Low-loss Fe-Si-Al soft magnetic powder core and preparation method thereof
Technical Field
The invention belongs to the technical field of soft magnetic materials, and particularly relates to a low-loss Fe-Si-Al soft magnetic powder core and a preparation method thereof.
Background
The metal soft magnetic powder core is a soft magnetic composite material obtained by pressing metal soft magnetic powder, an insulating agent, a binder and other materials through a pressing forming process, has the advantages of high resistivity, low coercive force, low loss and the like, and is widely applied to various devices such as a filter inductor, a differential mode inductor, an electric reactor and the like. When the working frequency is increased, the material loss is also increased, and particularly, the eddy current loss of the material is greatly increased. Therefore, further reduction of the powder core loss is a problem which needs to be solved at present. On the other hand, the dc bias characteristic of the soft magnetic core is another important characteristic of electronic components. The good anti-DC characteristic can ensure the stability of inductance value of the components in working and reduce the generation of noise such as circuit ripple waves and the like.
CN107424708B discloses a method for preparing an ultra-low iron loss sendust magnetic core, which comprises using sieved-200 mesh air atomized sendust powder, adding water glass solution, mica powder and the like to carry out insulation coating on the surface of metal magnetic powder, wherein the prepared powder core with the magnetic conductivity of 60 has the direct current bias characteristic of 57% under the condition of 100Oe, and the volume loss of 66mW/cm under the conditions of 50kHz and 100mT3(ii) a In order to prepare the low-loss Fe-Si-Al soft magnetic core disclosed by the patent, the heat treatment process of the core needs to be specially optimized, specifically, the core is firstly insulated for 30 minutes at the temperature of 300-350 ℃, is insulated for 30 minutes at the temperature of 500 ℃ and is insulated for 30 minutes at the temperature of 750 ℃, and the heat treatment needs to be carried out in a nitrogen atmosphere; patent CN108597714B discloses a Fe-Si-Al magnetic core and a preparation method thereof, wherein metal magnetic powder is subjected to particle size proportioning, and particularly, the proportion of fine powder of 400 meshes is not less than 32%; passivating and drying the surface of the Fe-Si-Al powder of the metal magnetic powder with phosphoric acid solution after the granularity is matched, then mixing the dried powder with silica sol aqueous solution to realize secondary insulation treatment of the surface of the metal powder, wherein the direct current bias performance of the prepared 60 mu Fe-Si-Al powder core is higher than 64 percent under the condition of 100Oe, and the core loss is lower than 300mW/cm at 100kHz and 100mT3. Through the analysis of the patents, the loss performance can be improved only by the current preparation process for preparing the low-loss iron-silicon-aluminum soft magnetic powder core by performing particle size ratio, secondary insulation coating process and multi-stage heat treatment process optimization on the powder, the process requirement is complex, and the process can be carried outThe variable parameters are more.
Aiming at the requirement of the field of electronic power devices for improving the performance of the soft magnetic powder core, the patent discloses a low-loss Fe-Si-Al soft magnetic powder core and a preparation method thereof, which can effectively improve the loss performance of Fe-Si-Al and obtain excellent soft magnetic performance, have simple and controllable process and can meet the development requirement of the future market.
Disclosure of Invention
The invention aims to solve the technical problem of providing a low-loss Fe-Si-Al soft magnetic powder core and a preparation method thereof aiming at the technical current situation of a metal soft magnetic powder core.
Specifically, the invention discloses a preparation method of a low-loss Fe-Si-Al soft magnetic powder core, which is characterized by comprising the following steps:
(1) selecting iron-silicon-aluminum magnetic powder: selecting gas atomized ferrum-silicon-aluminum magnetic powder with the particle size of less than 200 meshes, wherein the mass percentages of the alloy components are respectively 8.0-11.0% of Si, 4.0-8.0% of Al and the balance of Fe;
(2) preparation of dry insulating coated powder: taking the mass of the Fe-Si-Al metal magnetic powder in the step (1) as a proportion reference, adding 0.1-1.5 percent of organic silicon modified epoxy resin and 0.2-3.0 percent of SiO2Powder, 3.0-10.0% ethanol; stirring uniformly at normal temperature to form uniform mixed slurry; then heating to 60-90 ℃, and continuing to keep the temperature and stir; after the heat preservation is finished, sieving the dried insulating powder to obtain insulating coated powder;
(3) preparing magnetic powder to be molded: taking the mass of the Fe-Si-Al metal magnetic powder in the step (1) as a proportion reference, adding 0.1-0.8% of binder and 0.3-0.8% of release agent into the insulating coated 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 1600-2500 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 600-800 ℃ 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 usage amount of the organosilicon modified epoxy resin in the step (2) is 0.5-1.2 percent, and the SiO content is2The dosage of the powder is 1.0 to 2.5 percent, and the dosage of the ethanol is 6.0 to 8.0 percent.
Preferably, the stirring time in step (2) at normal temperature is 10 minutes to 50 minutes, preferably 15 minutes to 30 minutes.
Preferably, when the temperature in the step (2) is between 60 and 90 ℃, the stirring is continued for 15 to 60 minutes, preferably 20 to 40 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 pressing pressure of the press adopted in the step (4) is 1800 MPa-2200 MPa.
Preferably, the incubation time in step (5) is 30 to 150 minutes, preferably 60 to 120 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 8.0%, 9.0%, 9.5%, 10.0% and 11.0%; the Al content is selected from 4.0%, 5.0%, 6.0%, 7.0%, and 8.0%.
Preferably, the mass percent of the organic silicon modified epoxy resin can be selected from 0.1 percent, 0.5 percent, 1 percent, 1.2 percent and 1.5 percent; SiO 22The powder can be selected from 0.2%, 0.5%, 1.0%, 1.5%, 2.0%, 2.5%, 3.0%; the ethanol can be selected from 3.0%, 4.0%, 5.0%, 6.0%, 7.0%, 8.0%, 9.0%, and 10.0% by mass.
Preferably, the mass percent of the binder can be selected from 0.2 to 0.5 percent.
Preferably, the mass percent of the release agent can be selected from 0.4 to 0.6 percent.
The invention also relates to a gas atomized iron-silicon-aluminum soft magnetic powder core with the effective magnetic conductivity of 60, which is prepared by any one of the methods.
Preferably, the powder core direct current bias performance of the iron-silicon-aluminum soft magnetic powder core under the condition of 100Oe is higher than 59 percent, and the volume loss Pcv under the conditions of 50kHz and 100mT is lower than 90mW/cm3。
Compared with the prior art, the invention has the beneficial effects that: organic silicon modified epoxy resin is selected as a binder and SiO2The powder is used as an insulating coating, the insulating coating treatment of the iron-silicon-aluminum metal magnetic powder can be realized by a one-step method, and the iron-silicon-aluminum soft magnetic powder core with low loss and high direct current bias characteristic of 60 mu is prepared. The scheme disclosed by the patent is simple and convenient, is easy to operate, and can reduce different temperature zones in the heat treatment process through optimizing heat treatment parameters, so that the preparation cost can be greatly reduced. In addition, the technical scheme of the method does not need to carry out complex granularity screening and proportioning work on the metal magnetic powder, simplifies the working procedures and has good marketization application prospect.
Drawings
FIG. 1 is a loss chart of a low-loss sendust soft magnetic core under a condition of 50kHz in example 1 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 1000.0g of Fe-Si-Al magnetic powder with the raw powder granularity of-200 meshes, wherein the raw powder comprises 8.0 percent of Si, 8.0 percent of Al and the balance of Fe by mass percent; 1.0g of silicone-modified epoxy resin and 25.0g of SiO were added2Stirring the powder and 100.0g of ethanol for 50 minutes at normal temperature to form uniform mixed slurry; then, heating the mixed slurry to 90 ℃, keeping the temperature and stirring for 15 minutes, and after the heat preservation is finished, sieving the dried iron-silicon-aluminum insulating powder by using a 100-mesh sieve (sieving out oversize particles); to the sieved powderAdding 1.0g of adhesive siloxane resin powder and 3.0g of release agent zinc stearate, uniformly mixing to obtain magnetic powder to be molded, pressing the uniformly mixed magnetic powder to be molded into a powder core blank under the pressure of about 2000MPa, wherein the powder core blank is an annular powder core with the outer diameter of 27.00mm, ×, the inner diameter of 14.80mm, × and the height of 11.18mm, keeping the temperature of the powder core blank which is pressed and molded at 600 ℃ for 150 minutes by using nitrogen as protective gas to obtain a semi-finished product magnetic powder core, finally spraying a layer of insulating and high-temperature-resistant epoxy resin coating on the surface of the semi-finished product magnetic powder, and drying to obtain a finished metal soft magnetic powder core.
Winding 25 turns of inductance coils on the iron-silicon-aluminum metal soft magnetic powder core by adopting enameled wires with the wire diameter phi of 1.00mm and the wire length of 0.9m, wherein the powder core obtained by measurement has the following magnetoelectric properties:
the effective magnetic conductivity 60 crushing method iron-silicon-aluminum powder core prepared by the method disclosed by the patent has the direct current bias performance of 59.84% under the condition of 100Oe and the volume loss of 75.06mW/cm under 50kHz and 100mT3The loss performance is greatly improved, and the DC bias circuit has excellent DC bias characteristics.
Example 2
Selecting commercially available alloy components with the particle size of-200 meshes, wherein the commercially available alloy components comprise 9.0% of Si, 7.0% of Al and 1000.0g of Fe-Si-Al magnetic powder in percentage by mass; 5.0g of silicone-modified epoxy resin and 20.0g of SiO were added2Stirring the powder and 80.0g of ethanol at normal temperature for 40 minutes to form uniform mixed slurry, heating the mixed slurry to 80 ℃, preserving heat and stirring for 30 minutes, sieving the dried sendust insulating powder by using a 100-mesh sieve after heat preservation is finished, adding 2.0g of binder phenolic resin and 4.0g of release agent calcium stearate into the sieved powder, uniformly mixing to obtain magnetic powder to be molded, pressing the uniformly mixed powder by adopting a pressing pressure of about 2100MPa to form a powder core blank piece, wherein the powder core blank piece is an annular powder core with the outer diameter of 27.00mm ×, the inner diameter of 14.80mm × and the height of 11.18mm, and adopting nitrogen to press the uniformly mixed powder into a powder core blank pieceAs protective gas, the powder core blank formed by pressing is kept warm at 650 ℃ 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 25 turns of inductance coils on the iron-silicon-aluminum metal soft magnetic powder core by adopting enameled wires with the wire diameter phi of 1.00mm and the wire length of 0.9m, wherein the powder core obtained by measurement has the following magnetoelectric properties:
the direct current bias performance of the iron-silicon-aluminum powder core prepared by the method disclosed by the patent and having the effective magnetic permeability of 60 crushing method under the condition of 100Oe is as high as 59.42 percent, and the volume loss under 50kHz and 100mT is 84.06mW/cm3The loss performance is greatly improved, and the DC bias circuit has excellent DC bias characteristics.
Example 3
Selecting commercially available alloy components with the particle size of-200 meshes, wherein the commercially available alloy components comprise 9.5% of Si, 6.0% of Al and 1000.0g of Fe-Si-Al magnetic powder in percentage by mass; 10.0g of silicone-modified epoxy resin and 15.0g of SiO were added2Stirring the powder and 70.0g of ethanol at normal temperature for 30 minutes to form uniform mixed slurry, heating the mixed slurry to 75 ℃, keeping the temperature and stirring for 40 minutes, after the heat preservation is finished, sieving the dried sendust insulating powder by using a 100-mesh sieve, adding 3.0g of binder polyamide resin powder and 5.0g of release agent into the sieved powder, uniformly mixing to obtain magnetic powder to be molded, pressing the uniformly mixed powder by adopting a pressing pressure of about 2200MPa to form a powder core blank, wherein the powder core blank is an annular powder core with the outer diameter of 27.00mm ×, the inner diameter of 14.80mm × and the height of 11.18mm, keeping the temperature of the powder core blank pressed and molded at 700 ℃ for 100 minutes by adopting nitrogen as protective gas to obtain a semi-finished product magnetic powder core, and finally spraying a layer of insulating and high-temperature-resistant epoxy resin coating on the surface of the semi-finished product magnetic powder, and drying to obtain the metal soft magnetic powder core finished product.
Winding 25 turns of inductance coils on the iron-silicon-aluminum metal soft magnetic powder core by adopting enameled wires with the wire diameter phi of 1.00mm and the wire length of 0.9m, wherein the powder core obtained by measurement has the following magnetoelectric properties:
the direct current bias performance of the iron-silicon-aluminum powder core prepared by the method disclosed by the patent and having the effective magnetic conductivity of 60 crushing method under the condition of 100Oe is up to 59.07 percent, and the volume loss under 50kHz and 100mT is 85.03mW/cm3The loss performance is greatly improved, and the DC bias circuit has excellent DC bias characteristics.
Example 4
Selecting commercially available alloy components with the particle size of-200 meshes, wherein the mass percentages of the commercially available alloy components are respectively 10.0% of Si, 5.0% of Al and 1000.0g of Fe-Si-Al magnetic powder; 12.0g of silicone-modified epoxy resin and 10.0g of SiO were added2Stirring the powder and 60.0g of ethanol at normal temperature for 20 minutes to form uniform mixed slurry, heating the mixed slurry to 70 ℃, keeping the temperature and stirring for 50 minutes, after the heat preservation is finished, sieving the dried sendust insulating powder by using a 100-mesh sieve, adding 5.0g of binder polyamide resin powder and 6.0g of release agent into the sieved powder, uniformly mixing to obtain magnetic powder to be molded, pressing the uniformly mixed powder by adopting the pressing pressure of about 2300MPa to form a powder core blank, wherein the powder core blank is an annular powder core with the outer diameter of 27.00mm ×, the inner diameter of 14.80mm × and the height of 11.18mm, keeping the temperature of the powder core blank which is pressed and molded at 750 ℃ for 90 minutes by adopting argon as protective gas to obtain a semi-finished product magnetic powder core, and finally spraying a layer of insulating and high-temperature-resistant epoxy resin coating on the surface of the semi-finished product magnetic powder, and drying to obtain the metal soft magnetic powder core finished product.
Winding 25 turns of inductance coils on the iron-silicon-aluminum metal soft magnetic powder core by adopting enameled wires with the wire diameter phi of 1.00mm and the wire length of 0.9m, wherein the powder core obtained by measurement has the following magnetoelectric properties:
the direct current bias performance of the iron-silicon-aluminum powder core prepared by the method disclosed by the patent and having the effective magnetic conductivity of 60 crushing method under the condition of 100Oe is as high as 60.45 percent, and the volume loss under 50kHz and 100mT is 75.21mW/cm3The loss performance is greatly improved, and the DC bias circuit has excellent DC bias characteristics.
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 11.0%, Al 4.0% and the balance of Fe, namely, Fe-Si-Al magnetic powder is 1000.0 g; 15.0g of silicone-modified epoxy resin and 3.0g of SiO were added2Stirring the powder and 40.0g of ethanol at normal temperature for 15 minutes to form uniform mixed slurry, heating the mixed slurry to 60 ℃, keeping the temperature and stirring for 60 minutes, sieving the dried sendust insulating powder by using a 100-mesh sieve after the heat preservation is finished, adding 8.0g of binder phenolic resin powder and 8.0g of release agent mica powder into the sieved powder, uniformly mixing to obtain magnetic powder to be molded, pressing the uniformly mixed powder by adopting a pressing pressure of about 2500MPa to form a powder core blank, wherein the powder core blank is an annular powder core with the outer diameter of 27.00mm ×, the inner diameter of 14.80mm × and the height of 11.18mm, keeping the temperature of the powder core blank which is pressed and molded at 800 ℃ for 30 minutes by adopting argon as protective gas to obtain a semi-finished product magnetic powder core, and finally spraying a layer of insulating and high-temperature-resistant epoxy resin coating on the surface of the semi-finished product magnetic powder, and drying to obtain a metal soft magnetic powder core finished product.
Winding 25 turns of inductance coils on the iron-silicon-aluminum metal soft magnetic powder core by adopting enameled wires with the wire diameter phi of 1.00mm and the wire length of 0.9m, wherein the powder core obtained by measurement has the following magnetoelectric properties:
the direct current bias performance of the iron-silicon-aluminum powder core prepared by the method disclosed by the patent and having the effective magnetic permeability of 60 crushing method under the condition of 100Oe is as high as 61.33 percent, and the volume loss under 50kHz and 100mT is 75.06mW/cm3The loss performance is greatly improved, and the DC bias circuit has excellent DC bias characteristics.
Comparative example 1
Selecting 1000.0g of Fe-Si-Al magnetic powder with the raw powder granularity of-200 meshes, wherein the raw powder comprises 8.0 percent of Si, 8.0 percent of Al and the balance of Fe by mass percent; 0.4g of silicone-modified epoxy resin and 10.0g of SiO were added2Stirring the powder and 100.0g of ethanol at normal temperature for 50 minutes to form uniform mixed slurry, heating the mixed slurry to 90 ℃, keeping the temperature and stirring for 15 minutes, after the heat preservation is finished, sieving the dried iron-silicon-aluminum insulating powder by using a 100-mesh sieve (sieving out oversize particles), adding 1.0g of adhesive siloxane resin powder and 3.0g of release agent zinc stearate into the sieved powder, uniformly mixing to obtain magnetic powder to be formed, pressing the uniformly mixed magnetic powder to be formed into a powder core blank by adopting the pressing pressure of about 2000MPa, wherein the powder core blank is an annular powder core with the outer diameter of 27.00mm ×, the inner diameter of 14.80mm × mm and the height of 11.18mm, adopting nitrogen as protective gas, keeping the temperature of the pressed and formed powder core blank at 600 ℃ for 150 minutes to obtain a semi-finished product magnetic powder core, and finally spraying a layer of insulating and high-temperature-resistant epoxy resin coating on the surface of the semi-finished product, and drying to obtain the metal soft magnetic powder core finished product.
Winding 25 turns of inductance coils on the iron-silicon-aluminum metal soft magnetic powder core by adopting enameled wires with the wire diameter phi of 1.00mm and the wire length of 0.9m, wherein the powder core obtained by measurement has the following magnetoelectric properties:
in contrast to example 1, the silicone-modified epoxy resin and SiO were reduced in comparative example 12The powder dose, the inductance of the prepared powder is 52.65 muH, which is higher than that of the powder in example 1 and exceeds the inductance specification of 60 muH. The direct current bias performance of the powder core prepared in the comparative example 1 is far lower than that of the powder core prepared in the example 1, and the loss reaches 100mW/cm3The performance is deteriorated.
Comparative example 2
Selecting commercially available alloy components with the particle size of-200 meshes, wherein the mass percentages of the commercially available alloy components are Si 11.0%, Al 4.0% and the balance of Fe, namely, Fe-Si-Al magnetic powder is 1000.0 g; 15.0g of organic is addedSilicon-modified epoxy resin, 3.0g of SiO2Stirring the powder and 40.0g of ethanol at normal temperature for 15 minutes to form uniform mixed slurry, heating the mixed slurry to 60 ℃, keeping the temperature and stirring for 60 minutes, sieving the dried sendust insulating powder by using a 100-mesh sieve after the heat preservation is finished, adding 8.0g of binder phenolic resin powder and 8.0g of release agent mica powder into the sieved powder, uniformly mixing to obtain magnetic powder to be molded, pressing the uniformly mixed powder by adopting a pressing pressure of about 1500MPa to form a powder core blank, wherein the powder core blank is an annular powder core with the outer diameter of 27.00mm ×, the inner diameter of 14.80mm × and the height of 11.18mm, keeping the temperature of the pressed and molded powder core blank at 580 ℃ by adopting argon as protective gas for 30 minutes to obtain a semi-finished product magnetic powder core, and finally spraying a layer of insulating and high-temperature-resistant epoxy resin coating on the surface of the semi-finished product magnetic powder, and drying to obtain a metal soft magnetic powder core finished product.
Winding 25 turns of inductance coils on the iron-silicon-aluminum metal soft magnetic powder core by adopting enameled wires with the wire diameter phi of 1.00mm and the wire length of 0.9m, wherein the powder core obtained by measurement has the following magnetoelectric properties:
in comparison with example 5, in comparative example 2 in which the pressing pressure and the heat treatment temperature were reduced, the inductance of the powder prepared was 40.68. mu.H, which is lower than that of example 5 and exceeds the inductance specification of 60. mu.L. The core loss prepared in comparative example 2 was much higher than that in example 5, and serious deterioration occurred.