Iron-silicon-aluminum-nickel soft magnetic powder core with effective magnetic conductivity of 60 and preparation method thereof
Technical Field
The invention belongs to the technical field of soft magnetic materials, and particularly relates to an iron-silicon-aluminum-nickel soft magnetic powder core with the effective magnetic conductivity of 60 and a preparation method thereof.
Background
The metal soft magnetic powder core is a composite soft magnetic material formed by mixing and pressing ferromagnetic powder and an insulating medium. Because the surface of the ferromagnetic powder particles is uniformly coated with a layer of insulating medium film, the magnetic powder core has high resistivity, so the eddy current loss is very low, and the ferromagnetic powder is suitable for higher frequency application (more than 20 kHz). In addition, the magnetic powder core also has the advantages of higher saturation magnetic induction intensity, good frequency characteristic, constant magnetic conductivity and the like, so that the magnetic powder core is widely applied to the fields of electronic communication, radars, power switches and the like as an inductive filter and a choke coil.
During world war II, Fe-Si-Al alloy magnetic powder cores are developed successively in Japan and Germany, and have higher cost performance while having excellent magnetism of Fe-Ni alloy powder cores. United states Union used Fe in 198478Si16B6The amorphous powder is used for preparing the amorphous magnetic powder core, and new vitality is injected for the development of the metal magnetic powder core. In recent years, with the development of nano technology, mechanical alloying and other technologies, the development of magnetic powder cores has a new research trend.
Patent CN104036903B discloses a method for preparing an iron-silicon-nickel soft magnetic powder core, which comprises performing insulation treatment on the surface of iron-silicon-nickel magnetic powder particles by using passivating agents such as phosphoric acid or chromic acid to form an insulating layer with high resistivity; the prepared finished product of the iron-silicon-nickel soft magnetic powder core has excellent saturation magnetic induction intensity which is as high as 1.5T under the condition that the magnetic field intensity is 500 Oe; the DC bias performance can reach 67.4% under the condition of 50Oe of the DC bias field strength. Patent CN103824670A discloses that a doped ferrosilicon raw powder is obtained by adding trace elements Ni or Co on the basis of ferrosilicon and adopting a gas atomization powder preparation method; preparing a ferrosilicon green body by using potassium permanganate as a passivating agent and phenolic resin and epoxy resin as binding agents; the iron-silicon green body is required to be insulated for 1 to 5 hours at the temperature of between 200 and 400 ℃ and 0.5 to 1 hour at the temperature of between 600 and 800 ℃ to obtain the iron-silicon annular powder core finished product with high direct current bias performance.
At present, the sendust core is widely applied by virtue of excellent cost performance and lower loss level, but compared with the iron-nickel core and the iron-silicon core, the direct current bias performance has a small difference. Therefore, a metal soft magnetic powder core with high direct current bias performance and low loss needs to be developed.
Disclosure of Invention
The invention aims to solve the technical problem of providing an iron-silicon-aluminum-nickel soft magnetic powder core with the effective magnetic conductivity of 60 and a preparation method thereof aiming at the technical current situation of the metal soft magnetic powder core.
Specifically, the invention discloses a preparation method of an iron-silicon-aluminum-nickel soft magnetic powder core with the effective magnetic conductivity of 60, which is characterized by comprising the following steps:
(1) selecting iron-silicon-aluminum-nickel magnetic powder: selecting iron-silicon-aluminum-nickel magnetic powder with the particle size of less than 200 meshes, wherein the alloy comprises 3.5-5.5% of Si, 2.0-4.5% of Al, 1.0-3.5% of Ni and the balance of Fe by mass percent;
(2) preparation of dry insulating coated powder: taking the mass of the Fe-Si-Al-Ni metal magnetic powder in the step (1) as a proportion reference, and adding 0.5-1.0% of epoxy resin and 0.5-1.2% of SiO2Powder, 0.7 to 2.0 percent of acetone and 8.0 to 15.0 percent of water; stirring uniformly at normal temperature to form uniform mixed slurry; then, heating to 100-140 ℃, and continuing to keep the temperature and stir; after the heat preservation is finished, sieving the dried insulating powder (screening out oversize particles) to obtain insulating coated powder;
(3) preparing magnetic powder to be molded: taking the mass of the Fe-Si-Al-Ni metal magnetic powder in the step (1) as a proportion reference, adding 0.3-0.9 mass percent of binder and 0.4-1.0 mass percent of release agent into the insulating coated powder in the step (2), and uniformly mixing to obtain the magnetic powder to be molded;
(4) and (3) pressing and forming: pressing the magnetic powder to be molded prepared in the step (3) into a powder core blank by using a press, wherein the pressing pressure of the press is 1900 MPa-2500 MPa;
(5) and (3) heat treatment: under the protection of inert gas, preserving the heat of the powder core blank pressed and formed in the step (4) at 800-900 ℃ to obtain a semi-finished product of the powder core;
(6) insulating spraying: and (5) spraying a layer of insulating and high-temperature-resistant epoxy resin coating on the surface of the semi-finished magnetic powder core in the step (5) to obtain a finished metal soft magnetic powder core.
Preferably, the stirring time in step (2) at normal temperature is 15 to 60 minutes, preferably 20 to 40 minutes.
Preferably, when the temperature in the step (2) is between 100 and 140 ℃, the stirring is continued for 15 to 60 minutes, preferably 15 to 35 minutes, under the heat preservation condition.
Preferably, the binder in step (3) is selected from one or more of silicone resin, phenolic resin and polyamide resin.
Preferably, the release agent in step (3) is selected from one or more of zinc stearate, calcium stearate, talcum powder and mica powder.
Preferably, the incubation time in step (5) is 30 to 120 minutes, preferably 60 to 100 minutes.
Preferably, the inert gas in step (5) is argon, nitrogen, or the like.
Preferably, the mass percentage of Si in the alloy can be selected from 3.5%, 4.0%, 4.5%, 5% and 5.5%; the mass percent of Al can be selected from 2.0%, 2.5%, 3.0%, 3.5%, 4.0% and 4.5%; the mass percentage of Ni can be selected from 1.0%, 1.5%, 2.0%, 2.5%, 3.0% and 3.5%.
Preferably, the mass percent of the epoxy resin can be selected from 0.5%, 0.6%, 0.7%, 0.8%, 0.9% and 1.0%; SiO 22The powder can be selected from 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.2% by weight.
Preferably, the mass percent of the acetone can be selected from 0.7 to 1.0 percent; the mass percentage of the water can be 10.0-12.0%.
Preferably, the mass percent of the binder can be selected from 0.5 to 0.7 percent.
Preferably, the mass percent of the release agent can be selected from 0.6 to 0.8 percent.
Preferably, the pressing pressure of the press is 2000MPa to 2200 MPa.
The invention also relates to the iron-silicon-aluminum-nickel soft magnetic powder core with the effective magnetic permeability of 60, which is prepared by any one of the methods.
More specifically, the powder core direct current bias performance of the iron-silicon-aluminum-nickel soft magnetic powder core under the condition of 100Oe is higher than 65%, and the volume loss Pcv under the conditions of 50kHz and 100mT is lower than 550mW/cm3And has excellent frequency stability.
The invention surprisingly discovers that the epoxy resin and SiO are regulated2The powder consumption can effectively improve the performance of the powder core, and the product performance is greatly influenced by adjusting the conditions of the pressing pressure and the like of the press in the step (4). In addition, the preparation method is simple and convenient, is easy to operate and control, does not adopt the traditional acid passivation process, and effectively avoids the harm of an acidic reagent to the environment.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a diagram illustrating the variation of DC bias performance of Fe-Si-Al-Ni soft magnetic powder core under the condition of 0 Oe-200 Oe in example 1 of the present invention;
FIG. 2 is a graph showing the effective permeability change of the Fe-Si-Al-Ni soft magnetic powder core under the condition of 20 Hz-2 MHz in example 1 of the present invention;
FIG. 3 is a diagram showing the variation of DC bias performance of the Fe-Si-Al-Ni soft magnetic powder core under the condition of 0 Oe-200 Oe in example 2 of the present invention;
FIG. 4 is a graph showing the effective permeability change of the Fe-Si-Al-Ni soft magnetic powder core under the condition of 20 Hz-2 MHz in example 2 of the present invention;
FIG. 5 is a diagram showing the variation of DC bias performance of the Fe-Si-Al-Ni soft magnetic powder core under the condition of 0 Oe-200 Oe in example 3 of the present invention;
FIG. 6 is a graph showing the effective permeability change of the Fe-Si-Al-Ni soft magnetic powder core under the condition of 20 Hz-2 MHz in example 3 of the present invention;
FIG. 7 is a diagram showing the variation of DC bias performance of the Fe-Si-Al-Ni soft magnetic powder core under the condition of 0 Oe-200 Oe in example 4 of the present invention;
FIG. 8 is a graph showing the effective permeability change of the Fe-Si-Al-Ni soft magnetic powder core under the condition of 20 Hz-2 MHz in example 4 of the present invention;
FIG. 9 is a diagram showing the variation of DC bias performance of the Fe-Si-Al-Ni soft magnetic powder core under the condition of 0 Oe-200 Oe in example 5 of the present invention;
FIG. 10 is a graph showing the effective permeability change of the Fe-Si-Al-Ni soft magnetic powder core under the condition of 20 Hz-2 MHz in example 5 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples. The described embodiments and their results are only intended to illustrate the invention and should not be taken as limiting the invention described in detail in the claims.
Example 1:
selecting alloy components with the particle size of-200 meshes, wherein the alloy components comprise, by mass, 4.0% of Si, 3.5% of Al, 2.0% of Ni and 1000.0g of Fe-Si-Al-Ni magnetic powder as the balance; 5.0g of epoxy resin and 11.5g of SiO were added2Stirring the powder, 10.0g of acetone and 90.0g of water at normal temperature for 20 minutes to form uniform mixed slurry; then, heating the mixed slurry to 100 ℃, preserving heat and stirring for 35 minutes, and after the heat preservation is finished, sieving the dried iron-silicon-aluminum-nickel insulating powder by using a 100-mesh sieve (sieving off oversize particles); adding 3.0g of adhesive siloxane resin powder and 4.0g of release agent zinc stearate into the sieved powder, and uniformly mixing to obtain magnetic powder to be molded; pressing the uniformly mixed magnetic powder to be molded into a powder core blank by adopting a pressing pressure of about 1900MPa, wherein the powder core blank is an annular powder core with the outer diameter of 33.02mm, the inner diameter of 19.94mm and the height of 10.67 mm; adopting nitrogen as protective gas, and keeping the pressed powder core blank at 800 ℃ for 60 minutes to obtain a semi-finished product of the magnetic powder core; and finally, spraying a layer of insulating and high-temperature-resistant epoxy resin coating on the surface of the semi-finished magnetic powder, and drying to obtain a finished metal soft magnetic powder core.
Winding a 32-turn inductance coil on the iron-silicon-aluminum-nickel metal soft magnetic powder core by adopting an enameled wire with the wire diameter phi of 1.12mm and the wire length of 0.9m, wherein the powder core obtained by measurement has the following magnetoelectric properties:
(1) under the condition of 100kHz/1V, the inductance L is 59.55 mu H;
(2) under the condition of 100kHz/1V, the quality factor Q is 72.71;
(3) direct current superposition performance under the condition of 100 kHz: when H is 100Oe, LH/L072.32%; when H is 200Oe, LH/L0=38.71%;
(4) Under the condition of 50kHz/100mT, the volume loss of the iron-silicon-aluminum-nickel soft magnetic powder core is as follows: pv is 501.19mW/cm3。
FIG. 1 is a diagram illustrating the DC bias performance variation of the Fe-Si-Al-Ni soft magnetic powder core in example 1 under the condition of 0 Oe-200 Oe; along with the increase of the direct current bias field intensity, the direct current bias performance of the powder core is gradually reduced; under the condition of 100Oe, the direct current bias performance of the iron-silicon-aluminum nickel powder core reaches 72.32 percent, and the direct current bias performance is excellent; fig. 2 is a graph showing the change of the effective permeability of the sendust core in example 1 under the condition of 20Hz to 2MHz, and as the test frequency increases, the effective permeability of the sendust core is always maintained at about 60, and no trend of decrease of the effective permeability with the increase of the frequency occurs, so that the sendust core has excellent frequency stability.
Example 2:
selecting commercially available alloy components with the particle size of-200 meshes, wherein the commercially available alloy components comprise, by mass, 4.0% of Si, 3.5% of Al, 2.0% of Ni and 1000.0g of Fe-Si-Al-Ni magnetic powder as the balance; 9.8g of epoxy resin and 5.1g of SiO were added2Stirring the powder, 10.0g of acetone and 90.0g of water at normal temperature for 20 minutes to form uniform mixed slurry; then, heating the mixed slurry to 140 ℃, preserving heat and stirring for 15 minutes, and after the heat preservation is finished, sieving the dried iron-silicon-aluminum-nickel insulating powder by using a 100-mesh sieve; adding 3.0g of binder phenolic resin and 4.0g of release agent calcium stearate into the sieved powder, and uniformly mixing to obtain magnetic powder to be molded; pressing the uniformly mixed powder into a powder core blank piece by adopting a pressing pressure of about 2500MPa, wherein the powder core blank piece is an annular powder core with the outer diameter of 33.02mm, the inner diameter of 19.94mm and the height of 10.67 mm; using nitrogen as protective gas, pressing the formed powder core blank piece at 850Keeping the temperature at the temperature of 100 minutes to obtain a semi-finished magnetic powder core; and finally, spraying a layer of insulating and high-temperature-resistant epoxy resin coating on the surface of the semi-finished magnetic powder, and drying to obtain a finished metal soft magnetic powder core.
Winding a 32-turn inductance coil on the iron-silicon-aluminum-nickel metal soft magnetic powder core by adopting an enameled wire with the wire diameter phi of 1.12mm and the wire length of 0.9m, wherein the powder core obtained by measurement has the following magnetoelectric properties:
(1) under the condition of 100kHz/1V, the inductance L is 61.21 mu H;
(2) under the condition of 100kHz/1V, the quality factor Q is 70.50;
(3) direct current superposition performance under the condition of 100 kHz: when H is 100Oe, LH/L069.67%; when H is 200Oe, LH/L0=36.91%;
(4) Under the condition of 50kHz/100mT, the volume loss of the iron-silicon-aluminum-nickel soft magnetic powder core is as follows: pv is 480.74mW/cm3。
FIG. 3 is a diagram showing the DC bias performance variation of the Fe-Si-Al-Ni soft magnetic powder core in example 2 under the condition of 0 Oe-200 Oe; along with the increase of the direct current bias field intensity, the direct current bias performance of the powder core is gradually reduced; under the condition of 100Oe, the direct current bias performance of the iron-silicon-aluminum nickel powder core reaches 69.67 percent, and the direct current bias performance is excellent; fig. 4 is a graph showing the change of the effective permeability of the sendust core in example 2 under the condition of 20Hz to 2MHz, and as the test frequency increases, the effective permeability of the sendust core is always maintained at about 60, and no trend of decrease of the effective permeability with the increase of the frequency occurs, so that the sendust core has an excellent frequency stability characteristic.
Example 3
Selecting commercially available alloy components with the particle size of-200 meshes, wherein the commercially available alloy components comprise, by mass, 4.0% of Si, 4.5% of Al, 1.5% of Ni and 1000.0g of Fe-Si-Al-Ni magnetic powder as the balance; 7.8g of epoxy resin and 8.2g of SiO were added2Stirring the powder, 10.0g of acetone and 90.0g of water at normal temperature for 20 minutes to form uniform mixed slurry; heating the mixed slurry to 120 ℃, keeping the temperature and stirring for 25 minutes, and sieving the dried iron-silicon-aluminum-nickel insulating powder by using a 100-mesh sieve after the heat preservation is finished; 3.0g of a binder polyamide resin was added to the sieved powderMixing fat powder and 4.0g of release agent talcum powder uniformly to obtain magnetic powder to be molded; pressing the uniformly mixed powder into a powder core blank piece by adopting a pressing pressure of about 2200MPa, wherein the powder core blank piece is an annular powder core with the outer diameter of 33.02mm, the inner diameter of 19.94mm and the height of 10.67 mm; adopting nitrogen as protective gas, and keeping the pressed powder core blank at 900 ℃ for 80 minutes to obtain a semi-finished product of the magnetic powder core; and finally, spraying a layer of insulating and high-temperature-resistant epoxy resin coating on the surface of the semi-finished magnetic powder, and drying to obtain a finished metal soft magnetic powder core.
Winding a 32-turn inductance coil on the iron-silicon-aluminum-nickel metal soft magnetic powder core by adopting an enameled wire with the wire diameter phi of 1.12mm and the wire length of 0.9m, wherein the powder core obtained by measurement has the following magnetoelectric properties:
(1) under the condition of 100kHz/1V, the inductance L is 62.49 mu H;
(2) under the condition of 100kHz/1V, the quality factor Q is 57.01;
(3) direct current superposition performance under the condition of 100 kHz: when H is 100Oe, LH/L067.15%; when H is 200Oe, LH/L0=35.42%;
(4) Under the condition of 50kHz/100mT, the volume loss of the iron-silicon-aluminum-nickel soft magnetic powder core is as follows: pv is 527.30mW/cm3。
FIG. 5 is a diagram of DC bias performance variation of the Fe-Si-Al-Ni soft magnetic powder core under the condition of 0 Oe-200 Oe in example 3. With the increase of the DC bias field intensity, the DC bias performance of the powder core is gradually reduced. Under the condition of 100Oe, the direct current bias performance of the iron-silicon-aluminum-nickel powder core reaches 67.15 percent, and the direct current bias performance is excellent. FIG. 6 is a graph showing the effective permeability change of the Fe-Si-Al-Ni soft magnetic powder core in example 3 under the condition of 20 Hz-2 MHz. With the increase of the test frequency, the effective magnetic permeability of the iron-silicon-aluminum-nickel soft magnetic powder core is always maintained to be about 60, the trend that the effective magnetic permeability is reduced along with the increase of the frequency is avoided, and the iron-silicon-aluminum-nickel soft magnetic powder core has excellent frequency stability.
Example 4
Selecting commercially available alloy with the particle size of-200 meshes, wherein the commercially available alloy comprises 5.5% of Si, 3.0% of Al, 1.0% of Ni and 1000.0g of Fe-Si-Al-Ni magnetic powder as the rest; 7.5g of epoxy resin and 8.0g of SiO were added2Stirring the powder, 7.0g of acetone and 150.0g of water for 15 minutes at normal temperature to form uniform mixed slurry; then, heating the mixed slurry to 125 ℃, preserving heat and stirring for 60 minutes, and after the heat preservation is finished, sieving the dried iron-silicon-aluminum-nickel insulating powder by using a 100-mesh sieve; adding 3.0g of binder polyamide resin powder and 4.0g of release agent talcum powder into the sieved powder, and uniformly mixing to obtain magnetic powder to be molded; pressing the uniformly mixed powder into a powder core blank piece by adopting a pressing pressure of about 2200MPa, wherein the powder core blank piece is an annular powder core with the outer diameter of 33.02mm, the inner diameter of 19.94mm and the height of 10.67 mm; argon is used as protective gas, and the pressed powder core blank is subjected to heat preservation at 880 ℃ for 30 minutes to obtain a semi-finished product of the magnetic powder core; and finally, spraying a layer of insulating and high-temperature-resistant epoxy resin coating on the surface of the semi-finished magnetic powder, and drying to obtain a finished metal soft magnetic powder core.
Winding a 32-turn inductance coil on the iron-silicon-aluminum-nickel metal soft magnetic powder core by adopting an enameled wire with the wire diameter phi of 1.12mm and the wire length of 0.9m, wherein the powder core obtained by measurement has the following magnetoelectric properties:
(1) under the condition of 100kHz/1V, the inductance L is 60.59 mu H;
(2) under the condition of 100kHz/1V, the quality factor Q is 58.01;
(3) direct current superposition performance under the condition of 100 kHz: when H is 100Oe, LH/L067.36%; when H is 200Oe, LH/L0=35.43%;
(4) Under the condition of 50kHz/100mT, the volume loss of the iron-silicon-aluminum-nickel soft magnetic powder core is as follows: pv is 510.45mW/cm3。
FIG. 7 is a diagram of DC bias performance variation of the FeSiAlNi soft magnetic powder core in example 4 under the condition of 0 Oe-200 Oe. With the increase of the DC bias field intensity, the DC bias performance of the powder core is gradually reduced. Under the condition of 100Oe, the DC bias performance of the iron-silicon-aluminum nickel powder core reaches 67.36%, and the DC bias performance is excellent. FIG. 8 is a graph showing the effective permeability change of the Fe-Si-Al-Ni soft magnetic powder core of example 4 under the condition of 20 Hz-2 MHz. With the increase of the test frequency, the effective magnetic permeability of the iron-silicon-aluminum-nickel soft magnetic powder core is always maintained to be about 60, the trend that the effective magnetic permeability is reduced along with the increase of the frequency is avoided, and the iron-silicon-aluminum-nickel soft magnetic powder core has excellent frequency stability.
Example 5
Selecting commercially available alloy components with the particle size of-200 meshes, wherein the mass percentages of the commercially available alloy components are Si 3.5%, Al 2.0% and Ni 3.5%, and the balance is Fe, Si, Al and Ni magnetic powder 1000.0 g; 6.5g of epoxy resin and 10.2g of SiO were added2Stirring the powder, 20.0g of acetone and 80.0g of water at normal temperature for 60 minutes to form uniform mixed slurry; heating the mixed slurry to 130 ℃, preserving heat and stirring for 15 minutes, and sieving the dried iron-silicon-aluminum-nickel insulating powder by using a 100-mesh sieve after the heat preservation is finished; adding 9.0g of binder phenolic resin powder and 10.0g of release agent mica powder into the sieved powder, and uniformly mixing to obtain magnetic powder to be molded; pressing the uniformly mixed powder into a powder core blank piece by adopting a pressing pressure of about 2200MPa, wherein the powder core blank piece is an annular powder core with the outer diameter of 33.02mm, the inner diameter of 19.94mm and the height of 10.67 mm; argon is used as protective gas, and the pressed powder core blank is subjected to heat preservation at 850 ℃ for 120 minutes to obtain a semi-finished product of the magnetic powder core; and finally, spraying a layer of insulating and high-temperature-resistant epoxy resin coating on the surface of the semi-finished magnetic powder, and drying to obtain a finished metal soft magnetic powder core.
Winding a 32-turn inductance coil on the iron-silicon-aluminum-nickel metal soft magnetic powder core by adopting an enameled wire with the wire diameter phi of 1.12mm and the wire length of 0.9m, wherein the powder core obtained by measurement has the following magnetoelectric properties:
(1) under the condition of 100kHz/1V, the inductance L is 61.59 mu H;
(2) under the condition of 100kHz/1V, the quality factor Q is 59.01;
(3) direct current superposition performance under the condition of 100 kHz: when H is 100Oe, LH/L066.93%; when H is 200Oe, LH/L0=35.41%;
(4) Under the condition of 50kHz/100mT, the volume loss of the iron-silicon-aluminum-nickel soft magnetic powder core is as follows: pv is 495.86mW/cm3。
FIG. 9 is a graph showing the DC bias performance variation of the FeSiAlNi soft magnetic powder core in example 5 under the condition of 0 Oe-200 Oe. With the increase of the DC bias field intensity, the DC bias performance of the powder core is gradually reduced. Under the condition of 100Oe, the DC bias performance of the iron-silicon-aluminum nickel powder core reaches 66.93%, and the DC bias performance is excellent. FIG. 10 is a graph showing the effective permeability change of the Fe-Si-Al-Ni soft magnetic powder core of example 5 under the condition of 20 Hz-2 MHz. With the increase of the test frequency, the effective magnetic permeability of the iron-silicon-aluminum-nickel soft magnetic powder core is always maintained to be about 60, the trend that the effective magnetic permeability is reduced along with the increase of the frequency is avoided, and the iron-silicon-aluminum-nickel soft magnetic powder core has excellent frequency stability.