CN116013678B - Preparation method of low-loss ferrosilicon magnetic powder core material - Google Patents
Preparation method of low-loss ferrosilicon magnetic powder core material Download PDFInfo
- Publication number
- CN116013678B CN116013678B CN202310191231.4A CN202310191231A CN116013678B CN 116013678 B CN116013678 B CN 116013678B CN 202310191231 A CN202310191231 A CN 202310191231A CN 116013678 B CN116013678 B CN 116013678B
- Authority
- CN
- China
- Prior art keywords
- alloy
- treatment
- magnetic
- ferrosilicon
- loss
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a preparation method of a low-loss ferrosilicon magnetic powder core material, and belongs to the technical field of magnetic materials. Firstly, the invention adopts the ferrosilicon alloy with silicon content of 6.3-7.0% as raw material, alloy powder prepared by an air atomization method, and then alkaline silica sol and polymethylphenylsiloxane are used for forming insulating coating liquid, and the obtained ferrosilicon magnetic powder core is subjected to gradient concentration treatment from low concentration, medium concentration to high concentration, so that the obtained ferrosilicon magnetic powder core has excellent physical property and magnetic property, the insulating layer is effectively coated, the magnetic loss of the magnetic powder core is greatly reduced, and the whole process is chromium-free and phosphorus-free, green and environment-friendly and has extremely high market application value.
Description
Technical Field
The invention belongs to the technical field of magnetic materials, and particularly relates to a preparation method of a low-loss ferrosilicon magnetic powder core material.
Background
As is well known, magnetic materials are widely used in various fields because various electronic components realized by the magnetic materials have characteristics of converting, transmitting, processing information, storing energy and the like.
In order to accommodate the high frequency and high power of electronic products, the magnetic element is required to be light, thin and small. The silicon steel sheet and the iron powder core which are widely applied are difficult to meet the high-frequency application field due to the obvious eddy current effect. Soft magnetic ferrites, although having good high frequency application characteristics, have difficulty in meeting the application requirements of high power devices due to their relatively low magnetic flux density. The metal magnetic powder core can simultaneously realize the characteristics of high magnetic flux density, high resistivity, high magnetic permeability, low magnetostriction and the like through material composition and process design, and can meet the magnetic performance requirement of the magnetic element in a high frequency band. Therefore, research and development of the metal magnetic powder core with high frequency and low loss greatly promotes the development of the magnetic element to a high-power and miniaturized direction. The metal magnetic powder core is being widely applied in the fields of electronic products, household appliances, new energy sources and the like, and the production technology development and application research of the metal magnetic powder core are widely focused on related industries at home and abroad.
The ferrosilicon magnetic powder core has high saturation magnetic induction intensity, excellent direct current superposition characteristic and relatively low cost, and has become an application and research hot spot in the field of soft magnetic materials.
The magnetic powder core manufactured by adopting the iron-silicon soft magnetic alloy can reach 200 ℃, the heat aging problem of the magnetic core during high-temperature operation is avoided, and meanwhile, the performance characteristics of the magnetic powder core are just filled between the iron powder core and other three alloy magnetic powder cores (high magnetic flux, iron-silicon-aluminum, iron-nickel-molybdenum) by the characteristics of high cost performance, excellent direct current superposition characteristics, high frequency low loss characteristics and the like. Compared with the iron powder core, the iron silicon magnetic powder has the advantages of no aging and low power loss; compared with the iron silicon aluminum magnetic powder core, the iron silicon magnetic powder core has direct current superposition characteristics and lower price; compared with the iron-nickel magnetic powder core, the direct current superposition characteristics of the iron-nickel magnetic powder core and the iron-nickel magnetic powder core are equivalent, the loss is slightly higher than that of the iron-nickel magnetic powder core, but the cost of the iron-nickel magnetic powder core is far lower than that of the iron-nickel magnetic powder core because nickel is a noble metal and is high in price. Therefore, the alloy magnetic powder prepared from the ferrosilicon alloy material has wide application field and is widely focused in the industry.
For example, chinese patent CN201110235372.9 discloses a method for manufacturing iron-silicon material and mu 26 iron-silicon magnetic powder core, which comprises the steps of alloy smelting, powder preparation, powder reduction, powder classification, particle size proportioning, powder passivation, insulating coating, compression molding, heat treatment and surface coating, wherein small amounts of V and Nb elements are added during the alloy smelting process, so that the magnetic properties of the iron-silicon alloy are improved. Chinese patent CN201811236795.0 discloses a ferrosilicon magnetic powder core material and a preparation method thereof, wherein the composite material comprises iron powder, a small amount of silicon powder and superfine Fe 3 O 4 Mn-Zn ferrite particles and a proper binder are uniformly mixed, a novel powder metallurgy technology is adopted to prepare an annular material, and the binder is removed and then annealed and sintered at a high temperature to obtain the high-density and high-performance soft magnetic material.
However, in the prior art, the obtained ferrosilicon magnetic powder core has the problems of unstable magnetic performance and higher magnetic loss, so that the further improvement of the direct current superposition performance of the ferrosilicon magnetic powder core and the reduction of the loss are key and difficult to improve the application characteristics of the ferrosilicon magnetic powder core.
Disclosure of Invention
Aiming at the problems in the prior art, the invention discloses a preparation method of a low-loss ferrosilicon magnetic powder core material, and the obtained magnetic powder core material has good magnetic performance and low loss, and the comprehensive performance of the ferrosilicon magnetic powder core is greatly improved.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the preparation method of the low-loss ferrosilicon magnetic powder core material comprises the following steps:
(1) Smelting alloy: the ferrosilicon alloy is carried out in a magnesia crucible open type medium frequency induction furnace, the smelting temperature is above 1400 ℃, and the alloy melting time is above 50 min;
(2) Pulverizing by aerosol method: after the alloy is smelted, carrying out nitrogen spraying, crushing and pulverizing, carrying out annealing treatment, and reducing by using hydrogen after the treatment is finished to obtain alloy powder;
(3) Grading and screening proportion: sieving and mixing the alloy powder obtained in the step (2) according to the granularity ratio to obtain mixed alloy powder;
(4) Surface pretreatment: soaking the mixed alloy powder obtained in the step (3) in a passivation solution with the mass concentration of 0.3-0.5% for 10-20min, and drying at 180-200 ℃ after the soaking is completed, so as to finish surface pretreatment;
(5) Insulating coating: placing the alloy powder obtained in the step (4) into coating solutions with different concentrations for gradient concentration soaking treatment;
(6) And (3) lubrication treatment: adding zinc stearate with the mass of 0.5-0.7% into the powder obtained in the step (5), and uniformly mixing to obtain mixed magnetic powder;
(7) And (5) press forming: pressing the mixed magnetic powder obtained in the step (6) into a magnetic ring;
(8) And (3) heat treatment: and (3) performing heat treatment on the magnetic ring in a vacuum heat treatment furnace, adopting argon as a protective atmosphere, and then cooling to room temperature along with the furnace to obtain a finished product.
Preferably, in the ferrosilicon alloy in the step (1), silicon accounts for 6.3-7.0% by mass, and the balance is iron.
Preferably, the powder classification of step (3) is mixed according to the following mass ratio: 100-200 mesh: 200-400 mesh: 400-500 mesh = 1:3:2.
Preferably, the passivation solution in the step (4) is hydrogen peroxide.
Preferably, the effective components of the coating liquid in the step (5) are nano silica sol and polymethylphenylsiloxane, and the mass ratio of the nano silica sol to the polymethylphenylsiloxane is 1:1.
More preferably, the average particle size of the nano silica sol is less than or equal to 20nm, and the pH value is 9-11.
Preferably, the gradient concentration soaking treatment method in the step (5) comprises the following steps:
(1) Preparing a coating liquid: mixing nano silica sol and polymethylphenylsiloxane according to a mass ratio of 1:1, and dispersing the mixture in distilled water to prepare coating solutions with the mass concentration of 9-10%, 19-20% and 29-30% of the nano silica sol respectively;
(2) Gradient concentration soaking treatment: and then the alloy powder subjected to surface treatment is sequentially soaked in coating liquid with the mass concentration of 9-10%, 19-20% and 29-30% of nano silica sol for 1h respectively, and then dried at 80-85 ℃ to finish the treatment.
Preferably, the heat treatment temperature in the step (8) is 500-600 ℃, and the treatment time is 30-40min.
Advantageous effects
Firstly, the invention adopts the ferrosilicon alloy with silicon content of 6.3-7.0% as raw material, the alloy powder prepared by the gas atomization method has regular spherical particle morphology, the particles with designed particle size range can be obtained by sieving, and the particle size and the distribution of the powder can be effectively controlled;
secondly, spherical alloy particles are more beneficial to the coating of subsequent insulating layers, the insulating coating liquid is composed of alkaline silica sol and polymethylphenylsiloxane, and through the gradient concentration treatment from low concentration to medium concentration to high concentration, a compact, uniform and continuous insulating layer is gradually formed on the surface of the alloy, and the surface resistivity of the particles is favorably increased, so that the purpose of reducing the eddy current loss of the magnetic powder core is achieved. Compared with a single-component coating liquid, the mixed coating liquid of the silica sol and the polymethylphenylsiloxane has relatively good film forming property, on one hand, the nano-scale silica sol can promote the uniform dispersion and encapsulation of the polymethylphenylsiloxane, on the other hand, the silica sol and the polymethylphenylsiloxane can be uniformly and continuously encapsulated on the surfaces of particles by the treatment of the silica sol from low to high, the particles grow uniformly step by step, a compact and uniform insulating layer is formed on the surfaces of the particles, the surface resistivity of the particles is increased by the stable and uniform insulating layer, and the eddy current loss of the magnetic powder core is greatly reduced.
In conclusion, the ferrosilicon magnetic powder core obtained by the preparation method has higher quality factor and excellent direct current superposition characteristic, has excellent physical property and magnetic property, effectively wraps an insulating layer, greatly reduces the magnetic loss of the magnetic powder core, has no chromium and no phosphorus in the whole process, is environment-friendly, and has extremely high market application value.
Drawings
FIG. 1 is a microscopic morphology electron microscope image of the powder of example 3 and comparative examples 1-3 of the present invention after insulation coating.
Detailed Description
The technical scheme of the present invention is further described below with reference to specific examples, but is not limited thereto.
Example 1
The preparation method of the low-loss ferrosilicon magnetic powder core material comprises the following steps:
(1) Smelting alloy: the ferrosilicon alloy is carried out in a magnesia crucible open type medium frequency induction furnace, the smelting temperature is above 1400 ℃, and the alloy melting time is above 50 min;
(2) Pulverizing by aerosol method: after the alloy is smelted, carrying out nitrogen spraying, crushing and pulverizing, carrying out annealing treatment, and reducing by using hydrogen after the treatment is finished to obtain alloy powder;
(3) Grading and screening proportion: sieving and mixing the alloy powder obtained in the step (2) according to the granularity ratio to obtain mixed alloy powder;
(4) Surface pretreatment: soaking the mixed alloy powder obtained in the step (3) in a passivation solution with the mass concentration of 0.3% for 10min, and drying at 180-200 ℃ after the soaking is completed, so as to finish surface pretreatment;
(5) Insulating coating: placing the alloy powder obtained in the step (4) into coating solutions with different concentrations for gradient concentration soaking treatment;
(6) And (3) lubrication treatment: adding zinc stearate with the mass of 0.5% of the powder mass into the powder obtained in the step (5), and uniformly mixing to obtain mixed magnetic powder;
(7) And (5) press forming: pressing the mixed magnetic powder obtained in the step (6) into a magnetic ring;
(8) And (3) heat treatment: and (3) performing heat treatment on the magnetic ring in a vacuum heat treatment furnace, adopting argon as a protective atmosphere, and then cooling to room temperature along with the furnace to obtain a finished product.
In the ferrosilicon alloy in the step (1), silicon accounts for 6.3 mass percent, and the balance is iron.
The powder grading in the step (3) is mixed according to the following mass ratio: 100-200 mesh: 200-400 mesh: 400-500 mesh = 1:3:2.
And (4) the passivation solution in the step (4) is hydrogen peroxide.
The effective components of the coating liquid in the step (5) are nano silica sol and polymethylphenylsiloxane, and the mass ratio of the nano silica sol to the polymethylphenylsiloxane is 1:1.
The average grain diameter of the nano silica sol is less than or equal to 20nm, and the pH value is 9-11.
The gradient concentration soaking treatment method in the step (5) comprises the following steps:
(1) Preparing a coating liquid: mixing nano silica sol and polymethylphenylsiloxane according to a mass ratio of 1:1, and dispersing the mixture in distilled water to prepare coating solutions with the mass concentration of 9-10%, 19-20% and 29-30% of the nano silica sol respectively;
(2) Gradient concentration soaking treatment: and then the alloy powder subjected to surface treatment is sequentially soaked in coating liquid with the mass concentration of 9-10%, 19-20% and 29-30% of nano silica sol for 1h respectively, and then dried at 80-85 ℃ to finish the treatment.
The heat treatment temperature in the step (8) is 500-600 ℃ and the treatment time is 30min.
Example 2
The preparation method of the low-loss ferrosilicon magnetic powder core material comprises the following steps:
(1) Smelting alloy: the ferrosilicon alloy is carried out in a magnesia crucible open type medium frequency induction furnace, the smelting temperature is above 1400 ℃, and the alloy melting time is above 50 min;
(2) Pulverizing by aerosol method: after the alloy is smelted, carrying out nitrogen spraying, crushing and pulverizing, carrying out annealing treatment, and reducing by using hydrogen after the treatment is finished to obtain alloy powder;
(3) Grading and screening proportion: sieving and mixing the alloy powder obtained in the step (2) according to the granularity ratio to obtain mixed alloy powder;
(4) Surface pretreatment: soaking the mixed alloy powder obtained in the step (3) in a passivation solution with the mass concentration of 0.4% for 15min, and drying at 180-200 ℃ after the soaking is completed, so as to complete surface pretreatment;
(5) Insulating coating: placing the alloy powder obtained in the step (4) into coating solutions with different concentrations for gradient concentration soaking treatment;
(6) And (3) lubrication treatment: adding zinc stearate with the mass of 0.6% of the powder mass into the powder obtained in the step (5), and uniformly mixing to obtain mixed magnetic powder;
(7) And (5) press forming: pressing the mixed magnetic powder obtained in the step (6) into a magnetic ring;
(8) And (3) heat treatment: and (3) performing heat treatment on the magnetic ring in a vacuum heat treatment furnace, adopting argon as a protective atmosphere, and then cooling to room temperature along with the furnace to obtain a finished product.
In the ferrosilicon alloy in the step (1), silicon accounts for 6.3 mass percent, and the balance is iron.
The powder grading in the step (3) is mixed according to the following mass ratio: 100-200 mesh: 200-400 mesh: 400-500 mesh = 1:3:2.
And (4) the passivation solution in the step (4) is hydrogen peroxide.
The effective components of the coating liquid in the step (5) are nano silica sol and polymethylphenylsiloxane, and the mass ratio of the nano silica sol to the polymethylphenylsiloxane is 1:1.
The average grain diameter of the nano silica sol is less than or equal to 20nm, and the pH value is 9-11.
The gradient concentration soaking treatment method in the step (5) comprises the following steps:
(1) Preparing a coating liquid: mixing nano silica sol and polymethylphenylsiloxane according to a mass ratio of 1:1, and dispersing the mixture in distilled water to prepare coating solutions with the mass concentration of 9-10%, 19-20% and 29-30% of the nano silica sol respectively;
(2) Gradient concentration soaking treatment: and then the alloy powder subjected to surface treatment is sequentially soaked in coating liquid with the mass concentration of 9-10%, 19-20% and 29-30% of nano silica sol for 1h respectively, and then dried at 80-85 ℃ to finish the treatment.
The heat treatment temperature in the step (8) is 500-600 ℃ and the treatment time is 40min.
Example 3
The preparation method of the low-loss ferrosilicon magnetic powder core material comprises the following steps:
(1) Smelting alloy: the ferrosilicon alloy is carried out in a magnesia crucible open type medium frequency induction furnace, the smelting temperature is above 1400 ℃, and the alloy melting time is above 50 min;
(2) Pulverizing by aerosol method: after the alloy is smelted, carrying out nitrogen spraying, crushing and pulverizing, carrying out annealing treatment, and reducing by using hydrogen after the treatment is finished to obtain alloy powder;
(3) Grading and screening proportion: sieving and mixing the alloy powder obtained in the step (2) according to the granularity ratio to obtain mixed alloy powder;
(4) Surface pretreatment: soaking the mixed alloy powder obtained in the step (3) in a passivation solution with the mass concentration of 0.5% for 20min, and drying at 180-200 ℃ after the soaking is completed, so as to complete surface pretreatment;
(5) Insulating coating: placing the alloy powder obtained in the step (4) into coating solutions with different concentrations for gradient concentration soaking treatment;
(6) And (3) lubrication treatment: adding zinc stearate with the mass of 0.7% of the powder into the powder obtained in the step (5), and uniformly mixing to obtain mixed magnetic powder;
(7) And (5) press forming: pressing the mixed magnetic powder obtained in the step (6) into a magnetic ring;
(8) And (3) heat treatment: and (3) performing heat treatment on the magnetic ring in a vacuum heat treatment furnace, adopting argon as a protective atmosphere, and then cooling to room temperature along with the furnace to obtain a finished product.
In the ferrosilicon alloy in the step (1), silicon accounts for 6.3 mass percent, and the balance is iron.
The powder grading in the step (3) is mixed according to the following mass ratio: 100-200 mesh: 200-400 mesh: 400-500 mesh = 1:3:2.
And (4) the passivation solution in the step (4) is hydrogen peroxide.
The effective components of the coating liquid in the step (5) are nano silica sol and polymethylphenylsiloxane, and the mass ratio of the nano silica sol to the polymethylphenylsiloxane is 1:1.
The average grain diameter of the nano silica sol is less than or equal to 20nm, and the pH value is 9-11.
The gradient concentration soaking treatment method in the step (5) comprises the following steps:
(1) Preparing a coating liquid: mixing nano silica sol and polymethylphenylsiloxane according to a mass ratio of 1:1, and dispersing the mixture in distilled water to prepare coating solutions with the mass concentration of 9-10%, 19-20% and 29-30% of the nano silica sol respectively;
(2) Gradient concentration soaking treatment: and then the alloy powder subjected to surface treatment is sequentially soaked in coating liquid with the mass concentration of 9-10%, 19-20% and 29-30% of nano silica sol for 1h respectively, and then dried at 80-85 ℃ to finish the treatment.
The heat treatment temperature in the step (8) is 500-600 ℃ and the treatment time is 40min.
Comparative example 1
The preparation method of the low-loss ferrosilicon magnetic powder core material comprises the following steps:
(1) Smelting alloy: the ferrosilicon alloy is carried out in a magnesia crucible open type medium frequency induction furnace, the smelting temperature is above 1400 ℃, and the alloy melting time is above 50 min;
(2) Pulverizing by aerosol method: after the alloy is smelted, carrying out nitrogen spraying, crushing and pulverizing, carrying out annealing treatment, and reducing by using hydrogen after the treatment is finished to obtain alloy powder;
(3) Grading and screening proportion: sieving and mixing the alloy powder obtained in the step (2) according to the granularity ratio to obtain mixed alloy powder;
(4) Surface pretreatment: soaking the mixed alloy powder obtained in the step (3) in a passivation solution with the mass concentration of 0.5% for 20min, and drying at 180-200 ℃ after the soaking is completed, so as to complete surface pretreatment;
(5) Insulating coating: placing the alloy powder obtained in the step (4) into a coating liquid for soaking treatment;
(6) And (3) lubrication treatment: adding zinc stearate with the mass of 0.7% of the powder into the powder obtained in the step (5), and uniformly mixing to obtain mixed magnetic powder;
(7) And (5) press forming: pressing the mixed magnetic powder obtained in the step (6) into a magnetic ring;
(8) And (3) heat treatment: and (3) performing heat treatment on the magnetic ring in a vacuum heat treatment furnace, adopting argon as a protective atmosphere, and then cooling to room temperature along with the furnace to obtain a finished product.
In the ferrosilicon alloy in the step (1), silicon accounts for 6.3 mass percent, and the balance is iron.
The powder grading in the step (3) is mixed according to the following mass ratio: 100-200 mesh: 200-400 mesh: 400-500 mesh = 1:3:2.
And (4) the passivation solution in the step (4) is hydrogen peroxide.
The effective components of the coating liquid in the step (5) are nano silica sol and polymethylphenylsiloxane, and the mass ratio of the nano silica sol to the polymethylphenylsiloxane is 1:1.
The average grain diameter of the nano silica sol is less than or equal to 20nm, and the pH value is 9-11.
The method for soaking the coating liquid in the step (5) comprises the following steps:
(1) Mixing nano silica sol and polymethylphenylsiloxane according to a mass ratio of 1:1, and dispersing the mixture in distilled water to respectively prepare coating liquid with the mass concentration of 9-10% of the nano silica sol;
(2) Then the alloy powder after surface treatment is soaked in coating liquid with the mass concentration of 9-10% of nano silica sol for 3 hours, and then dried in the environment of 80-85 ℃ to finish the treatment.
The heat treatment temperature in the step (8) is 500-600 ℃ and the treatment time is 40min.
In this comparative example, the raw materials and the process steps were the same as in example 3 except that only the coating liquid having a nano silica sol mass concentration of 9 to 10% was immersed in the insulating coating treatment.
Comparative example 2
The preparation method of the low-loss ferrosilicon magnetic powder core material comprises the following steps:
(1) Smelting alloy: the ferrosilicon alloy is carried out in a magnesia crucible open type medium frequency induction furnace, the smelting temperature is above 1400 ℃, and the alloy melting time is above 50 min;
(2) Pulverizing by aerosol method: after the alloy is smelted, carrying out nitrogen spraying, crushing and pulverizing, carrying out annealing treatment, and reducing by using hydrogen after the treatment is finished to obtain alloy powder;
(3) Grading and screening proportion: sieving and mixing the alloy powder obtained in the step (2) according to the granularity ratio to obtain mixed alloy powder;
(4) Surface pretreatment: soaking the mixed alloy powder obtained in the step (3) in a passivation solution with the mass concentration of 0.5% for 20min, and drying at 180-200 ℃ after the soaking is completed, so as to complete surface pretreatment;
(5) Insulating coating: placing the alloy powder obtained in the step (4) into a coating liquid for soaking treatment;
(6) And (3) lubrication treatment: adding zinc stearate with the mass of 0.7% of the powder into the powder obtained in the step (5), and uniformly mixing to obtain mixed magnetic powder;
(7) And (5) press forming: pressing the mixed magnetic powder obtained in the step (6) into a magnetic ring;
(8) And (3) heat treatment: and (3) performing heat treatment on the magnetic ring in a vacuum heat treatment furnace, adopting argon as a protective atmosphere, and then cooling to room temperature along with the furnace to obtain a finished product.
In the ferrosilicon alloy in the step (1), silicon accounts for 6.3 mass percent, and the balance is iron.
The powder grading in the step (3) is mixed according to the following mass ratio: 100-200 mesh: 200-400 mesh: 400-500 mesh = 1:3:2.
And (4) the passivation solution in the step (4) is hydrogen peroxide.
The effective components of the coating liquid in the step (5) are nano silica sol and polymethylphenylsiloxane, and the mass ratio of the nano silica sol to the polymethylphenylsiloxane is 1:1.
The average grain diameter of the nano silica sol is less than or equal to 20nm, and the pH value is 9-11.
The method for soaking the coating liquid in the step (5) comprises the following steps:
(1) Mixing nano silica sol and polymethylphenylsiloxane according to a mass ratio of 1:1, and dispersing the mixture in distilled water to respectively prepare coating liquid with the mass concentration of 9-10% of the nano silica sol;
(2) Then the alloy powder after surface treatment is soaked in coating liquid with the mass concentration of 19-20% of nano silica sol for 3 hours, and then dried in the environment of 80-85 ℃ to finish the treatment.
The heat treatment temperature in the step (8) is 500-600 ℃ and the treatment time is 40min.
In this comparative example, the raw materials and the process steps were the same as in example 3 except that only the coating liquid having a nano silica sol mass concentration of 19 to 20% was immersed in the insulating coating treatment.
Comparative example 3
The preparation method of the low-loss ferrosilicon magnetic powder core material comprises the following steps:
(1) Smelting alloy: the ferrosilicon alloy is carried out in a magnesia crucible open type medium frequency induction furnace, the smelting temperature is above 1400 ℃, and the alloy melting time is above 50 min;
(2) Pulverizing by aerosol method: after the alloy is smelted, carrying out nitrogen spraying, crushing and pulverizing, carrying out annealing treatment, and reducing by using hydrogen after the treatment is finished to obtain alloy powder;
(3) Grading and screening proportion: sieving and mixing the alloy powder obtained in the step (2) according to the granularity ratio to obtain mixed alloy powder;
(4) Surface pretreatment: soaking the mixed alloy powder obtained in the step (3) in a passivation solution with the mass concentration of 0.5% for 20min, and drying at 180-200 ℃ after the soaking is completed, so as to complete surface pretreatment;
(5) Insulating coating: placing the alloy powder obtained in the step (4) into a coating liquid for soaking treatment;
(6) And (3) lubrication treatment: adding zinc stearate with the mass of 0.7% of the powder into the powder obtained in the step (5), and uniformly mixing to obtain mixed magnetic powder;
(7) And (5) press forming: pressing the mixed magnetic powder obtained in the step (6) into a magnetic ring;
(8) And (3) heat treatment: and (3) performing heat treatment on the magnetic ring in a vacuum heat treatment furnace, adopting argon as a protective atmosphere, and then cooling to room temperature along with the furnace to obtain a finished product.
In the ferrosilicon alloy in the step (1), silicon accounts for 6.3 mass percent, and the balance is iron.
The powder grading in the step (3) is mixed according to the following mass ratio: 100-200 mesh: 200-400 mesh: 400-500 mesh = 1:3:2.
And (4) the passivation solution in the step (4) is hydrogen peroxide.
The effective components of the coating liquid in the step (5) are nano silica sol and polymethylphenylsiloxane, and the mass ratio of the nano silica sol to the polymethylphenylsiloxane is 1:1.
The average grain diameter of the nano silica sol is less than or equal to 20nm, and the pH value is 9-11.
The method for soaking the coating liquid in the step (5) comprises the following steps:
(1) Mixing nano silica sol and polymethylphenylsiloxane according to a mass ratio of 1:1, and dispersing the mixture in distilled water to respectively prepare coating liquid with the mass concentration of 9-10% of the nano silica sol;
(2) Then the alloy powder after surface treatment is soaked in coating liquid with the mass concentration of 29-30% of nano silica sol for 3 hours, and then dried in the environment of 80-85 ℃ to finish the treatment.
The heat treatment temperature in the step (8) is 500-600 ℃ and the treatment time is 40min.
In this comparative example, the raw materials and the process steps were the same as in example 3 except that only the coating liquid having a nano silica sol mass concentration of 29 to 30% was immersed in the insulating coating treatment.
Performance testing
Performance test reference standards of GB/T3658-2008 annular test method for measuring alternating current magnetic performance of soft magnetic material, GB/T13012-2008 method for measuring direct current magnetic performance of soft magnetic material, SJ20966-2006 method for measuring soft magnetic ferrite material and GB/T6525-2019 method for measuring room temperature compression strength of sintered metal material are adopted to observe the morphology of soft magnetic powder by adopting a Japanese JSM-6490LV electron microscope.
TABLE 1 Performance test results
It should be noted that the above-mentioned embodiments are merely some, but not all embodiments of the preferred mode of carrying out the invention. It is evident that all other embodiments obtained by a person skilled in the art without making any inventive effort, based on the above-described embodiments of the invention, shall fall within the scope of protection of the invention.
Claims (7)
1. The preparation method of the low-loss ferrosilicon magnetic powder core material is characterized by comprising the following steps of:
(1) Smelting alloy: the ferrosilicon alloy is carried out in a magnesia crucible open type medium frequency induction furnace, the smelting temperature is above 1400 ℃, and the alloy melting time is above 50 min;
(2) Pulverizing by aerosol method: after the alloy is smelted, carrying out nitrogen spraying, crushing and pulverizing, carrying out annealing treatment, and reducing by using hydrogen after the treatment is finished to obtain alloy powder;
(3) Grading and screening proportion: sieving and mixing the alloy powder obtained in the step (2) according to the granularity ratio to obtain mixed alloy powder;
(4) Surface pretreatment: soaking the mixed alloy powder obtained in the step (3) in a passivation solution with the mass concentration of 0.3-0.5% for 10-20min, and drying at 180-200 ℃ after the soaking is completed, so as to finish surface pretreatment;
(5) Insulating coating: placing the alloy powder obtained in the step (4) into coating solutions with different concentrations for gradient concentration soaking treatment;
(6) And (3) lubrication treatment: adding zinc stearate with the mass of 0.5-0.7% into the powder obtained in the step (5), and uniformly mixing to obtain mixed magnetic powder;
(7) And (5) press forming: pressing the mixed magnetic powder obtained in the step (6) into a magnetic ring;
(8) And (3) heat treatment: performing heat treatment on the magnetic ring in a vacuum heat treatment furnace, adopting argon as a protective atmosphere, and then cooling to room temperature along with the furnace to obtain a finished product;
the gradient concentration soaking treatment method in the step (5) comprises the following steps:
(1) Preparing a coating liquid: mixing nano silica sol and polymethylphenylsiloxane according to a mass ratio of 1:1, and dispersing the mixture in distilled water to prepare coating solutions with the mass concentration of 9-10%, 19-20% and 29-30% of the nano silica sol respectively;
(2) Gradient concentration soaking treatment: and then the alloy powder subjected to surface treatment is sequentially soaked in coating liquid with the mass concentration of 9-10%, 19-20% and 29-30% of nano silica sol for 1h respectively, and then dried at 80-85 ℃ to finish the treatment.
2. The method of producing a low-loss ferrosilicon magnetic powder core material according to claim 1, wherein in the ferrosilicon alloy of step (1), silicon is 6.3 to 7.0% by mass, and the balance is iron.
3. A method for producing a low-loss ferromagnetic powder core material according to claim 1, wherein the powder classification in step (3) is mixed in the following mass ratio: 100-200 mesh: 200-400 mesh: 400-500 mesh = 1:3:2.
4. The method for preparing a low-loss ferromagnetic powder core material according to claim 1, wherein the passivation solution in step (4) is hydrogen peroxide.
5. The method for preparing a low-loss ferrosilicon magnetic powder core material according to claim 1, wherein the effective components of the coating liquid in the step (5) are nano silica sol and polymethylphenylsiloxane, and the mass ratio of the nano silica sol to the polymethylphenylsiloxane is 1:1.
6. A method for preparing a low-loss ferromagnetic powder core material according to claim 5, wherein said nanosilicon sol has an average particle size of 20nm or less and a ph of 9-11.
7. A method for producing a low-loss ferromagnetic powder core material according to claim 1, wherein the heat treatment temperature in step (8) is 500-600 ℃ and the treatment time is 30-40min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310191231.4A CN116013678B (en) | 2023-03-02 | 2023-03-02 | Preparation method of low-loss ferrosilicon magnetic powder core material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310191231.4A CN116013678B (en) | 2023-03-02 | 2023-03-02 | Preparation method of low-loss ferrosilicon magnetic powder core material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116013678A CN116013678A (en) | 2023-04-25 |
| CN116013678B true CN116013678B (en) | 2023-10-17 |
Family
ID=86025036
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310191231.4A Active CN116013678B (en) | 2023-03-02 | 2023-03-02 | Preparation method of low-loss ferrosilicon magnetic powder core material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116013678B (en) |
Citations (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2545640A1 (en) * | 1983-05-05 | 1984-11-09 | Gen Electric | MAGNETIC CORE IN IRON POWDER |
| RU2043375C1 (en) * | 1992-11-23 | 1995-09-10 | Институт горного дела им.А.А.Скочинского | Silicate dye |
| JPH09125111A (en) * | 1995-10-30 | 1997-05-13 | Tokin Corp | Magnetic material powder and magnetic material formed by using the same |
| JP2003282317A (en) * | 2002-03-25 | 2003-10-03 | Nec Tokin Corp | Alloy powder surface treatment method and dust core |
| DE102006018530A1 (en) * | 2006-04-21 | 2007-10-25 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Stabilizer for sedimentation inhibition in dispersions |
| CN102294476A (en) * | 2011-08-17 | 2011-12-28 | 天通控股股份有限公司 | Ferrosilicon material and mu75 ferrosilicon magnetic powder core manufacturing method |
| CN102294475A (en) * | 2011-08-17 | 2011-12-28 | 天通控股股份有限公司 | Ferrosilicon material and mu60 ferrosilicon magnetic powder core manufacturing method |
| CN102294474A (en) * | 2011-08-17 | 2011-12-28 | 天通控股股份有限公司 | Ferrosilicon material and mu50 ferrosilicon magnetic powder core manufacturing method |
| CN102303115A (en) * | 2011-08-17 | 2012-01-04 | 天通控股股份有限公司 | Manufacturing method of ferrum silicon material and mu26 ferrum silicon magnetic powder core |
| CN102436895A (en) * | 2011-12-19 | 2012-05-02 | 浙江大学 | Preparation method of iron-silicon-aluminum magnetic powder core |
| US8562878B1 (en) * | 2007-03-02 | 2013-10-22 | Sandia Corporation | Stress-tuned conductor-polymer composite for use in sensors |
| CN103567436A (en) * | 2013-11-28 | 2014-02-12 | 四川东阁科技有限公司 | Manufacturing method of iron-silicon material and iron-silicon magnetic powder core having permeability mu of 55 |
| CN103725074A (en) * | 2014-01-06 | 2014-04-16 | 武汉双虎涂料有限公司 | High-temperature-resisting heat-insulation coating as well as preparation method and application thereof |
| CN104867642A (en) * | 2015-05-20 | 2015-08-26 | 自贡兆强密封制品实业有限公司 | Preparation method for silicone-oil-based magnetic liquid |
| CN108329021A (en) * | 2017-12-25 | 2018-07-27 | 日照亿鑫电子材料有限公司 | Low-frequency current sensor core material and preparation method thereof |
| CN110922179A (en) * | 2019-12-06 | 2020-03-27 | 深圳信义磁性材料有限公司 | High-permeability low-loss ferrite material and preparation method thereof |
| CN112479699A (en) * | 2020-12-22 | 2021-03-12 | 深圳信义磁性材料有限公司 | Low-loss nano ferrite magnetic material and preparation method thereof |
| CN112530656A (en) * | 2020-12-22 | 2021-03-19 | 湖州浩通电子科技有限公司 | Preparation method of low-loss iron-silicon magnetic powder core |
| CN114105627A (en) * | 2021-12-24 | 2022-03-01 | 深圳信义磁性材料有限公司 | Wide-temperature low-loss ferrite and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101255252B1 (en) * | 2011-06-20 | 2013-04-16 | 고려대학교 산학협력단 | Mutifunctional colloid nano composite derived from nucleophilic substitution-induced layer-by-layer assembly in organic media and fabrication the same |
| US11535943B2 (en) * | 2016-10-31 | 2022-12-27 | Nippon Steel Corporation | Grain-oriented electrical steel sheet |
| EP3839093B1 (en) * | 2018-08-17 | 2024-07-31 | JFE Steel Corporation | Production method for treatment solution for forming insulating coating and production method for steel sheet having insulating coating |
-
2023
- 2023-03-02 CN CN202310191231.4A patent/CN116013678B/en active Active
Patent Citations (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2545640A1 (en) * | 1983-05-05 | 1984-11-09 | Gen Electric | MAGNETIC CORE IN IRON POWDER |
| RU2043375C1 (en) * | 1992-11-23 | 1995-09-10 | Институт горного дела им.А.А.Скочинского | Silicate dye |
| JPH09125111A (en) * | 1995-10-30 | 1997-05-13 | Tokin Corp | Magnetic material powder and magnetic material formed by using the same |
| JP2003282317A (en) * | 2002-03-25 | 2003-10-03 | Nec Tokin Corp | Alloy powder surface treatment method and dust core |
| DE102006018530A1 (en) * | 2006-04-21 | 2007-10-25 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Stabilizer for sedimentation inhibition in dispersions |
| US8562878B1 (en) * | 2007-03-02 | 2013-10-22 | Sandia Corporation | Stress-tuned conductor-polymer composite for use in sensors |
| CN102303115A (en) * | 2011-08-17 | 2012-01-04 | 天通控股股份有限公司 | Manufacturing method of ferrum silicon material and mu26 ferrum silicon magnetic powder core |
| CN102294474A (en) * | 2011-08-17 | 2011-12-28 | 天通控股股份有限公司 | Ferrosilicon material and mu50 ferrosilicon magnetic powder core manufacturing method |
| CN102294475A (en) * | 2011-08-17 | 2011-12-28 | 天通控股股份有限公司 | Ferrosilicon material and mu60 ferrosilicon magnetic powder core manufacturing method |
| CN102294476A (en) * | 2011-08-17 | 2011-12-28 | 天通控股股份有限公司 | Ferrosilicon material and mu75 ferrosilicon magnetic powder core manufacturing method |
| CN102436895A (en) * | 2011-12-19 | 2012-05-02 | 浙江大学 | Preparation method of iron-silicon-aluminum magnetic powder core |
| CN103567436A (en) * | 2013-11-28 | 2014-02-12 | 四川东阁科技有限公司 | Manufacturing method of iron-silicon material and iron-silicon magnetic powder core having permeability mu of 55 |
| CN103725074A (en) * | 2014-01-06 | 2014-04-16 | 武汉双虎涂料有限公司 | High-temperature-resisting heat-insulation coating as well as preparation method and application thereof |
| CN104867642A (en) * | 2015-05-20 | 2015-08-26 | 自贡兆强密封制品实业有限公司 | Preparation method for silicone-oil-based magnetic liquid |
| CN108329021A (en) * | 2017-12-25 | 2018-07-27 | 日照亿鑫电子材料有限公司 | Low-frequency current sensor core material and preparation method thereof |
| CN110922179A (en) * | 2019-12-06 | 2020-03-27 | 深圳信义磁性材料有限公司 | High-permeability low-loss ferrite material and preparation method thereof |
| CN112479699A (en) * | 2020-12-22 | 2021-03-12 | 深圳信义磁性材料有限公司 | Low-loss nano ferrite magnetic material and preparation method thereof |
| CN112530656A (en) * | 2020-12-22 | 2021-03-19 | 湖州浩通电子科技有限公司 | Preparation method of low-loss iron-silicon magnetic powder core |
| CN114105627A (en) * | 2021-12-24 | 2022-03-01 | 深圳信义磁性材料有限公司 | Wide-temperature low-loss ferrite and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 徐小军 ; 王鲜 ; 魏鼎 ; 李喜雄 ; 冯则坤 ; 龚荣洲.铁硅合金粉末的改性硅溶胶表面包覆及其磁粉芯性能.《磁性材料及器件》.2014,33-36. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116013678A (en) | 2023-04-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109285685B (en) | Preparation method of high-permeability gas-atomized Fe-Si-Al magnetic powder core | |
| CN106158340B (en) | A kind of Fe Si Al powder core toroidal magnets and preparation method thereof | |
| CN115101322A (en) | Preparation method of composite magnetic powder core | |
| CN117038244B (en) | Preparation method of insulating coated magnetic powder, soft magnetic powder core and preparation method thereof | |
| CN112530656A (en) | Preparation method of low-loss iron-silicon magnetic powder core | |
| CN110783091B (en) | Preparation method of nanocrystalline FeSiBCr magnetic powder core | |
| CN116612975A (en) | Preparation method of high-frequency low-loss iron-based soft magnetic composite material | |
| CN116013678B (en) | Preparation method of low-loss ferrosilicon magnetic powder core material | |
| CN113025927A (en) | Iron-based amorphous composite material and preparation method and application thereof | |
| CN104036903B (en) | A kind of preparation method of ferrum tantnickel powder core | |
| CN114496544B (en) | Manufacturing method of low-power consumption iron-nickel-molybdenum magnetic powder core | |
| CN115938782A (en) | Preparation method of high-performance Fe-Si-Al magnetic powder core | |
| CN113838658B (en) | Preparation method of ferrosilicon magnetic powder core | |
| CN116031037A (en) | Rare earth ion doped soft magnetic alloy, soft magnetic composite material and preparation method thereof | |
| CN113658769A (en) | High-frequency high-Q-value FeSiAl @ MnZn ferrite soft magnetic composite magnetic powder core and preparation method thereof | |
| CN114133231A (en) | Nickel-zinc ferrite material and method for producing same | |
| CN113658768A (en) | FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss and preparation method thereof | |
| CN109192430B (en) | Preparation method for improving high-frequency effective magnetic conductivity of metal soft magnetic powder core and product | |
| CN109513933B (en) | Preparation method of iron-based soft magnetic core with high temperature resistance and high surface resistance | |
| CN114156035B (en) | Aerosol sendust magnetic powder core and preparation method thereof | |
| CN111029124A (en) | Powder efficient coating method and finished product powder and finished product magnetic powder core preparation method | |
| CN116206840B (en) | Low-loss iron-nickel-molybdenum magnetic powder core and preparation method thereof | |
| CN113539663B (en) | Soft magnetic composite material and preparation method and application thereof | |
| CN116110673A (en) | Preparation process of ferrosilicon material and ferrosilicon magnetic powder core | |
| CN115064328A (en) | Low-power-consumption soft magnetic alloy material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |