Iron-silicon-aluminum-nickel soft magnetic powder core with magnetic conductivity of 26 for charging pile 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 magnetic conductivity of 26 for a charging pile 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, has the excellent characteristics of low loss, low coercive force, high saturation magnetic induction intensity and the like compared with the traditional silicon steel material, and is widely applied to various electronic circuits. Especially, in order to realize high frequency, high width, constant magnetic conductivity and high quality factor of the inductance device, the magnetic device is developed towards the direction of miniaturization, intellectualization, high integration, ultra-fast transmission and the like, and the unique magnetic performance of the metal magnetic powder core has more advantages than other materials in special use occasions.
Patent CN102303115B discloses a preparation method of a 26 mu iron-silicon soft magnetic powder core, which can improve the direct current bias performance and the magnetic core loss level of the powder core by doping microelements Nb and V in iron-silicon alloy; the powder core insulation coating method adopted in the patent method is a phosphoric acid passivation method; carrying out heat treatment on the magnetic powder at the temperature of 100-200 ℃, then adding a phosphoric acid aqueous solution with the powder mass ratio of 1.6-1.8% to carry out magnetic powder insulation coating treatment, carrying out compression molding, and carrying out heat treatment at the temperature of 600-800 ℃; by the preparation method disclosed by the patent, the DC bias performance of the 26 mu iron-silicon soft magnetic powder core in a 100Oe DC bias field reaches 88 percent; in CN102543345B, a preparation method of a 26 mu Fe-Si-Al soft magnetic powder core is disclosed. The comprehensive performance of the Fe-Si-Al soft magnetic powder core is regulated and controlled by doping Ni with the impurity amount ratio of 1% and Cr with the impurity amount ratio of 1%; similarly, the DC bias performance of the 26 mu Fe-Si-Al soft magnetic powder core prepared by the traditional phosphoric acid passivation process under the condition of 100Oe can reach 76.0 percent at most.
At present, with the development of new energy electric automobile industry, supporting equipment such as charging piles and the like is actively built. The metal soft magnetic powder core adopted in the charging pile needs to have excellent direct current bias performance, namely, the magnetic core can still normally work under the condition of large-current charging, the phenomenon of magnetic saturation cannot occur, and the stability and the reliability of the charging efficiency are influenced. Therefore, on the basis of the existing soft magnetic powder core material, the metal soft magnetic powder core with high direct current bias performance and low loss is prepared by selecting magnetic powder with proper alloy components, and the development requirement of the electric automobile industry is met.
Disclosure of Invention
The invention aims to solve the technical problem of providing an iron-silicon-aluminum-nickel soft magnetic powder core with the magnetic conductivity of 26 for a charging pile and a preparation method thereof aiming at the technical current situation of the metal soft magnetic powder core.
Specifically, the invention discloses an iron-silicon-aluminum-nickel soft magnetic powder core with the effective magnetic conductivity of 26 and a preparation method thereof, and is characterized in that the method comprises 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 1.5-3.5% of epoxy resin and 1.5-3.0% of SiO2Powder, 0.8 to 2.0 percent of acetone and 7.0 to 12.0 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: adding a binder accounting for 0.2-0.8% of the powder mass and a release agent accounting for 0.3-0.8% of the powder mass into the insulated coating powder in the step (2), and uniformly mixing to obtain 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 700-800 ℃ 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, mica powder and talcum powder.
Preferably, the incubation time in step (5) is 30 to 120 minutes, preferably 60 to 100 minutes.
Preferably, the mass percentage of Si in the alloy can be selected from 3.5%, 4.0%, 4.5%, 5.0% 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 1.5%, 2.0%, 2.5%, 3.0% and 3.5%; SiO 22The powder can be selected from 1.5%, 2.0%, 2.5%, and 3.0% by weight.
Preferably, the mass percent of the acetone can be selected from 1.0 to 1.5 percent; the mass percentage of the water can be selected from 8.0 percent to 10.0 percent.
Preferably, the mass percent of the binder can be selected from 0.4 to 0.6 percent.
Preferably, the mass percent of the release agent can be selected from 0.4 to 0.6 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 26, 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 90%, and the volume loss Pcv under the conditions of 100kHz and 50mT is lower than 450mW/cm3。
The invention also relates to application of the iron-silicon-aluminum-nickel soft magnetic powder core with the effective magnetic conductivity of 26 prepared by any one of the methods in preparation of a soft magnetic powder core for a charging pile.
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; 15.2g of epoxy resin, 29.5g 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 binder siloxane resin 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 powder into a powder core blank piece by adopting a pressing pressure of about 1900MPa, 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 700 ℃ 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 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 28.01 mu H;
(2) under the condition of 100kHz/1V, the quality factor Q is 40.71;
(3) direct current superposition performance under the condition of 100 kHz: when H is 100Oe, LH/L091.09%; when H is 200Oe, LH/L0=82.22%;
(4) Under the condition of 100kHz/50mT, the volume loss of the iron-silicon-aluminum-nickel soft magnetic powder core is as follows: pv is 412.35mW/cm3。
Fig. 1 is a graph of the change of the dc bias performance of the sendust soft magnetic powder core in example 1 under the condition of 0Oe to 200Oe, the dc bias performance of the powder core gradually decreases with the increase of the dc bias field strength, and the dc bias performance of the sendust soft magnetic powder core is still as high as 91.09% under the condition of 100Oe and 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 near 26, which 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; 34.8g of epoxy resin and 16.1g 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; argon is used as protective gas, and the pressed powder core blank is subjected to heat preservation at 750 ℃ for 100 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 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 27.56 mu H;
(2) under the condition of 100kHz/1V, the quality factor Q is 38.50;
(3) direct current superposition performance under the condition of 100 kHz: when H is 100Oe, LH/L091.87%; when H is 200Oe, LH/L0=82.41%;
(4) Under the condition of 100kHz/50mT, the volume loss of the iron-silicon-aluminum-nickel soft magnetic powder core is as follows: pv is 435.12mW/cm3。
FIG. 3 is a diagram of the variation of DC bias performance of the Fe-Si-Al-Ni soft magnetic powder core in example 2 under the condition of 0 Oe-200 Oe, wherein the DC bias performance of the powder core is gradually reduced with the increase of DC bias field strength; under the condition of 100Oe, the direct current bias performance of the iron-silicon-aluminum nickel powder core reaches 91.87 percent, and the direct current bias performance is excellent; FIG. 4 is a graph showing the effective permeability change of the Fe-Si-Al-Ni soft magnetic powder core in example 2 under the condition of 20 Hz-2 MHz; with the increase of the testing frequency, the effective magnetic permeability of the iron-silicon-aluminum-nickel soft magnetic powder core is always maintained to be close to 26, and the iron-silicon-aluminum-nickel soft magnetic powder core has excellent frequency stability.
Example 3
Selecting commercial alloy components with the particle size of-200 meshes, including Si 4%, Al 4.5% and Ni1.5% in percentage by mass, and Fe-Si-Al-Ni magnetic powder 1000.0g in balance, and then adding 22.8g of epoxy resin and 20.2g of SiO2Stirring 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; adding 3.0g of binder polyamide resin and 4.0g 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; adopting nitrogen as protective gas, and keeping the pressed powder core blank at 800 ℃ 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 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 26.52 mu H;
(2) under the condition of 100kHz/1V, the quality factor Q is 47.01;
(3) direct current superposition performance under the condition of 100 kHz: when H is 100Oe, LH/L090.95%; when H is 200Oe, LH/L0=83.93%;
(4) Under the condition of 100kHz/50mT, the volume loss of the iron-silicon-aluminum-nickel soft magnetic powder core is as follows: pv 433.28mW/cm3。
FIG. 5 is a graph of the DC bias performance of the Fe-Si-Al-Ni soft magnetic powder core in example 3 under the condition of 0 Oe-200 Oe, and the DC bias performance of the powder core is gradually reduced with the increase of the DC bias field strength; under the condition of 100Oe, the direct current bias performance of the iron-silicon-aluminum-nickel powder core reaches 90.95 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 testing frequency, the effective magnetic permeability of the iron-silicon-aluminum-nickel soft magnetic powder core is always maintained to be close to 26, and the iron-silicon-aluminum-nickel soft magnetic powder core has excellent frequency stability.
Example 4
Selecting commercially available alloy with-200 mesh particle size containing Si 5.5%, Al 3.0%, Ni 1.0%, and Fe-Si-Al-Ni magnetic powder 1000.0g, adding epoxy resin 24.8g and SiO 15.2g2Stirring the powder, 8.0g of acetone and 120.0g of water for 15 minutes at normal temperature to form uniform mixed slurry; then, heating the mixed slurry to 100 ℃, 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 2.0g of binder polyamide resin and 3.0g 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; with argonTaking gas as protective gas, and keeping the pressed powder core blank at 800 ℃ 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 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 25.98 mu H;
(2) under the condition of 100kHz/1V, the quality factor Q is 46.01;
(3) direct current superposition performance under the condition of 100 kHz: when H is 100Oe, LH/L090.89%; when H is 200Oe, LH/L0=84.00%;
(4) Under the condition of 100kHz/50mT, the volume loss of the iron-silicon-aluminum-nickel soft magnetic powder core is as follows: pv is 413.58mW/cm3。
FIG. 7 is a graph showing the variation of DC bias performance of the Fe-Si-Al-Ni soft magnetic powder core in example 4 under the condition of 0 Oe-200 Oe, wherein the DC bias performance of the powder core is gradually reduced with the increase of DC bias field strength; under the condition of 100Oe, the direct current bias performance of the iron-silicon-aluminum-nickel powder core reaches 90.89%, and the direct current bias performance is excellent; FIG. 8 is a graph showing the effective permeability change of the Fe-Si-Al-Ni soft magnetic powder core in example 4 under the condition of 20 Hz-2 MHz; with the increase of the testing frequency, the effective magnetic permeability of the iron-silicon-aluminum-nickel soft magnetic powder core is always maintained to be close to 26, and the iron-silicon-aluminum-nickel soft magnetic powder core has excellent frequency stability.
Example 5
Selecting commercially available alloy with-200 mesh particle size containing Si 3.5%, Al 2%, and Ni3.5% by weight, and Fe-Si-Al-Ni magnetic powder 1000.0g as the rest, adding 21.8g epoxy resin, and 25.2g SiO2Stirring the powder, 20.0g of acetone and 70.0g 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; 8.0g of a binder phenol was added to the sieved powderResin and 8.0g of release agent zinc stearate are uniformly mixed 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 780 ℃ 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 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 26.82 mu H;
(2) under the condition of 100kHz/1V, the quality factor Q is 47.54;
(3) direct current superposition performance under the condition of 100 kHz: when H is 100Oe, LH/L090.38%; when H is 200Oe, LH/L0=83.96%;
(4) Under the condition of 100kHz/50mT, the volume loss of the iron-silicon-aluminum-nickel soft magnetic powder core is as follows: pv is 403.28mW/cm3。
FIG. 9 is a graph of the DC bias performance of the Fe-Si-Al-Ni soft magnetic powder core in example 5 under the condition of 0 Oe-200 Oe, and the DC bias performance of the powder core is gradually reduced with the increase of the DC bias field strength; under the condition of 100Oe, the direct current bias performance of the iron-silicon-aluminum nickel powder core reaches 90.38 percent, and the direct current 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 testing frequency, the effective magnetic permeability of the iron-silicon-aluminum-nickel soft magnetic powder core is always maintained to be close to 26, and the iron-silicon-aluminum-nickel soft magnetic powder core has excellent frequency stability.