a preparation method thereof.
  • the biggest advantage of soft magnetic alloy is that it has high saturation magnetic flux density (Bs), good temperature stability, low stability coefficient and good DC superposition characteristics.
  • the biggest advantage of soft ferrite is that it has high magnetic permeability. And resistivity (10 2 ⁇ 10 6 ⁇ ⁇ cm).
  • the power inductor is generally used at a frequency of 100 kHz or higher.
  • the soft magnetic alloy tends to have lower resistivity, lower insulation and withstand voltage performance, and high frequency loss, which causes the core to generate more heat, resulting in deterioration of the performance of the device.
  • the magnetic permeability of the device changes greatly with temperature, which results in unstable performance of the device under low temperature or high temperature environment.
  • the magnetic permeability of the soft magnetic alloy powder core is generally low.
  • the device In order to obtain a higher inductance, the device often needs to increase the number of turns of the winding, thereby causing an increase in copper loss and deterioration of the performance of the device, thereby improving the starting of the material.
  • Magnetic permeability is necessary.
  • it is necessary to develop composite soft magnetic materials with high magnetic permeability, high Bs, and excellent temperature stability.
  • the publication number is CN201410214573.4, the publication date is 2015.03.04, and the Chinese patent entitled "A composite soft magnetic material and a preparation method thereof" discloses a composite soft magnetic material and a preparation method thereof, and the composite soft
  • the composition of the magnetic material is included in terms of mass percentage: FeSiCr 82.56% to 98.45%, Fe2O 30.3% to 8.9%, NiO 0.1% to 1.93%, ZnO 0.1% to 2.13%, CuO 0.1% to 0.53. %.
  • the preparation method of the composite soft magnetic material includes mixing, calcination, pulverization, pressing, and sintering.
  • the invention adjusts the saturation magnetic induction intensity of the composite soft magnetic material by adjusting the content of FeSiCr, adjusts the content of the NiCuZn ferrite formed by adjusting the content of Fe2O3, NiO, ZnO and CuO, thereby improving the insulation and resistance of the composite soft magnetic material. Pressure performance.
  • the publication number is CN201410214841.2, the publication date is 2015.03.04, and the Chinese patent entitled "A composite soft magnetic material and its preparation method” discloses a composite soft magnetic material and a preparation method thereof, and the composite soft
  • the magnetic material includes the following components by weight: 75.13 to 86.12 wt% of FeSiCr alloy powder, 9 to 14.5 wt% of Fe2O3, 1.95 to 2.99 wt% of NiO, 2.15 to 3.75 wt% of ZnO, 0.55 to 1.43 wt%. CuO, 0.03 to 0.85 wt% of Bi2O3, 0.15 to 0.45 wt% of V2O5, and 0.05 to 0.9 wt% of SiO2.
  • the composite soft magnetic material is obtained by mixing, calcining, pulverizing, granulating, pressing and sintering according to the group distribution ratio as described above.
  • the composite soft magnetic material of the invention and the preparation method thereof are prepared by using a component with a specific proportion, thereby obtaining high insulation and high withstand voltage by adjusting the content of each material or adding some components, and the production process.
  • Composite soft magnetic material with high Bs performance are prepared by using a component with a specific proportion, thereby obtaining high insulation and high withstand voltage by adjusting the content of each material or adding some components, and the production process.
  • the publication number is CN201410214819.8, the publication date is 2015.03.11
  • the Chinese patent entitled "Composite soft magnetic material and its preparation method” discloses a composite soft magnetic material and a preparation method thereof, and the composite soft magnetic
  • the material includes the following components: 48.25 to 76.91 wt% FeSiCr, 15 to 30.5 wt% Fe2O3, 3 to 9 wt% NiO, 3.8 to 7.3 wt% ZnO, 1.0 to 2.5 wt% CuO, 0.01 to 0.65 wt% Bi2O3, 0.03 to 0.55.
  • the composite soft magnetic material has a high initial permeability and a high Bs.
  • the publication number is CN201110152217.0, the publication date is 2012.02.22, and the Chinese patent entitled "A composite soft magnetic material and its preparation method” discloses a composite soft magnetic body with high density and high magnetic sensation. Materials and methods for their preparation.
  • the composite soft magnetic material is composed of atomized iron-based powder, lubricant and metal adhesion promoter, wherein the mass of the lubricant is 0.01-2% of the mass of the atomized iron-based powder, and the mass of the metal adhesion promoter is atomized iron base.
  • the powder mass is 0.01-2%; the metal adhesion promoter and the lubricant are uniformly coated on the surface of the atomized iron-based powder particles.
  • the lubricant is nano-active calcium carbonate and/or nano-aluminum oxide, and the metal adhesion promoter is titanate.
  • the invention has simple preparation process, low material cost, high density and large magnetic induction intensity.
  • the present invention provides a composite soft magnetic material and a preparation method thereof to obtain a composite soft magnetic material having high initial magnetic permeability and high Bs and stable temperature characteristics.
  • a composite soft magnetic material comprising the following weight percentage components:
  • FeSiCr is a powder having an average particle diameter of 5 to 100 ⁇ m.
  • the particle diameters of TiO 2 , SiO 2 , Mn 3 O 4 , ZnO, BaO, B 2 O 3 , CaO and CuO are both 50 to 100 nm.
  • FeSiCr, TiO 2 , SiO 2 , Mn 3 O 4 , ZnO, BaO, B 2 O 3 , CaO and CuO account for 90.1 wt%, 0.17 wt%, 0.3 wt%, 0.45 of the composite soft magnetic material, respectively.
  • a method for preparing the composite soft magnetic material includes the following steps:
  • Mixing step dry mixing FeSiCr, TiO 2 , SiO 2 , Mn 3 O 4 and ZnO to obtain a mixture;
  • Pre-compression step mixing the mixture with a powder molding machine
  • Pre-burning step pre-burning the mixture under nitrogen protection to obtain a pre-burned material
  • a pulverization step using a solvent, mixing BaO, B 2 O 3 , CaO, CuO with the pre-sintered material, followed by wet pulverization to obtain a pulverized slurry;
  • a granulation step adding a granulation auxiliary agent to the pulverized slurry, dispersing it under ultrasonic waves, and performing granulation to obtain a granule;
  • Pressing step pressing the pellets by a powder molding machine to obtain a blank
  • a sintering step sintering the blank to obtain the composite soft magnetic material
  • the solvent is anhydrous ethanol.
  • the granulation aid is polyacrylamide.
  • the method satisfies any one or more of the following process conditions:
  • the mixing time is 30 to 70 minutes
  • the pre-compression pressure is 5 tons / cm 2 ;
  • the calcination temperature is controlled at 750 ⁇ 20 ° C, the calcination time is 100 to 200 minutes, and the oxygen content is controlled below 1%;
  • the pulverization time is 120 to 240 minutes, and the particle size of the slurry after pulverization is controlled to be 1.5 to 35 ⁇ m;
  • the polyacrylamide is equal to 2% to 6% by weight of the pulverized slurry
  • the pressing density of the blank is controlled at (5.80 ⁇ 0.10) g / cm 3 ;
  • the sintering temperature is controlled at 920 ° C to 960 ° C, and the temperature is maintained for 200 to 300 minutes, the sintering atmosphere is nitrogen gas, and the oxygen content is controlled to be 1% or less.
  • FeSiCr is a powder having an average particle diameter of 5 to 100 ⁇ m, and the particle diameters of TiO 2 , SiO 2 , Mn 3 O 4 , ZnO, BaO, B 2 O 3 , CaO, and CuO are both 50 to 100 nm.
  • the invention adopts a reasonable main formula, adjusts the saturation magnetic induction intensity of the material by setting the content of FeSiCr powder, improves the insulation and pressure resistance of the material by increasing the content of nano SiO 2 , and increases the material by adding nano Mn 3 O 4 and nano ZnO.
  • the magnetic permeability; the temperature coefficient of the material is adjusted by adding nano TiO 2 ; the content of the low melting point phase is adjusted by setting the contents of nano BaO, B 2 O 3 , CaO, CuO, thereby improving the magnetic permeability of the material and Further increase the insulation and pressure resistance of the material; further adjust the material crystal distribution through the preparation production process, thereby obtaining higher magnetic permeability and Bs, and ensuring certain insulation and pressure resistance.
  • the material has the characteristics of high magnetic permeability and high Bs, and is suitable for the requirements of soft magnetic materials for miniaturization and large current of power inductors.
  • Figure 1 is a graph showing the temperature of ⁇ i of the examples and comparative examples of the present invention.
  • a composite soft magnetic material comprising the following components:
  • FeSiCr is a powder having an average particle diameter of 5 to 100 ⁇ m.
  • the particle sizes of TiO 2 , SiO 2 , Mn 3 O 4 , ZnO, BaO, B 2 O 3 , CaO, and CuO are all 50 to 100 nm.
  • FeSiCr, TiO 2 , SiO 2 , Mn 3 O 4 , ZnO, BaO, B 2 O 3 , CaO, and CuO account for 90.1 wt% and 0.17 wt%, respectively, of the composite soft magnetic material.
  • a method for preparing a composite soft magnetic material comprising the following steps:
  • Pre-compression step mixing the mixture with a powder molding machine
  • Pre-burning step pre-burning the mixture under nitrogen protection to obtain a pre-burned material
  • a pulverization step using a solvent, BaO, B 2 O 3 , CaO, and CuO are mixed with the pre-sintered material according to 7.41 wt%, 0.92 wt%, 0.26 wt%, and 0.09 wt%, followed by wet pulverization to obtain a pulverized pulp.
  • the solvent is preferably anhydrous ethanol;
  • a granulation step adding a granulation aid, preferably polyacrylamide, to the pulverized slurry, and dispersing it under ultrasonic waves, and then granulating to obtain a granule;
  • a granulation aid preferably polyacrylamide
  • Pressing step pressing the pellets by a powder molding machine to obtain a blank
  • Sintering step sintering of the blank in a nitrogen blanket after sintering is completed and then cooled to room temperature with the furnace.
  • the pre-burning step dry mixing is used to facilitate the pre-burning step, otherwise the wet mixing is used to extend the pre-burning step; the pre-pressing step is further used to reduce the calcining step; and in the pulverizing step, the wet method is employed.
  • Mixing facilitates the subsequent granulation step, and the use of ultrasonic dispersion prior to granulation facilitates a more uniform coating of the glue on the surface of the powder granules for better granulation.
  • the mixing time is 30 to 70 minutes.
  • the calcination temperature is controlled at 750 ⁇ 20 ° C, the calcination time is 100 to 200 minutes, and the oxygen content is controlled to be 1% or less.
  • the pulverization time is 120 to 240 minutes, and the particle size of the slurry after pulverization is controlled to be 1.5 to 35 ⁇ m.
  • the polyacrylamide in the granulation step, is from 2% to 6%, preferably 4.5% by weight of the comminuted slurry.
  • the compact density of the green body is controlled at (5.80 ⁇ 0.10) g/cm 3 ;
  • the sintering temperature is controlled at 920 ° C to 960 ° C for 200 to 300 minutes, the sintering atmosphere is nitrogen, and the amount of oxygen is controlled to be 1% or less.
  • the invention adopts a reasonable main formula, adjusts the saturation magnetic induction intensity of the material by adjusting the content of FeSiCr powder, improves the insulation and pressure resistance of the material by increasing the content of nano SiO 2 , and increases the material by adding nano Mn 3 O 4 and nano ZnO. Permeability; adjust the temperature coefficient of the material by adding nano-TiO 2 ; adjust the content of low-melting phase formed by adjusting the content of nano-BaO, B 2 O 3 , CaO, CuO, thereby increasing the magnetic permeability of the material and further increasing The insulation and pressure resistance of the material; further adjust the material crystal distribution through the preparation production process, thereby obtaining higher magnetic permeability and Bs, and ensuring certain insulation and pressure resistance.
  • the material has the characteristics of high magnetic permeability and high Bs, and is suitable for the requirements of soft magnetic materials for miniaturization of power inductors and high current.
  • the material performance indicators are as follows:
  • the composite soft magnetic material is prepared as follows:
  • Pre-pressing pre-compressing the mixed powder into pieces by a powder molding machine at a pressure of 5 tons/cm 2
  • the block-shaped material is pre-fired in a nitrogen-protected push-plate kiln, the pre-firing temperature is controlled at 550 ⁇ 20° C., the calcination time is 100-200 minutes, and the oxygen content is controlled below 1%;
  • Sintering sintering in a nitrogen protective resistance furnace, the sintering temperature is controlled at 920 ° C ⁇ 960 ° C, and the temperature is kept for 200 to 300 minutes, the sintering atmosphere is nitrogen, the oxygen content is controlled below 1%, and after cooling, the furnace is cooled to Room temperature.
  • the composite magnetic ring sample (magnet ring size T8 ⁇ 5 ⁇ 2) was obtained by the above procedure.
  • the sintered composite magnetic rings were tested and evaluated separately.
  • Table 2 lists the performance and evaluation of the examples and comparative examples.
  • the present invention effectively improves the initial permeability of the material and can be compared with the comparative examples. Maintain the corresponding insulation and pressure resistance, high saturation magnetic induction, close to zero temperature coefficient.
  • the initial magnetic permeability of the present invention can reach 115 (1 ⁇ 20%).
  • the Bs of Example 1 was significantly superior to Comparative Example 1, and the specific temperature coefficient ⁇ i ⁇ of Example 1 was significantly superior to Comparative Example 1.
  • the temperature stability characteristics of the examples were significantly more stable than the comparative examples for the ⁇ i temperature profiles of the comparative examples and comparative examples (Fig. 1).
  • the characteristics are basically the same as the corresponding ferrite materials.
  • the material of the present invention should be able to meet the requirements of miniaturization and high current of automotive electronic power inductors and soft magnetic materials for wide temperature applications.

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Abstract

本发明公开了一种复合软磁材料及其制备方法，该复合软磁材料包括如下组份：67.9～95.54wt％FeSiCr、0.1～0.3wt％TiO2、0.15～0.75wt％SiO2、0.1～0.5wt％Mn3O4、0.1～0.5wt％ZnO、3.4～25.9wt％BaO、0.4～3wt％B2O3、0.2～0.85wt％CaO、0.01～0.3wt％CuO。该复合软磁材料具有高起始磁导率和高Bs、优秀的温度稳定性、低温度系数的复合软磁材料。

Description

复合软磁材料及其制备方法 技术领域
本发明涉及软磁材料领域，具体涉及复合软磁材料及其制备方法。
背景技术
软磁合金的最大优点是具有较高的饱和磁通密度(Bs)，温度稳定性好，稳定系数低，直流叠加特性好的特点，软磁铁氧体最大优点是在具有较高的磁导率和电阻率(102～106Ω·cm)。
随着电动汽车的发展汽车电子元器件向着小型化和大电流化、宽温度应用方向发展，对软磁材料性能提出了更高的要求。功率电感器使用频率一般在100KHz及以上使用，一方面软磁合金往往由于电阻率较低，绝缘和耐压性能较低，高频损耗大而使磁心发热较大，造成器件的性能恶化，另一方面软磁铁氧体由于温度系数相对较高，造成器件的随温度变化磁导率变化大，造成器件在低温或高温环境下性能不稳定。另外，软磁合金粉芯的磁导率一般较低，为得到较高的电感量，器件往往需要增加绕线的圈数，从而造成铜损增加，器件的性能恶化，因而提高材料的起始磁导率必要。为对汽车电子应用功率电感的小型化和大电流化、宽温度应用的要求，开发对应的较高磁导率和高Bs、温度稳定性优良的复合软磁材料非常必要。
在国内已有一些相关复合软磁材料的制造方法的专利，具体如下：
(1)公开号为CN201410214573.4，公开日为2015.03.04，发明名称为“一种复合软磁材料及其制备方法”的中国专利公开了一种复合软磁材料及其制备方法，复合软磁材料的组分按包括按质量百分比计：FeSiCr82.56％～98.45％、Fe2O30.3％～8.9％、NiO0.1％～1.93％、ZnO0.1％～2.13％、CuO0.1％～0.53％。复合软磁材料的制备方法包括混合、预烧、粉碎、压制和烧结。本发明通过调整FeSiCr的含量来调整复合软磁材料的饱和磁感应强度，通过调整Fe2O3、NiO、ZnO、CuO的含量来调整生成的NiCuZn铁氧体的含量，从而提高复合软磁材料的绝缘和耐压性能。
(2)公开号为CN201410214841.2，公开日为2015.03.04，发明名称为“一种复合软磁材料及其制备方法”的中国专利公开了一种复合软磁材料及其制备方法，复合软磁材料中包括如下重量百分比的组分：75.13～86.12wt％的FeSiCr合金粉末、9～14.5wt％的Fe2O3、1.95～2.99wt％的NiO、2.15～3.75wt％的ZnO、0.55～1.43wt％的CuO、0.03～0.85wt％的Bi2O3、0.15～0.45wt％的V2O5、0.05～0.9wt％的SiO2。制备 时，按照如上所述组分配比配料，经过混合、预烧、粉碎、造粒、压制和烧结后，制得所述复合软磁材料。本发明的复合软磁材料及其制备方法，采用特定配比含量的组分，从而通过各材料的含量调整或者某些组分的添加，配合生产工艺，制得具有高绝缘﹑高耐压﹑高Bs性能的复合软磁材料。
(3)公开号为CN201410214819.8，公开日为2015.03.11，发明名称为“复合软磁材料及其制备方法”的中国专利公开了一种复合软磁材料及其制备方法，该复合软磁材料包括如下组份：48.25～76.91wt％FeSiCr、15～30.5wt％Fe2O3、3～9wt％NiO、3.8～7.3wt％ZnO、1.0～2.5wt％CuO、0.01～0.65wt％Bi2O3、0.03～0.55wt％V2O5、0.15～0.75wt％SiO2、0.1～0.5wt％Mn3O4。该复合软磁材料具有高起始磁导率和高Bs。
(4)公开号为CN201110152217.0，公开日为2012.02.22，发明名称为“一种复合软磁材料及其制备方法”的中国专利公开了一种具有高密度、高磁感的复合软磁材料及其制备方法。该复合软磁材料由雾化铁基粉末、润滑剂和金属助粘剂组成，其中润滑剂的质量为雾化铁基粉末质量的0.01-2％，金属助粘剂的质量为雾化铁基粉末质量的0.01-2％；所述金属助粘剂和润滑剂均匀包覆在雾化铁基粉末颗粒表面。所述润滑剂为纳米活性碳酸钙和/或纳米三氧化二铝，金属助粘剂为钛酸酯。本发明制备工艺简单、材料成本低，密度高、磁感应强度大。
发明内容
为了克服现有技术的不足，本发明提供了一种复合软磁材料及其制备方法，以得到具有高起始磁导率和高Bs、稳定的温度特性的复合软磁材料。
一种复合软磁材料，包括如下重量百分比的组份：
67.9～95.54wt％FeSiCr、0.1～0.3wt％TiO2、0.15～0.75wt％SiO2、0.1～0.5wt％Mn3O4、0.1～0.5wt％ZnO、3.4～25.9wt％BaO、0.4～3wt％B2O3、0.2～0.85wt％CaO、0.01～0.3wt％CuO。
进一步地，FeSiCr为平均粒径为5～100μm的粉末。
进一步地，TiO2、SiO2、Mn3O4、ZnO、BaO、B2O3、CaO和CuO的粒径均为50～100nm。
进一步地，FeSiCr、TiO2、SiO2、Mn3O4、ZnO、BaO、B2O3、CaO和CuO分别占所述复合软磁材料的90.1wt％、0.17wt％、0.3wt％、0.45wt％、0.3wt％、7.41wt％、0.92wt％、0.26wt％、0.09wt％。
一种所述复合软磁材料的制备方法，包括如下步骤：
混合步骤：将FeSiCr、TiO2、SiO2、Mn3O4和ZnO进行干法混合，得到混合料；
预压步骤：将所述混合料采用粉末成型机压制的混合坯料；
预烧步骤：将所述混合料在氮气保护进行预烧，得到预烧料；
粉碎步骤：使用溶剂，将BaO、B2O3、CaO、CuO与所述预烧料进行混合后进行湿法粉碎，得到粉碎浆料；
造粒步骤：在所述粉碎浆料中加入造粒辅助剂，在超声波下分散后，进行造粒，得到颗粒料；
压制步骤：将所述颗粒料采用粉末成型机压制得到坯件；
烧结步骤：烧结所述坯件以得到所述复合软磁材料；
其中FeSiCr、TiO2、SiO2、Mn3O4、ZnO、BaO、B2O3、CaO、CuO的添加量满足如下重量百分比关系：
67.9～95.54wt％FeSiCr、0.1～0.3wt％TiO2、0.15～0.75wt％SiO2、0.1～0.5wt％Mn3O4、0.1～0.5wt％ZnO、3.4～25.9wt％BaO、0.4～3wt％B2O3、0.2～0.85wt％CaO、0.01～0.3wt％CuO。
进一步地，FeSiCr、TiO2、SiO2、Mn3O4、ZnO、BaO、B2O3、CaO、CuO的添加量满足如下重量百分比关系：
90.1wt％FeSiCr、0.17wt％TiO2、0.3wt％SiO2、0.45wt％Mn3O4、0.3wt％ZnO、7.41wt％BaO、0.92wt％B2O3、0.26wt％CaO、0.09wt％CuO。
进一步地，所述溶剂为无水乙醇。
进一步地，所述造粒辅助剂为聚丙烯酰胺。
进一步地，所述方法满足以下工艺条件中的任一者或多者：
a)在所述混合步骤中，混合时间为30～70分钟；
b)在所述预压步骤中，预压压力为5吨/cm2；
c)在所述预烧步骤中，预烧温度控制在750±20℃，预烧时间为100～200分钟，氧含量控制在1％以下；
d)在所述粉碎步骤中，粉碎时间为120～240分钟，粉碎后料浆粒径控制在1.5～35μm；
e)在所述造粒步骤，聚丙烯酰胺等于所述粉碎浆料重量的2％至6％；
f)在所述压制步骤中，所述坯件的压制密度控制在(5.80±0.10)g/cm3；
g)在所述烧结步骤中，烧结温度控制在920℃～960℃，保温200～300分钟，烧结气氛为氮气，氧含量控制在1％以下。
进一步地，FeSiCr为平均粒径为5～100μm的粉末，TiO2、SiO2、Mn3O4、ZnO、BaO、B2O3、CaO和CuO的粒径均为50～100nm。
本发明的有益技术效果：
本发明采用合理的主配方，通过设定FeSiCr粉末的含量来调整材料的饱和磁感应强度；通过增加纳米SiO2的含量提高材料的绝缘和耐压性能；加入纳米Mn3O4和纳米 ZnO提高材料的磁导率；通过加入纳米TiO2来调整材料温度系数；通过设定纳米BaO、B2O3、CaO、CuO的含量来调整生成的低熔点相的含量，从而提高材料的磁导率和进一步增加材料的绝缘和耐压性能；再通过制备生产工艺进一步调整材料结晶分布，从而得到较高的磁导率和Bs，并且保证一定的绝缘和耐压性能。该材料具有较高磁导率和高Bs的特点，适应功率电感的小型化和大电流化对软磁材料的的要求。
附图说明
图1是本发明实施例和对比例的μi温度曲线图。
具体实施方式
以下对发明的较佳实施例作进一步详细说明。
一种复合软磁材料，包括如下组分：
67.9～95.54wt％FeSiCr、0.1～0.3wt％TiO2、0.15～0.75wt％SiO2、0.1～0.5wt％Mn3O4、0.1～0.5wt％ZnO、3.4～25.9wt％BaO、0.4～3wt％B2O3、0.2～0.85wt％CaO、0.01～0.3wt％CuO。
在一些实施例中，FeSiCr为平均粒径为5～100μm的粉末。
在一些实施例中，TiO2、SiO2、Mn3O4、ZnO、BaO、B2O3、CaO和CuO的粒径均为50～100nm。
在特别优选的实施例中，FeSiCr、TiO2、SiO2、Mn3O4、ZnO、BaO、B2O3、CaO和CuO分别占所述复合软磁材料的90.1wt％、0.17wt％、0.3wt％、0.45wt％、0.3wt％、7.41wt％、0.92wt％、0.26wt％、0.09wt％。
一种所述的复合软磁材料制备方法，包括如下步骤：
混合步骤：先将FeSiCr、TiO2、SiO2、Mn3O4和ZnO分别按照90.1wt％、0.17wt％、0.3wt％、0.45wt％、0.3wt％进行干法混合，得到混合料；
预压步骤：将所述混合料采用粉末成型机压制的混合坯料；
预烧步骤：将所述混合料在氮气保护进行预烧，得到预烧料；
粉碎步骤：使用溶剂，将BaO、B2O3、CaO、CuO按照7.41wt％、0.92wt％、0.26wt％、0.09wt％与所述预烧料进行混合后进行湿法粉碎，得到粉碎浆料；溶剂优选可采用无水乙醇；
造粒步骤：在所述粉碎浆料中加入造粒辅助剂，优选为聚丙烯酰胺，在超声波下分散后，进行造粒，得到颗粒料；
压制步骤：将所述颗粒料采用粉末成型机压制得到坯件；
烧结步骤：在氮气保护中烧结所述坯件烧结结束后随炉冷却至室温。
其中，上述混合步骤中，采用干法混合以利于预烧步骤，否则采用湿法混合，则延长了预烧步骤；采用预压步骤进一步降低了预烧步骤；而在粉碎步骤中，采用湿法混合则利于接着的造粒步骤，造粒前时使用超声波分散有利于胶水更加均匀的包覆在粉末颗粒表面，这样才能更好地进行造粒。
在一些实施例中，在所述混合步骤中，混合时间为30～70分钟。
在一些实施例中，在所述预烧步骤中，预烧温度控制在750±20℃，预烧时间为100～200分钟，氧气含量控制在1％以下。
在一些实施例中，在所述粉碎步骤中，粉碎时间为120～240分钟，粉碎后料浆粒径控制在1.5～35μm。
在一些实施例中，在所述造粒步骤，聚丙烯酰胺等于粉碎浆料重量的2％～6％，优选为4.5％。
在一些实施例中，在所述压制步骤中，所述坯体的压制密度控制在(5.80±0.10)g/cm3；
在一些实施例中，在所述烧结步骤中，烧结温度控制在920℃～960℃，保温200～300分钟，烧结气氛为氮气，氧气量控制在1％以下。
本发明采用合理的主配方，通过调整FeSiCr粉末的含量来调整材料的饱和磁感应强度；通过增加纳米SiO2的含量提高材料的绝缘和耐压性能；加入纳米Mn3O4和纳米ZnO提高材料的磁导率；通过加入纳米TiO2来调整材料温度系数；通过调整纳米BaO、B2O3、CaO、CuO的含量来调整生成的低熔点相的含量，从而提高材料的磁导率和进一步增加材料的绝缘和耐压性能；再通过制备生产工艺进一步调整材料结晶分布，从而得到较高的磁导率和Bs，并且保证一定的绝缘和耐压性能。该材料具有较高磁导率和高Bs的特点，适应功率电感的小型化和大电流化对软磁材料的要求。
材料的性能指标如下：
(1)起始磁导率μi：115(1±20％)
(2)饱和磁感应强度Bs：≥1000mT
(3)绝缘电阻：≥50MΩ
(4)耐压：≥50V
温度系数αμiγ(10-6/℃)：-10～10。
在一些具体实施例中，复合软磁材料的制备方法如下：
(1)混合：按表1(实施例和对比例)所述的起始配料成分后进行干法混合，混合时间为30～70分钟；
(2)预压：采用粉末成型机按照5吨/cm2的压力将混合后粉末预压成块
(3)预烧：将块状的材料在氮气保护推板窑中进行预烧，预烧温度控制在550±20℃，预烧时间为100～200分钟，氧含量控制在1％以下；
(4)粉碎：在上步预烧得到的预烧料中加入粉碎添加成分进行湿法粉碎，以无水 乙醇为溶剂，粉碎时间为120～240分钟，粉碎后料浆粒径控制在1.5～35μm；
(5)造粒：在上步的料浆加入相当于料浆重量的4.5％的聚丙烯酰胺在超声波下分散，进行造粒，得到颗粒料；
(6)压制：将上步的颗粒料采用粉末成型机压制得到坯件，坯件的压制密度控制在(5.80±0.10)g/cm3；
(7)烧结：在氮气保护电阻炉中进行烧结，烧结温度控制在920℃～960℃，保温200～300分钟，烧结气氛为氮气，氧含量控制在1％以下，烧结结束后随炉冷却至室温。
通过以上工序制得所述复合材料磁环样品(磁环尺寸为T8×5×2)。
将烧结后的复合材料磁环分别进行测试和评价。在匝数N＝26Ts条件下，使用HP-4284型LCR测试仪测试磁环样品的起始磁导率μi；用SY-8218型B-H分析仪测试样品的饱和磁感应强度Bs；用CH-333型绝缘耐压测试仪测试样品的绝缘和耐压性能；用WKS3-270/70/20快速温变箱和ZM2371型LCR表测试磁环样品的温度特性
表1  实施例和对比例的成分配比
Figure PCTCN2016082075-appb-000001
Figure PCTCN2016082075-appb-000002
表2  实施例和对比例的性能及评价
Figure PCTCN2016082075-appb-000003
Figure PCTCN2016082075-appb-000004
注意:超过规格的附加“*”。
表2列出了实施例和对比例的性能及评价，从表2中可以看出，本发明的实施例和对比例相比较，本发明有效地提高了材料的起始磁导率，并能保持相应的绝缘和耐压性能，较高的饱和磁感应强度，接近零的温度系数。本发明的起始磁导率可以达到115(1±20％)。如表所示，实施例1的Bs明显优于对比例1，实施例1的比温度系数αμiγ明显优于对比例1。对比实施例和对比例的μi温度曲线图(图1)，实施例的温度稳定特性明显比对比例的更加稳定。拥有较高的Bs，而较高的Bs通常对应较高的饱和电流；并且拥有接近于0的比温度系数αμiγ，而接近于0的比温度系数对应材料可工作的应用范围更加广泛，并且频率特性基本与相应的铁氧体材料基本一致，本发明的材料应该能够满足汽车电子用功率电感的小型化和大电流化、宽温度应用对软磁材料的要求。
以上内容是结合具体的优选实施方式对本发明所作的进一步详细说明，不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干简单推演或替换，都应当视为属于本发明由所提交的权利要求书确定的专利保护范围。

Claims (10)

  1. 一种复合软磁材料，其特征是，包括如下重量百分比的组份：
    67.9～95.54wt％FeSiCr、0.1～0.3wt％TiO2、0.15～0.75wt％SiO2、0.1～0.5wt％Mn3O4、0.1～0.5wt％ZnO、3.4～25.9wt％BaO、0.4～3wt％B2O3、0.2～0.85wt％CaO、0.01～0.3wt％CuO。
  2. 如权利要求1所述的复合软磁材料，其特征是，FeSiCr为平均粒径为5～100μm的粉末。
  3. 如权利要求1或2所述的复合软磁材料，其特征是，TiO2、SiO2、Mn3O4、ZnO、BaO、B2O3、CaO和CuO的粒径均为50～100nm。
  4. 如权利要求1至3任一项所述的复合软磁材料，其特征是：FeSiCr、TiO2、SiO2、Mn3O4、ZnO、BaO、B2O3、CaO和CuO分别占所述复合软磁材料的90.1wt％、0.17wt％、0.3wt％、0.45wt％、0.3wt％、7.41wt％、0.92wt％、0.26wt％、0.09wt％。
  5. 一种如权利要求1至4任一所述的复合软磁材料的制备方法，其特征是，包括如下步骤：
    混合步骤：将FeSiCr、TiO2、SiO2、Mn3O4和ZnO进行干法混合，得到混合料；
    预压步骤：将所述混合料采用粉末成型机压制的混合坯料；
    预烧步骤：将所述混合料在氮气保护进行预烧，得到预烧料；
    粉碎步骤：使用溶剂，将BaO、B2O3、CaO、CuO与所述预烧料进行混合后进行湿法粉碎，得到粉碎浆料；
    造粒步骤：在所述粉碎浆料中加入造粒辅助剂，在超声波下分散后，进行造粒，得到颗粒料；
    压制步骤：将所述颗粒料采用粉末成型机压制得到坯件；
    烧结步骤：烧结所述坯件以得到所述复合软磁材料；
    其中FeSiCr、TiO2、SiO2、Mn3O4、ZnO、BaO、B2O3、CaO、CuO的添加量满足如下重量百分比关系：
    67.9～95.54wt％FeSiCr、0.1～0.3wt％TiO2、0.15～0.75wt％SiO2、0.1～0.5wt％Mn3O4、0.1～0.5wt％ZnO、3.4～25.9wt％BaO、0.4～3wt％B2O3、0.2～0.85wt％CaO、0.01～0.3wt％CuO。
  6. 如权利要求5所述的复合软磁材料的制备方法，其特征是：FeSiCr、TiO2、SiO2、Mn3O4、ZnO、BaO、B2O3、CaO、CuO的添加量满足如下重量百分比关系：
    90.1wt％FeSiCr、0.17wt％TiO2、0.3wt％SiO2、0.45wt％Mn3O4、0.3wt％ZnO、7.41wt％BaO、0.92wt％B2O3、0.26wt％CaO、0.09wt％CuO。
  7. 如权利要求5或6所述的复合软磁材料的制备方法，其特征是：所述溶剂为无 水乙醇。
  8. 如权利要求5至7任一项所述的复合软磁材料的制备方法，其特征是：所述造粒辅助剂为聚丙烯酰胺。
  9. 如权利要求5至8任一项所述的复合软磁材料的制备方法，其特征是：满足以下工艺条件中的任一者或多者：
    a)在所述混合步骤中，混合时间为30～70分钟；
    b)在所述预压步骤中，预压压力为5吨/cm2；
    c)在所述预烧步骤中，预烧温度控制在750±20℃，预烧时间为100～200分钟，氧含量控制在1％以下；
    d)在所述粉碎步骤中，粉碎时间为120～240分钟，粉碎后料浆粒径控制在1.5～35μm；
    e)在所述造粒步骤，造粒辅助剂等于所述粉碎浆料重量的2％至6％；
    f)在所述压制步骤中，所述坯件的压制密度控制在(5.80±0.10)g/cm3；
    g)在所述烧结步骤中，烧结温度控制在920℃～960℃，保温200～300分钟，烧结气氛为氮气，氧含量控制在1％以下。
  10. 如权利要求5至9任一项所述的复合软磁材料的制备方法，其特征是：FeSiCr为平均粒径为5～100μm的粉末，TiO2、SiO2、Mn3O4、ZnO、BaO、B2O3、CaO和CuO的粒径均为50～100nm。
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