CN113436876B - High-antirust high-saturation inductance material, preparation method and integrated inductor - Google Patents

High-antirust high-saturation inductance material, preparation method and integrated inductor Download PDF

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CN113436876B
CN113436876B CN202110714339.8A CN202110714339A CN113436876B CN 113436876 B CN113436876 B CN 113436876B CN 202110714339 A CN202110714339 A CN 202110714339A CN 113436876 B CN113436876 B CN 113436876B
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powder
hydroxide
antirust
resin
spherical powder
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CN113436876A (en
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练坚平
曾艳丽
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Guangdong Precision Dragon Electronic Technology Co ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/02Apparatus 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
    • H01F41/0206Manufacturing of magnetic cores by mechanical means
    • H01F41/0246Manufacturing of magnetic circuits by moulding or by pressing powder
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F27/00Details of transformers or inductances, in general
    • H01F27/24Magnetic cores
    • H01F27/255Magnetic cores made from particles

Abstract

The invention discloses a high-rust-resistance high-saturation inductance material, a preparation method and an integrated inductor. B can inhibit the migration of Fe so that the alpha-Fe in the softened spherical powder particles keeps a high proportion, and therefore the softened spherical powder has high Bs and high direct current superposition resistance. Therefore, the antirust performance of the inductor can be effectively improved, the inductance value of the inductor is improved, and the application requirements of different environments are met. The invention forms a high-density anti-corrosion layer on the surface of the material by controlling the components and the process of the material, and homogenizes the air gap of the magnet by the uniform anti-corrosion layer and the uniformly filled material so as to ensure that the material is more excellent in saturation.

Description

High-antirust high-saturation inductance material, preparation method and integrated inductor
Technical Field
The invention relates to the technical field of inductors, in particular to a high-rust-resistance high-saturation inductor material, a preparation method and an integrally formed inductor.
Background
With the rapid development of microelectronic semiconductor technology, the switching power supply is widely applied to various fields closely related to life, such as personal computers, base stations, radio equipment, aerospace and the like, and gradually takes a small volume, a large output current capability and good transient response as a main development situation. The integrally formed inductor has the characteristics of small volume and good direct current superposition performance, is widely applied to the power supply technology of electronic equipment, and plays a key role in energy conversion from a power supply to a device.
However, the resistivity of the traditional alloy soft magnetic material is low, the eddy current is large under high frequency, the use of the traditional alloy soft magnetic material under high frequency is limited seriously, and the solution of the metal material is rusted under the environment of high temperature and high humidity to cause failure, so that the working requirement under severe environment can not be met, a material with high direct current superposition performance and an integrated inductor need to be developed, and the possibility of long-term use of the device under severe environment is improved.
CN110181036A discloses a composite soft magnetic metal powder, a preparation method and an integrally formed inductor, wherein the preparation method of the composite soft magnetic metal powder comprises the following steps: passivating, preparing a coating agent, coating soft magnetic metal powder, granulating and adding a lubricant. The invention has the advantages that the high-voltage impact resistance of the soft magnetic composite metal powder is greatly improved by adding the rare earth oxide into the soft magnetic composite metal powder, and the performance of the integrally formed inductor is further improved. The invention has certain rust prevention and insulation properties through the phosphorus-containing solution passivation powder, and is further enhanced by adding the rare earth oxide, but the magnetic conductivity of the material is greatly reduced due to the addition of the phosphating passivation, and the phosphating passivation film is a reticular film layer and has poor rust prevention performance, while the rare earth oxide cannot react with the phosphating film and cannot play a role in compacting the phosphating film, so the rust prevention performance of the inductor is not ideal.
CN111383835A discloses FeSiCr particles for integrally forming inductors and a preparation method thereof. The preparation method of the FeSiCr particle material for the integrally formed inductor is characterized by taking FeSiCr alloy powder as a raw material and carrying out phosphoric acid passivation, primary baking, glue preparation, glue coating, granulation, air drying, secondary baking and material mixing on the raw material, wherein the glue preparation raw material comprises an organic solvent, silicon dioxide coated nano aluminum nitride, methyl phenyl silicone resin, epoxy resin and epoxy resin curing agent. According to the invention, the FeSiCr material is coated, the double-layer coating is formed by coating the organic resin to improve the insulation of the material, reduce the loss and provide the adhesive force, and the nano oxide is coated and coated to improve the insulation of the material, but the organic coating is gradually aged due to environmental changes such as high temperature, acid and alkali and the like and has a larger risk, so that the organic coating is not an ideal antirust insulation coating, the inductor can lose effectiveness after being used for a long time or under a severe condition, the resin needs a larger thickness to achieve higher resistance and antirust effect, and the oxide powder is coated with a large amount of gaps, so that the coating density is insufficient and the antirust effect is poor.
Accordingly, the prior art is deficient and needs improvement.
Disclosure of Invention
The invention provides a high-antirust high-saturation inductor material, a preparation method and an integrally formed inductor, which can improve the antirust performance of the inductor, improve the inductance value of the inductor and meet the application requirements of different environments.
The technical scheme of the invention is as follows: the preparation method of the high-antirust high-saturation inductance material comprises the following steps.
S1: adding the raw material alloy into plasma spheroidizing equipment, and making the raw material alloy into initial spherical powder of 15-55 um through plasma spheroidizing; wherein the raw material alloy comprises the following material components: 88-96 wt% Fe, 2.9-4.5 wt% Si, 0.5-3.0 wt% Co, 0.5-3.0 wt% B, 0.05-0.75 wt% Cr and/or Al and/or Ti, 0.05-0.75 wt% Y and/or Ca and/or Ba and/or Na and/or Li.
S2: treating the initial spherical powder in a reducing atmosphere of 400-1100 ℃ for 10min-10h to obtain softened spherical powder.
S3: mixing the softened spherical powder with a high Bs material with the particle size of 0.1-10um to obtain mixed powder; wherein, the high Bs material needs to be added with hydroxide and phosphoric acid in advance and mixed evenly, and then dried in inert gas, the drying temperature is 80-600 ℃, and the surface of the high Bs material is coated with a layer of hydroxide and phosphoric acid; wherein the addition amount of the high Bs material is 1-75% of the mass of the softened spherical powder.
S4: uniformly mixing the mixed powder with bonding resin to obtain bonding powder; wherein the binding resin accounts for 0.005-0.1 wt% of the mixed powder. The bonding resin is epoxy resin, and the hydroxyl value of the epoxy resin is less than 5.5 wt%; or the bonding resin is unsaturated polyester resin, and the molecular weight of the unsaturated polyester resin is less than 15000; or, the bonding resin is epoxy resin and unsaturated polyester resin, wherein the epoxy resin: the weight ratio of the unsaturated polyester resin is 0.2-2:1, the molecular weight of the unsaturated polyester resin is less than 15000, and the percentage of hydroxyl groups of the epoxy resin in the total amount of the epoxy resin is as follows: less than 5.5 wt%.
S5: drying the bonding powder under the protection of inert gas for 20min-10h to obtain a high-rust-resistance high-saturation inductance material; wherein the drying temperature is 30-90 ℃. The inert gas is preferably nitrogen or argon.
In step S1, the raw material alloy is processed by a plasma spheroidizing device to form an initial spherical powder, and due to the high temperature environment of the spheroidizing process, Cr and/or Al and/or Ti, Y and/or Ca and/or Ba and/or Na and/or Li in the initial spherical powder are segregated, so that a dense composite oxide film is formed on the surface of the initial spherical powder to form a rust-proof layer, and the rust-proof layer has high rust-proof performance and is tightly bonded with particles without falling off. In step S2, the reducing atmosphere reduces the surface of the dense composite oxide film to form a reducing layer, and the inside of the reducing layer is also the dense composite oxide film; after the inductor product is made, when the inductor product is used in a high-temperature and high-humidity environment, the reduction layer can be preferentially oxidized into a compact oxidation film, so that internal particles are protected from rusting. The step S2 is to reduce the surface of the dense oxide layer on the surface of the initial spherical powder by one layer, so that the surface can be softened for the convenience of the subsequent press molding. B can inhibit the migration of Fe so that the alpha-Fe in the softened spherical powder particles keeps a high proportion, so that the softened spherical powder has high Bs and high direct current superposition resistance; the addition of a trace amount of Co forms partial Co-based alloy, so that Ms of the material is further improved, and the direct current superposition resistance of the material is improved; furthermore, the anti-direct current superposition performance is further improved by adding small-particle high Bs materials into the softened spherical powder, and the oxide layer on the surface of the softened spherical powder is sufficient to isolate small-particle Fe materials and the like, so that the antirust performance of the product is not reduced. The steric hindrance of the powder to the powder in the moving process is increased by controlling the proportion of the epoxy resin hydroxyl groups, and the small particles are more uniformly distributed in the large particles by coating the surfaces of the small particles with the nonmetal structures, so that the whole air gap of the product is more uniformly distributed. Therefore, the antirust performance of the inductor can be effectively improved, the inductance value of the inductor is improved, and the application requirements of different environments are met.
The high Bs material is one or a mixture of at least two of Fe powder, FeSi powder, FeNi powder, Fe-based amorphous powder and Ni-based amorphous powder.
The hydroxide is: at least one of sodium hydroxide, aluminum hydroxide, potassium hydroxide, magnesium hydroxide, barium hydroxide, lithium hydroxide, strontium hydroxide, calcium hydroxide, and manganese hydroxide.
The raw material alloy is firstly drawn into a metal wire with the diameter of 0.1mm-5mm, then the metal wire is added into plasma spheroidization equipment, and the raw material alloy is made into initial spherical powder of 15um-55um through plasma spheroidization.
In step S3, the softened spherical powder is mixed with the high Bs material using a mixer at high speed with the rotation speed of the paddle being greater than 1000 rpm.
The reducing atmosphere comprises hydrogen and/or carbon monoxide and/or ammonia.
A high-antirust high-saturation inductance material is prepared by the preparation method of the high-antirust high-saturation inductance material.
An integrally formed inductor is formed in a die by adopting the high-rust-resistance high-saturation inductor material, and the pressure is 400-600 MPa.
By adopting the scheme, the invention provides the high-antirust high-saturation inductance material, the preparation method and the integrally formed inductor, the raw material alloy forms initial spherical powder through plasma spheroidization equipment, and Cr and/or Al and/or Ti, Y and/or Ca and/or Ba and/or Na and/or Li in the initial spherical powder are segregated due to the high-temperature environment in the spheroidization process, so that a compact composite oxide film is formed on the surface of the initial spherical powder to form an antirust layer, the antirust layer has high antirust performance and is tightly combined with particles without falling off. B can inhibit the migration of Fe so that the alpha-Fe in the softened spherical powder particles keeps a high proportion, so that the softened spherical powder has high Bs and high direct current superposition resistance; the addition of a trace amount of Co forms partial Co-based alloy, so that Ms of the material is further improved, and the direct current superposition resistance of the material is improved; furthermore, the anti-direct current superposition performance is further improved by adding small-particle high Bs materials into the softened spherical powder, and the oxide layer on the surface of the softened spherical powder is sufficient to isolate small-particle Fe materials and the like, so that the antirust performance of the product is not reduced. Therefore, the antirust performance of the inductor can be effectively improved, the inductance value of the inductor is improved, and the application requirements of different environments are met.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1
The embodiment provides a preparation method of a high-antirust high-saturation inductance material, which comprises the following steps.
S1: adding the raw material alloy into plasma spheroidizing equipment, and making the raw material alloy into initial spherical powder of 15-55 um through plasma spheroidizing; wherein the raw material alloy comprises the following material components: 96 wt% Fe, 2.9 wt% Si, 0.5 wt% Co, 0.5 wt% B, 0.05 wt% Al, 0.05 wt% Y.
S2: the initial spherical powder was treated in a reducing atmosphere at 800 ℃ for 3 hours to obtain a softened spherical powder. Wherein the reducing atmosphere is nitrogen and hydrogen, and the volume ratio of the nitrogen to the hydrogen is 6: 4.
S3: mixing the softened spherical powder with a high Bs material with the particle size of 2-10um to obtain mixed powder; in this embodiment, the high Bs material is Fe; the addition amount of the high Bs material is 10 wt% of the softened spherical powder, the surface of the high Bs material is coated with a mixed solution of sodium hydroxide and phosphoric acid and dried by nitrogen at 300 ℃, wherein the addition amount of the sodium hydroxide is 0.05% of the weight of the high Bs material powder, the addition amount of the phosphoric acid is 0.5% of the weight of the high Bs material powder, high-speed mixing is adopted for mixing, and the rotating speed of a stirring paddle is more than 1000 rpm.
S4: uniformly mixing the mixed powder with bonding resin to obtain bonding powder; wherein the binding resin is 0.01 wt% of the mixed powder. The bonding resin is epoxy resin and unsaturated polyester resin, wherein the epoxy resin: the weight ratio of the unsaturated polyester resin is 3:7, the molecular weight of the unsaturated polyester resin is less than 14000 +/-500, and the percentage of hydroxyl groups of the epoxy resin in the total amount of the epoxy resin is as follows: 5.45 wt%. In this step, a mixer is used to mix for 60min to obtain a cohesive powder.
S5: drying the bonding powder for 1h under the protection of nitrogen to obtain a high-rust-resistance high-saturation inductance material; wherein the drying temperature is 80 ℃.
This embodiment still provides an integrated into one piece inductance, wherein the spot welding coil parameter that contains among the integrated into one piece inductance specifically is: the wire diameter is 0.28mm, the inner diameter is 2.7mm, the number of turns is 17.75, the integrally formed inductor has the size of 6mm multiplied by 3mm, and the pressing pressure is 400MPa-600 MPa; and detecting the inductance value L and the saturation current of the integrated inductor by using WK6500B under the conditions of 1MHz and 1V. And (3) carrying out neutral salt spray test on the antirust performance of the integrally formed inductor by using a salt spray test box, wherein the test temperature is 35 +/-2 ℃, and the salt concentration is 5 +/-1%. See table 1 for specific numerical ranges.
Example 2
The embodiment provides a preparation method of a high-antirust high-saturation inductance material, which comprises the following steps.
S1: adding the raw material alloy into plasma spheroidizing equipment, and making the raw material alloy into initial spherical powder of 15-55 um through plasma spheroidizing; wherein the raw material alloy comprises the following material components: 88 wt% Fe, 4.5 wt% Si, 3.0 wt% Co, 3.0 wt% B, 0.75 wt% Co, 0.75 wt% Li.
S2: the initial spherical powder was treated in a reducing atmosphere at 500 ℃ for 8h to give a softened spherical powder. Wherein the reducing atmosphere is ammonia gas and argon gas, and the volume ratio of the ammonia gas to the argon gas is 7: 3.
S3: mixing the softened spherical powder with a high Bs material with the particle size of 2-10um to obtain mixed powder; in this embodiment, the high Bs material is FeSi; the addition amount of the high Bs material is 50 wt% of the softened spherical powder, the surface of the high Bs material is coated with a mixed solution of sodium hydroxide and phosphoric acid and dried by nitrogen at 500 ℃, wherein the addition amount of the sodium hydroxide is 0.08% of the weight of the high Bs material powder, the addition amount of the phosphoric acid is 0.7% of the weight of the high Bs material powder, high-speed mixing is adopted for mixing, and the rotating speed of a stirring paddle is more than 1000 rpm.
S4: uniformly mixing the mixed powder with bonding resin to obtain bonding powder; wherein the binding resin is 0.05 wt% of the mixed powder. The bonding resin is epoxy resin and unsaturated polyester resin, wherein the epoxy resin: the weight ratio of the unsaturated polyester resin is 4:6, the molecular weight of the unsaturated polyester resin is 12000 +/-500, and the percentage of hydroxyl groups of the epoxy resin in the total amount of the epoxy resin is as follows: 5.32 wt%. In this step, a mixer is used to mix for 10min to obtain a cohesive powder.
S5: drying the bonding powder for 3h under the protection of argon to obtain a high-rust-resistance high-saturation inductance material; wherein the drying temperature is 50 ℃.
This embodiment still provides an integrated into one piece inductance, wherein the spot welding coil parameter that contains among the integrated into one piece inductance specifically is: the wire diameter is 0.28mm, the inner diameter is 2.7mm, the number of turns is 17.75, the integrally formed inductor has the size of 6mm multiplied by 3mm, and the pressing pressure is 400MPa-600 MPa; and detecting the inductance value L and the saturation current of the integrated inductor by using WK6500B under the conditions of 1MHz and 1V. And (3) carrying out neutral salt spray test on the antirust performance of the integrally formed inductor by using a salt spray test box, wherein the test temperature is 35 +/-2 ℃, and the salt concentration is 5 +/-1%. See table 1 for specific numerical ranges.
Example 3
The embodiment provides a preparation method of a high-antirust high-saturation inductance material, which comprises the following steps.
S1: adding the raw material alloy into plasma spheroidizing equipment, and making the raw material alloy into initial spherical powder of 15-55 um through plasma spheroidizing; wherein the raw material alloy comprises the following material components: 93 wt% Fe, 3.5 wt% Si, 2.5 wt% Co, 1.5 wt% B, 0.35 wt% Ti, 0.15 wt% Ca.
S2: the initial spherical powder was treated in a reducing atmosphere at 700 ℃ for 4 hours to obtain a softened spherical powder. Wherein the reducing atmosphere is carbon monoxide and nitrogen, and the volume ratio of the carbon monoxide to the nitrogen is 5: 5.
S3: mixing the softened spherical powder with a high Bs material with the particle size of 2-8um to obtain mixed powder; in this embodiment, the high Bs material is FeSiB; the addition amount of the high Bs material is 30 wt% of the softened spherical powder, the surface of the high Bs material is coated with a mixed solution of magnesium hydroxide and phosphoric acid and dried by nitrogen gas at 400 ℃, wherein the addition amount of the magnesium hydroxide is 0.10% of the weight of the high Bs material powder, the addition amount of the phosphoric acid is 1% of the weight of the high Bs material powder, high-speed mixing is adopted for mixing, and the rotation speed of a stirring paddle is more than 1000 rpm.
S4: uniformly mixing the mixed powder with bonding resin to obtain bonding powder; wherein the binding resin is 0.05 wt% of the mixed powder. The bonding resin is epoxy resin and unsaturated polyester resin, wherein the epoxy resin: the weight ratio of the unsaturated polyester resin is 6:4, the molecular weight of the unsaturated polyester resin is 11000 +/-500, and the percentage of hydroxyl groups of the epoxy resin in the total amount of the epoxy resin is as follows: 5.48 wt%. In this step, a mixer is used to mix for 30min to obtain a cohesive powder.
S5: drying the bonding powder for 2h under the protection of argon to obtain a high-rust-resistance high-saturation inductance material; wherein the drying temperature is 70 ℃.
This embodiment still provides an integrated into one piece inductance, wherein the spot welding coil parameter that contains among the integrated into one piece inductance specifically is: the wire diameter is 0.28mm, the inner diameter is 2.7mm, the number of turns is 17.75, the integrally formed inductor has the size of 6mm multiplied by 3mm, and the pressing pressure is 400MPa-600 MPa; and detecting the inductance value L and the saturation current of the integrated inductor by using WK6500B under the conditions of 1MHz and 1V. And (3) carrying out neutral salt spray test on the antirust performance of the integrally formed inductor by using a salt spray test box, wherein the test temperature is 35 +/-2 ℃, and the salt concentration is 5 +/-1%. See table 1 for specific numerical ranges.
Example 4
The embodiment provides a preparation method of a high-antirust high-saturation inductance material, which comprises the following steps.
S1: adding the raw material alloy into plasma spheroidizing equipment, and making the raw material alloy into initial spherical powder of 15-55 um through plasma spheroidizing; wherein the raw material alloy comprises the following material components: 91 wt% Fe, 4.0 wt% Si, 2.0 wt% Co, 2.0 wt% B, 0.6 wt% Al, 0.4 wt% Y.
S2: the initial spherical powder was treated in a reducing atmosphere at 650 ℃ for 7h to give a softened spherical powder. Wherein the reducing atmosphere is hydrogen and nitrogen, and the volume ratio of the hydrogen to the nitrogen is 4: 6.
S3: mixing the softened spherical powder with a high Bs material with the particle size of 2-5um to obtain mixed powder; in this embodiment, the high Bs material is FeNi; the addition amount of the high Bs material is 25 wt% of the softened spherical powder, the surface of the high Bs material is coated with a mixed solution of manganese hydroxide and phosphoric acid and dried by nitrogen at 450 ℃, wherein the addition amount of the manganese hydroxide is 0.06% of the weight of the high Bs material powder, the addition amount of the phosphoric acid is 0.8% of the weight of the high Bs material powder, high-speed mixing is adopted for mixing, and the rotating speed of a stirring paddle is more than 1000 rpm.
S4: uniformly mixing the mixed powder with bonding resin to obtain bonding powder; wherein the binding resin is 0.02 wt% of the mixed powder. The bonding resin is epoxy resin and unsaturated polyester resin, wherein the epoxy resin: the weight ratio of the unsaturated polyester resin is 5:5, the molecular weight of the unsaturated polyester resin is 7000 +/-500, and the percentage of hydroxyl groups of the epoxy resin in the total amount of the epoxy resin is as follows: 5.31 wt%. In this step, a mixer is used to mix for 40min to obtain a cohesive powder.
S5: drying the bonding powder for 2.5h under the protection of argon to obtain a high-rust-resistance high-saturation inductance material; wherein the drying temperature is 60 ℃.
This embodiment still provides an integrated into one piece inductance, wherein the spot welding coil parameter that contains among the integrated into one piece inductance specifically is: the wire diameter is 0.28mm, the inner diameter is 2.7mm, the number of turns is 17.75, the integrally formed inductor has the size of 6mm multiplied by 3mm, and the pressing pressure is 400MPa-600 MPa; and detecting the inductance value L and the saturation current of the integrated inductor by using WK6500B under the conditions of 1MHz and 1V. And (3) carrying out neutral salt spray test on the antirust performance of the integrally formed inductor by using a salt spray test box, wherein the test temperature is 35 +/-2 ℃, and the salt concentration is 5 +/-1%. See table 1 for specific numerical ranges.
Comparative example 1
The material comprises 91 wt% of Fe, 4.0 wt% of Si, 2.0 wt% of Co, 2.0 wt% of B, 0.6 wt% of Al and 0.4 wt% of Y. Smelting the material in a high-frequency furnace to form molten metal, spraying the molten metal into a cooling tower through high-speed airflow, and quickly cooling the molten metal through rotating water flow to form metal spheroidal powder; mixing the treated metal spheroidal powder with FeNi powder with the grain diameter of 2-5um to obtain mixed powder, wherein the addition proportion of the FeNi powder is 25 wt% of the metal spheroidal powder, the mixing adopts high-speed mixing, and the rotating speed of a stirring paddle is more than 1000 rpm. Adding 0.02 wt% of epoxy resin and unsaturated polyester resin mixed solution into the mixed powder, wherein the weight ratio of the epoxy resin to the unsaturated polyester resin is 5:5, the molecular weight of the unsaturated polyester resin is 7000 +/-500, and the percentage of hydroxyl groups of the epoxy resin in the total amount of the epoxy resin is as follows: 5.31 wt%; mixed in a mixer for 40min and then dried at 60 ℃ for 2.5 hours under nitrogen or argon atmosphere to give a cohesive powder. The bonding powder obtained by the comparative example is used for preparing the integrally formed inductor, wherein the parameters of the spot welding coil contained in the integrally formed inductor are as follows: the wire diameter is 0.28mm, the inner diameter is 2.7mm, the number of turns is 17.75, the integrally formed inductor has the size of 6mm multiplied by 3mm, and the pressing pressure is 400MPa-600 MPa. See table 1 for specific numerical ranges.
Comparative example 2
The material composition is FeSiCr powder with 91 wt% of Fe, 4.5 wt% of Si and 4.5 wt% of Cr. Adding a phosphoric acid solution with the concentration of 10 percent and the weight of 0.5 percent of that of FeSiCr powder, treating, drying, adding a mixed solution of epoxy resin and unsaturated polyester resin with the weight of 0.02 percent of that of the powder into the treated FeSiCr powder, wherein the weight ratio of the epoxy resin to the unsaturated polyester resin is 5:5, the molecular weight of the unsaturated polyester resin is 7000 +/-500, and the percentage of hydroxyl groups of the epoxy resin in the total amount of the epoxy resin is as follows: 5.31 wt%; mixed in a mixer for 40min and then dried at 60 ℃ for 2.5 hours under nitrogen or argon atmosphere to give a cohesive powder. The bonding powder obtained by the comparative example is used for preparing the integrally formed inductor, wherein the parameters of the spot welding coil contained in the integrally formed inductor are as follows: the wire diameter is 0.28mm, the inner diameter is 2.7mm, the number of turns is 17.75, the integrally formed inductor has the size of 6mm multiplied by 3mm, and the pressing pressure is 400MPa-600 MPa. See table 1 for specific numerical ranges.
TABLE 1
Figure BDA0003134266770000101
Referring to table 1, the rust inhibitive performance of the integrally formed inductors fabricated in examples 1 to 4 was much better than that of comparative examples 1 and 2; the current values of examples 1 to 4 at which the inductance was reduced by 30% were also significantly higher than those of comparative examples 1 and 2, and it can be seen that the present invention is more advantageous in practical large current applications; the inductance values of the integrally formed inductors manufactured in the embodiments 1 to 4 are superior to those of the comparative examples 1 and 2, and the application prospect is good. By controlling the material components and the process, a high-density anti-corrosion layer is formed on the surface of the material, the material saturation is better due to the homogenization of the air gaps of the magnet through the uniform anti-corrosion layer and the uniformly filled material, and the high-rust-resistance and high-saturation integrally-formed inductance material and the integrally-formed inductor can be prepared by using the method disclosed by the invention.
In summary, the invention provides a high-rust-resistance high-saturation inductance material, a preparation method and an integrated inductor, wherein a raw material alloy forms initial spherical powder through plasma spheroidization equipment, and Cr and/or Al and/or Ti, Y and/or Ca and/or Ba and/or Na and/or Li in the initial spherical powder are segregated due to the high-temperature environment in the spheroidization process, so that a dense composite oxide film is formed on the surface of the initial spherical powder to form a rust-proof layer, and the rust-proof layer has high rust-resistance performance and is tightly combined with particles without falling off. B can inhibit the migration of Fe so that the alpha-Fe in the softened spherical powder particles keeps a high proportion, so that the softened spherical powder has high Bs and high direct current superposition resistance; the addition of a trace amount of Co forms partial Co-based alloy, so that Ms of the material is further improved, and the direct current superposition resistance of the material is improved; furthermore, the anti-direct current superposition performance is further improved by adding small-particle high Bs materials into the softened spherical powder, and the oxide layer on the surface of the softened spherical powder is sufficient to isolate small-particle Fe materials and the like, so that the antirust performance of the product is not reduced. Therefore, the antirust performance of the inductor can be effectively improved, the inductance value of the inductor is improved, and the application requirements of different environments are met.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (7)

1. The preparation method of the high-antirust high-saturation inductance material is characterized by comprising the following steps of:
s1: adding the raw material alloy into plasma spheroidizing equipment, and making the raw material alloy into initial spherical powder of 15-55 um through plasma spheroidizing; wherein the raw material alloy comprises the following material components: 88-96 wt% Fe, 2.9-4.5 wt% Si, 0.5-3.0 wt% Co, 0.5-3.0 wt% B, 0.05-0.75 wt% Cr and/or Al and/or Ti, 0.05-0.75 wt% Y and/or Ca and/or Ba and/or Na and/or Li;
s2: treating the initial spherical powder in a reducing atmosphere at 400-1100 ℃ for 10min-10h to obtain softened spherical powder;
s3: mixing the softened spherical powder with a high Bs material with the particle size of 0.1-10um to obtain mixed powder; wherein, the high Bs material needs to be added with hydroxide and phosphoric acid in advance and mixed evenly, and then dried in inert gas, and the drying temperature is 80-600 ℃; wherein, the addition amount of the high Bs material is 1% -75% of the mass of the softened spherical powder;
s4: uniformly mixing the mixed powder with bonding resin to obtain bonding powder; wherein, the bonding resin accounts for 0.005-0.1 wt% of the mixed powder;
the bonding resin is epoxy resin, and the hydroxyl value of the epoxy resin is less than 5.5 wt%; or the bonding resin is unsaturated polyester resin, and the molecular weight of the unsaturated polyester resin is less than 15000; or, the bonding resin is epoxy resin and unsaturated polyester resin, wherein the epoxy resin: the weight ratio of the unsaturated polyester resin is 0.2-2:1, the molecular weight of the unsaturated polyester resin is less than 15000, and the percentage of hydroxyl groups of the epoxy resin in the total amount of the epoxy resin is as follows: less than 5.5 wt%;
s5: drying the bonding powder under the protection of inert gas for 20min-10h to obtain a high-rust-resistance high-saturation inductance material; wherein the drying temperature is 30-90 ℃;
the high Bs material is one or a mixture of at least two of Fe powder, FeSi powder, FeNi powder, Fe-based amorphous powder and Ni-based amorphous powder.
2. The method for preparing a high-antirust high-saturation inductance material according to claim 1, wherein the hydroxide is: at least one of sodium hydroxide, aluminum hydroxide, potassium hydroxide, magnesium hydroxide, barium hydroxide, lithium hydroxide, strontium hydroxide, calcium hydroxide, and manganese hydroxide.
3. The method for preparing a high-antirust high-saturation inductance material according to claim 1, wherein the raw material alloy is firstly drawn into a metal wire with a diameter of 0.1mm-5mm, and then is added into a plasma spheroidizing device, so that the raw material alloy is turned into initial spherical powder of 15um-55um through plasma spheroidization.
4. The method for preparing a highly antirust and highly saturated inductance material according to claim 1, wherein in step S3, the softened spherical powder is mixed with the high Bs material by a mixer at high speed, and the rotation speed of the paddle is greater than 1000 rpm.
5. The method for preparing a high-antirust high-saturation inductance material according to claim 1, wherein the reducing atmosphere contains hydrogen and/or carbon monoxide and/or ammonia.
6. A high-rust-prevention high-saturation inductance material, which is characterized by being prepared by the preparation method of the high-rust-prevention high-saturation inductance material according to any one of claims 1 to 5.
7. An integrally formed inductor, characterized in that the high antirust and high saturated inductor material as claimed in claim 6 is formed in a mold under a pressure of 400MPa to 600 MPa.
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