CN113658768A - FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss and preparation method thereof - Google Patents
FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a stable-permeability low-loss FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core and a preparation method thereof. The preparation method mainly adopts a phosphoric acid/MnZn ferrite composite coating process, and MnZn ferrite coating is carried out on phosphated FeSiAl powder by a high-energy ball milling method. The invention has convenient material preparation, simple operation, uniform coating and good coating effect, is more beneficial to industrialized popularization, and simultaneously takes the ferrimagnetic MnZn ferrite as the insulating coating agent to reduce the magnetic dilution phenomenon caused by taking nonmagnetic substances as the coating agent. The invention can improve the high-frequency performance of the sendust core, and the provided FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core has low loss and stable magnetic conductivity under high frequency.
Description
Technical Field
The invention belongs to the technical field of magnetic material and device preparation, and particularly relates to a FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss and a preparation method thereof.
Background
The metal magnetic powder core is a soft magnetic composite material prepared by taking metal soft magnetic powder as a raw material and carrying out processes such as insulation coating, compression molding, heat treatment and the like. The metal magnetic powder core has higher saturation magnetic flux density than a soft magnetic ferrite core and lower medium-high frequency loss than a silicon steel lamination, so that the metal magnetic powder core can show excellent soft magnetic property, energy storage capacity and better cost performance under the conditions of proper application frequency range, higher working current and higher power. The performance of the metal magnetic powder core mainly depends on the magnetic conductivity, the particle size and the shape of the powder material, the addition of an insulating medium, the molding pressure, the heat treatment process and the like.
With the rapid development of the electronic information industry, miniaturization, high frequency and low power consumption of magnetic devices are inevitable trends of development, and the key to the performance of the magnetic devices lies in the magnetic powder core. In the current research, the sendust core has excellent performance, high saturation magnetic induction, low loss, low noise and low cost, and is widely applied in many fields. However, the sendust core has high loss and is easy to generate heat at high frequency, which limits its application in the high frequency field.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide the FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss and the preparation method thereof.
The technical scheme adopted by the invention is as follows:
the raw materials of the FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core comprise an adhesive, a lubricant and FeSiAl/MnZn ferrite composite magnetic powder, wherein the FeSiAl/MnZn ferrite composite magnetic powder comprises phosphated FeSiAl magnetic powder and a MnZn ferrite layer coated on the surface of the phosphated FeSiAl magnetic powder through ball milling.
Preferably, the FeSiAl magnetic powder comprises the following components in percentage by mass: si: 8% -13%, Al: 4 to 7 percent of the magnetic powder, and the balance of Fe, wherein the MnZn ferrite accounts for 2 to 10 percent of the mass of the phosphated FeSiAl magnetic powder.
The invention also provides a preparation method of the FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss, which comprises the following steps:
mixing the phosphated FeSiAl magnetic powder with MnZn ferrite powder, and performing ball milling to coat the MnZn ferrite on the surface of the phosphated FeSiAl magnetic powder, so as to form a MnZn ferrite layer on the surface of the phosphated FeSiAl magnetic powder, thereby obtaining FeSiAl/MnZn ferrite composite magnetic powder;
uniformly mixing FeSiAl/MnZn ferrite composite magnetic powder, an adhesive and a lubricant, and performing compression molding to obtain a FeSiAl/MnZn ferrite composite magnetic powder core blank;
and performing stress relief annealing on the FeSiAl/MnZn ferrite composite magnetic powder core blank in an inert atmosphere to obtain the FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss.
Preferably, the phosphating process of the FeSiAl magnetic powder comprises the following steps:
adding the annealed FeSiAl magnetic powder into a phosphoric acid solution for phosphorization and drying to obtain phosphorized FeSiAl magnetic powder;
the annealing process of the FeSiAl magnetic powder comprises the following steps: putting the FeSiAl magnetic powder into an atmosphere furnace, introducing reducing gas, controlling the temperature at 600-800 ℃, and carrying out heat treatment for 0.5-5 h;
the particle size of the FeSiAl magnetic powder is not more than 75 microns.
Preferably, in the phosphoric acid solution, the solvent is selected from water, alcohol or acetone, and the amount of phosphoric acid accounts for 0.1-1.5% of the weight of the FeSiAl magnetic powder.
Preferably, when the phosphated FeSiAl magnetic powder and the MnZn ferrite powder are subjected to ball milling, the ball material mass ratio is (10-15): 1, the used grinding balls are hard alloy balls with the diameter of 5-10 mm, the rotation speed of ball milling is 50-300 r/min, and the ball milling time is 4-15 h.
Preferably, the FeSiAl/MnZn ferrite composite magnetic powder, the adhesive and the lubricant are subjected to compression molding at normal temperature, the molding pressure is 1900-2500MPa, the pressurizing rate is 1-10MPa/s, and the pressure maintaining time is 10 s-3 min.
Preferably, when the FeSiAl/MnZn ferrite composite magnetic powder core blank is subjected to stress relief annealing in an inert atmosphere, the annealing temperature is 600-850 ℃, and the time is 0.5-3 h.
Preferably, the adhesive is one or a mixture of sodium silicate, silicone resin and epoxy resin, and the lubricant is one or a mixture of zinc stearate and magnesium stearate.
Preferably, the mass of the MnZn ferrite is 0-10% of that of the phosphated FeSiAl magnetic powder, the mass of the adhesive is 0.2-1.5% of that of the FeSiAl/MnZn ferrite composite magnetic powder, and the mass of the lubricant is 0.2-1.5% of that of the FeSiAl/MnZn ferrite composite magnetic powder.
Compared with the prior art, the invention has the following excellent effects:
in the FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss, the surface of the phosphated FeSiAl magnetic powder is coated with the MnZn ferrite layer through ball milling, firstly, the MnZn ferrite layer can effectively isolate the electric contact among Fe-Si-Al powder particles, increase the powder resistivity and reduce the power loss of the magnetic powder core; the MnZn ferrite is adopted for coating, so that the reduction of the saturation magnetization and the magnetic conductivity of the magnetic powder core caused by the magnetic dilution effect of the non-magnetic coating agent can be avoided; and secondly, the MnZn ferrite layer is coated on the surface of the phosphated FeSiAl magnetic powder by ball milling, so that the MnZn ferrite layer has the characteristics of uniformity and firmness, and the frequency stability of the magnetic powder core is improved. The FeSiAl/MnZn ferrite composite magnetic powder core has stable magnetic conductivity within the range of 100kHz to 1MHz, and the power loss of the magnetic powder core is 200mW/cm under the test conditions of 50kHz at 25 ℃ and 100mT (Bm)3The following. In conclusion, the invention improves the high-frequency performance of the sendust core, and the provided FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core has low loss and stable magnetic conductivity at high frequency.
Drawings
FIG. 1 is a graph showing the permeability variation with frequency of a FeSiAl/MnZn ferrite composite magnetic powder core coated with MnZn ferrite with different permeability according to an embodiment of the present invention.
FIG. 2 shows the permeability of FeSiAl/MnZn ferrite composite magnetic powder core prepared with different MnZn ferrite coating amounts according to the embodiment of the present invention as a function of frequency.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, various embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be understood, however, that in various embodiments of the invention, numerous technical details are set forth in order to provide a better understanding of the present application. However, the technical solution claimed in the present application can be implemented without these technical details and various changes and modifications based on the following embodiments.
According to the invention, the insulating coating is carried out on the surface of the iron-silicon-aluminum magnetic powder, so that the electric contact among powder particles can be blocked, the resistivity is increased, the eddy current loss of the magnetic powder core is reduced, and the high-frequency performance of the magnetic powder core is improved. The ferrite is used as the insulating coating agent, so that the magnetic dilution phenomenon caused by using a non-magnetic substance as the coating agent is reduced, and the ferrite has the advantages of high resistivity, low loss, low cost and the like, and is very suitable for the requirements of low-loss and high-frequency practical performance occasions.
Specifically, the preparation method of the FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss comprises the following steps:
s1, powder screening: taking the crushed FeSiAl powder, wherein the components and the mass percentage of each component are as follows: si: 8% -13%, Al: 4 to 7 percent of Fe, and the balance of Fe. Sieving the crushed FeSiAl powder through a screen to obtain FeSiAl powder with the particle size not more than 75 microns;
s2, powder annealing: putting the FeSiAl magnetic powder into an atmosphere furnace, introducing reducing gas, controlling the temperature at 600-800 ℃, and carrying out heat treatment for 0.5-5 h; the reducing gas is one or a mixture of hydrogen and argon;
s3, phosphorization of phosphoric acid: adding the annealed FeSiAl magnetic powder into a phosphoric acid solution for phosphorization and drying to obtain phosphorized FeSiAl magnetic powder; wherein, in the phosphoric acid solution, the solvent is one or more of water, alcohol and acetone, and the amount of phosphoric acid accounts for 0.1-1.5% of the weight of the FeSiAl magnetic powder.
S4, ball milling and coating: mixing the phosphated FeSiAl magnetic powder with MnZn ferrite powder, and performing ball-milling coating by using a high-energy ball mill to obtain FeSiAl/MnZn ferrite composite magnetic powder, wherein the magnetic conductivity of the MnZn ferrite is 1400-3000; wherein, when grinding the ball: the ball material mass ratio is (10-15): 1, using hard alloy balls as grinding balls, wherein the diameter of each hard alloy ball is 5-10 mm, the ball milling speed is 50-300 r/min, the ball milling time is 4-15 h, and the mass of MnZn ferrite is 2-10% of that of FeSiAl magnetic powder;
s5, adding an adhesive and a lubricant: mixing the adhesive and the lubricant with the FeSiAl/MnZn ferrite composite magnetic powder uniformly in sequence to ensure that the adhesive and the lubricant are mixed with the FeSiAl/MnZn ferrite composite magnetic powder uniformly, and then drying the powder; wherein, the adhesive is one or a mixture of several of sodium silicate, organic silicon resin and epoxy resin, and the lubricant is one or a mixture of two of zinc stearate and magnesium stearate; the addition amount of the adhesive is 0.2-1.5% of the mass of the FeSiAl/MnZn ferrite composite magnetic powder; the addition amount of the lubricant is 0.2-1.5% of the mass of the FeSiAl/MnZn ferrite composite magnetic powder;
s6, normal-temperature compression molding: putting the mixed and dried powder into an alloy die, and pressing at normal temperature to obtain a FeSiAl/MnZn ferrite composite magnetic powder core blank; wherein the molding pressure is 1900-2500MPa, the pressurizing rate is 1-10MPa/s, and the pressure maintaining time is 10 s-3 min;
s7, heat treatment: performing stress relief annealing on the obtained FeSiAl/MnZn ferrite composite magnetic powder core blank in an inert atmosphere to obtain the FeSiAl/MnZn ferrite composite magnetic powder core with stable magnetic conductivity and low loss; wherein the annealing temperature is 600-850 ℃, and the time is 0.5-3 h; the inert atmosphere is argon or nitrogen;
s8, spraying: and spraying epoxy resin paint on the surface of the annealed magnetic powder core.
The invention adopts a composite coating process to prepare the FeSiAl/MnZn ferrite composite soft magnetic powder core, and obtains the magnetic powder core with stable magnetic conductivity and low power loss. By adopting the phosphoric acid-MnZn ferrite composite coating process, the electric contact between iron-silicon-aluminum powder particles can be effectively isolated, the powder resistivity is increased, and the power loss of the magnetic powder core is reduced; the MnZn ferrite is adopted for coating, so that the reduction of the saturation magnetization and the magnetic conductivity of the magnetic powder core caused by the magnetic dilution effect of the non-magnetic coating agent can be avoided; the MnZn ferrite is coated on the surface of the iron-silicon-aluminum powder in a high-energy ball milling mode, and the ferrite powder is uniformly coated on the surface of the iron-silicon-aluminum alloy powder by means of the rolling effect during ball milling to form a uniform and firm ferrite insulation coating layer, so that the frequency stability of the magnetic powder core is improved. The method has the advantages of simple process, easily obtained equipment, environmental protection and easy large-scale production and industrial application.
Compared with the prior art for insulating and coating FeSiAl powder, the invention has the outstanding characteristics that the phosphoric acid/manganese zinc ferrite composite coating process is adopted, MnZn ferrite coating is carried out on the phosphated FeSiAl powder by a high-energy ball milling method, the batching is easy, the operation is simple, the coating is uniform, and the better coating effect can be realized; in addition, the use of soft magnetic MnZn ferrite cladding with higher initial permeability, high resistivity and relatively higher saturation flux density overcomes the dilution of the non-magnetic insulating cladding agent to the magnetic powder core permeability.
Example 1
The preparation method of the FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss comprises the following steps:
1. taking the crushed FeSiAl powder, wherein the components in percentage by weight are Si: 8%, Al: 7 percent and the balance of Fe. Sieving the crushed powder by a screen, and selecting powder (less than 75 microns) with a 200-mesh sieve;
2. putting the FeSiAl magnetic powder into an atmosphere furnace, introducing hydrogen, controlling the temperature at 600 ℃, and annealing for 5 hours;
3. adding the annealed FeSiAl magnetic powder into a phosphoric acid acetone solution with solute mass percent of 0.1 wt.% for phosphorization and drying to obtain phosphorized FeSiAl magnetic powder;
4. mixing phosphatized FeSiAl magnetic powder with MnZn ferrite powder, wherein the magnetic conductivity of the MnZn ferrite is 1400, the addition amount is 6% of the mass of the FeSiAl magnetic powder, performing ball-milling coating by using a high-energy ball mill, and the ball material mass ratio is 10: 1, the number ratio of large and small grinding balls (large ball diameter 10mm, small ball diameter 5mm) is 5: 1, ball milling for 15 hours at the rotating speed of 50r/min to obtain FeSiAl/MnZn ferrite composite magnetic powder;
5. sequentially adding epoxy resin and zinc stearate, uniformly mixing with the FeSiAl/MnZn ferrite composite magnetic powder, and drying; wherein the addition amount of the epoxy resin is 0.2 wt% of the FeSiAl/MnZn ferrite composite magnetic powder, and the addition amount of the zinc stearate is 0.2 wt% of the FeSiAl/MnZn ferrite composite magnetic powder;
6. putting the mixed and dried powder into an alloy die, pressing at normal temperature, wherein the pressing rate is 10MPa/s, the pressure maintaining time is 3min, and pressing and forming at 1900MPa to obtain a FeSiAl/MnZn ferrite composite magnetic powder core blank with the outer diameter of 18.00mm, the inner diameter of 8.00mm and the height of 5.00 mm;
7. annealing the obtained FeSiAl/MnZn ferrite composite magnetic powder core blank body for 3h at 600 ℃ in a nitrogen atmosphere, and cooling to room temperature along with the furnace;
8. and spraying epoxy resin paint on the surface of the annealed magnetic powder core.
Winding 10 turns of enameled copper wire on the obtained FeSiAl/MnZn ferrite composite magnetic powder core, and testing the magnetic powder core by a SY-8218B-H analyzer to ensure that the power loss of the magnetic powder core is 193.09mW/cm under the test conditions of 50kHz and 100mT3The effective permeability as a function of frequency is shown in Table 1.
TABLE 1
Example 2
The preparation method of the FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss comprises the following steps:
1. taking the crushed FeSiAl powder, wherein the components in percentage by weight are Si: 13%, Al: 4 percent and the balance of Fe. Sieving the crushed powder by a screen, and selecting powder (less than 75 microns) with a 200-mesh sieve;
2. putting the FeSiAl magnetic powder into an atmosphere furnace, introducing hydrogen-argon mixed gas, controlling the temperature at 800 ℃, and annealing for 0.5 h;
3. adding the annealed FeSiAl magnetic powder into phosphoric acid aqueous solution with solute mass percent of 1.5 wt.% for phosphorization and drying to obtain phosphorized FeSiAl magnetic powder;
4. mixing phosphated FeSiAl magnetic powder with MnZn ferrite powder, wherein the magnetic conductivity of the MnZn ferrite is 2000, the addition amount is 6% of the mass of the FeSiAl magnetic powder, performing ball-milling coating by using a high-energy ball mill, and the ball material mass ratio is 15: 1, the number ratio of large and small grinding balls (large ball diameter 10mm, small ball diameter 5mm) is 5: 1, ball-milling for 4 hours at the rotating speed of 300r/min to obtain FeSiAl/MnZn ferrite composite magnetic powder;
5. sequentially adding organic silicon resin and magnesium stearate to the FeSiAl/MnZn ferrite composite magnetic powder, uniformly mixing, and drying; wherein, the addition amount of the organic silicon resin is 1.5 wt% of the FeSiAl/MnZn ferrite composite magnetic powder, and the addition amount of the magnesium stearate is 1.5 wt% of the FeSiAl/MnZn ferrite composite magnetic powder;
6. putting the mixed and dried powder into an alloy die, pressing at normal temperature, wherein the pressing rate is 1MPa/s, the pressure maintaining time is 10s, and pressing and forming are carried out at 2500MPa to obtain a FeSiAl/MnZn ferrite composite magnetic powder core blank with the outer diameter of 18.00mm, the inner diameter of 8.00mm and the height of 5.00 mm;
7. annealing the obtained FeSiAl/MnZn ferrite composite magnetic powder core blank at 850 ℃ for 0.5h in a nitrogen atmosphere, and cooling to room temperature along with the furnace;
8. and spraying epoxy resin paint on the surface of the annealed magnetic powder core.
Winding 10 turns of enameled copper wire on the obtained FeSiAl/MnZn ferrite composite magnetic powder core, and testing the magnetic powder core by a SY-8218B-H analyzer to obtain the magnetic powder core with the power loss of 184.8mW/cm under the test conditions of 50kHz and 100mT3The effective permeability as a function of frequency is shown in Table 2.
TABLE 2
Example 3
The preparation method of the FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss comprises the following steps:
1. taking the crushed FeSiAl powder, wherein the components in percentage by weight are Si: 9%, Al: 6 percent and the balance of Fe. Sieving the crushed powder by a screen, and selecting powder (less than 75 microns) with a 200-mesh sieve;
2. putting the FeSiAl magnetic powder into an atmosphere furnace, introducing hydrogen, controlling the temperature at 700 ℃, and annealing for 1 h;
3. adding the annealed FeSiAl magnetic powder into phosphoric acid alcohol solution with solute mass percent of 0.6 wt.% for phosphorization and drying to obtain phosphorized FeSiAl magnetic powder;
4. mixing phosphatized FeSiAl magnetic powder with MnZn ferrite powder, wherein the magnetic conductivity of the MnZn ferrite is 3000, the addition amount is 6% of the mass of the FeSiAl magnetic powder, performing ball-milling coating by using a high-energy ball mill, and the ball material mass ratio is 10: 1, the number ratio of large and small grinding balls (large ball diameter 10mm, small ball diameter 5mm) is 5: 1, ball milling for 10 hours at the rotating speed of 150r/min to obtain FeSiAl/MnZn ferrite composite magnetic powder;
5. sequentially adding sodium silicate and zinc stearate, uniformly mixing with the FeSiAl/MnZn ferrite composite magnetic powder, and drying; wherein the addition amount of the sodium silicate is 0.6 wt% of the FeSiAl/MnZn ferrite composite magnetic powder, and the addition amount of the zinc stearate is 0.6 wt% of the FeSiAl/MnZn ferrite composite magnetic powder;
6. putting the mixed and dried powder into an alloy die, pressing at normal temperature, wherein the pressing rate is 10MPa/s, the pressure maintaining time is 1min, and pressing and forming are carried out at 2100MPa to obtain a FeSiAl/MnZn ferrite composite magnetic powder core blank with the outer diameter of 18.00mm, the inner diameter of 8.00mm and the height of 5.00 mm;
7. annealing the obtained FeSiAl/MnZn ferrite composite magnetic powder core blank at 700 ℃ for 1h in an argon atmosphere, and cooling to room temperature along with the furnace;
8. and spraying epoxy resin paint on the surface of the annealed magnetic powder core.
Winding 10 turns of enameled copper wire on the obtained FeSiAl/MnZn ferrite composite magnetic powder core, and testing the magnetic powder core by a SY-8218B-H analyzer to ensure that the power loss of the magnetic powder core is 195.28mW/cm under the test conditions of 50kHz and 100mT3The effective permeability as a function of frequency is shown in Table 3.
TABLE 3
Example 4
The preparation method of the FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss comprises the following steps:
1. taking the crushed FeSiAl powder, wherein the components in percentage by weight are Si: 9.5%, Al: 6.5 percent and the balance of Fe. Sieving the crushed powder by a screen, and selecting powder (less than 75 microns) with a 200-mesh sieve;
2. putting the FeSiAl magnetic powder into an atmosphere furnace, introducing hydrogen, controlling the temperature at 700 ℃, and annealing for 1 h;
3. adding the annealed FeSiAl magnetic powder into phosphoric acid alcohol solution with solute mass percent of 0.6 wt.% for phosphorization and drying to obtain phosphorized FeSiAl magnetic powder;
4. mixing phosphated FeSiAl magnetic powder with MnZn ferrite powder, wherein the magnetic conductivity of the MnZn ferrite is 2000, the addition amounts of the MnZn ferrite are 2%, 4%, 6%, 8% and 10% of the mass of the FeSiAl magnetic powder, performing ball-milling coating by using a high-energy ball mill, and the ball material mass ratio is 10: 1, the number ratio of large and small grinding balls (large ball diameter 10mm, small ball diameter 5mm) is 5: 1, ball milling for 10 hours at the rotating speed of 150r/min to obtain FeSiAl/MnZn ferrite composite magnetic powder;
5. sequentially adding sodium silicate and zinc stearate, uniformly mixing with the FeSiAl/MnZn ferrite composite magnetic powder, and drying; wherein the addition amount of the sodium silicate is 0.6 wt% of the FeSiAl/MnZn ferrite composite magnetic powder, and the addition amount of the zinc stearate is 0.6 wt% of the FeSiAl/MnZn ferrite composite magnetic powder;
6. putting the mixed and dried powder into an alloy die, pressing at normal temperature, wherein the pressing rate is 10MPa/s, the pressure maintaining time is 1min, and pressing and forming are carried out at 2100MPa to obtain a FeSiAl/MnZn ferrite composite magnetic powder core blank with the outer diameter of 18.00mm, the inner diameter of 8.00mm and the height of 5.00 mm;
7. annealing the obtained FeSiAl/MnZn ferrite composite magnetic powder core blank body for 1h at 700 ℃ in a nitrogen atmosphere, and cooling to room temperature along with the furnace;
8. and spraying epoxy resin paint on the surface of the annealed magnetic powder core.
The obtained FeSiAl/MnZn ferrite composite magnetic powder core is wound with 10 turns of enameled copper wires, and the effective magnetic conductivity of the enameled copper wires is shown in Table 4 along with the frequency change after being tested by a SY-8218B-H analyzer.
TABLE 4
Fig. 1 and fig. 2 show the effective permeability of the FeSiAl/MnZn ferrite composite magnetic powder core prepared by the above four examples as a function of frequency, respectively. As can be seen from the figure, in the frequency range of 100kHz-1MHz, the magnetic permeability of the coated composite magnetic powder core shows better frequency stability, and the value of the magnetic permeability is higher. The ferrite belongs to soft magnetic materials, the ferrite-coated magnetic powder core can overcome the problem of magnetic dilution caused by non-magnetic coating, and the ferrite-coated magnetic powder core has increased resistivity, thereby improving the frequency stability of the effective magnetic conductivity of the magnetic powder core.
In conclusion, the preparation method of the FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss mainly comprises the steps of powder screening, annealing, phosphorization by phosphoric acid, high-energy ball milling and coating of manganese-zinc (MnZn) ferrite, compression molding and heat treatment; the method adopts a phosphoric acid/MnZn ferrite composite coating process, and MnZn ferrite coating is carried out on phosphated FeSiAl powder by a high-energy ball milling method. Its main advantage is: the preparation method has the advantages of convenient proportioning, simple operation, uniform coating, good coating effect and contribution to industrial popularization, and simultaneously reduces the magnetic dilution phenomenon caused by using a non-magnetic substance as a coating agent by using the ferrimagnetic MnZn ferrite as an insulating coating agent. The method has the advantages of simple process, easily obtained equipment, environmental friendliness and easy large-scale production and industrial application. The experimental result shows that the preparation method provided by the inventionThe magnetic powder core has stable magnetic permeability in the range of 100kHz to 1MHz, and the power loss of the magnetic powder core is 200mW/cm under the test conditions of 50kHz and 100mT of Bm at 25 DEG C3The following.
The above description is only a preferred embodiment of the present invention, and it should be noted that modifications and embellishments can be made without departing from the core technology of the present invention, and the modifications and embellishments also belong to the protection scope of the present invention. Any changes which come within the meaning and range of equivalency of the claims are to be embraced within their scope.
Claims (10)
1. The FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core is characterized in that raw materials comprise a bonding agent, a lubricating agent and FeSiAl/MnZn ferrite composite magnetic powder, and the FeSiAl/MnZn ferrite composite magnetic powder comprises phosphated FeSiAl magnetic powder and a MnZn ferrite layer coated on the surface of the phosphated FeSiAl magnetic powder through ball milling.
2. The stable-permeability low-loss FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core as claimed in claim 1, wherein the FeSiAl magnetic powder comprises the following components by mass percent: si: 8% -13%, Al: 4 to 7 percent of the magnetic powder, and the balance of Fe, wherein the MnZn ferrite accounts for 2 to 10 percent of the mass of the phosphated FeSiAl magnetic powder.
3. The preparation method of the FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss is characterized by comprising the following steps of:
mixing the phosphated FeSiAl magnetic powder with MnZn ferrite powder, and performing ball milling to coat the MnZn ferrite on the surface of the phosphated FeSiAl magnetic powder, so as to form a MnZn ferrite layer on the surface of the phosphated FeSiAl magnetic powder, thereby obtaining FeSiAl/MnZn ferrite composite magnetic powder;
uniformly mixing FeSiAl/MnZn ferrite composite magnetic powder, an adhesive and a lubricant, and performing compression molding to obtain a FeSiAl/MnZn ferrite composite magnetic powder core blank;
and performing stress relief annealing on the FeSiAl/MnZn ferrite composite magnetic powder core blank in an inert atmosphere to obtain the FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss.
4. The method for preparing the stable-permeability low-loss FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core according to claim 3, wherein the phosphating process of the FeSiAl magnetic powder comprises the following steps:
adding the annealed FeSiAl magnetic powder into a phosphoric acid solution for phosphorization and drying to obtain phosphorized FeSiAl magnetic powder;
the annealing process of the FeSiAl magnetic powder comprises the following steps: putting the FeSiAl magnetic powder into an atmosphere furnace, introducing reducing gas, controlling the temperature at 600-800 ℃, and carrying out heat treatment for 0.5-5 h;
the particle size of the FeSiAl magnetic powder is not more than 75 microns.
5. The method for preparing the FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss as claimed in claim 4, wherein in the phosphoric acid solution, the solvent is selected from water, alcohol or acetone, and the amount of phosphoric acid is 0.1-1.5% of the weight of the FeSiAl magnetic powder.
6. The preparation method of the stable-permeability low-loss FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core according to claim 3, wherein when the phosphated FeSiAl magnetic powder and the MnZn ferrite powder are subjected to ball milling, the mass ratio of the ball materials is (10-15): 1, the used grinding balls are hard alloy balls with the diameter of 5-10 mm, the rotation speed of ball milling is 50-300 r/min, and the ball milling time is 4-15 h.
7. The method for preparing the stable-permeability low-loss FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core according to claim 3, wherein the compression molding of the FeSiAl/MnZn ferrite composite magnetic powder, the binder and the lubricant is performed at normal temperature, the molding pressure is 1900-2500MPa, the pressurizing rate is 1-10MPa/s, and the pressure maintaining time is 10 s-3 min.
8. The preparation method of the stable-permeability low-loss FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core as claimed in claim 3, wherein the annealing temperature is 600-850 ℃ and the time is 0.5-3 h when the FeSiAl/MnZn ferrite composite magnetic powder core blank is subjected to stress relief annealing in an inert atmosphere.
9. The stable magnetic permeability low loss FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core according to claim 3, characterized in that the adhesive is one or a mixture of several of sodium silicate, organic silicon resin and epoxy resin, and the lubricant is one or a mixture of two of zinc stearate and magnesium stearate.
10. The stable-permeability low-loss FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core according to claim 3 or 9, characterized in that the mass of the MnZn ferrite is 2-10% of the mass of the phosphated FeSiAl magnetic powder, the mass of the adhesive is 0.2-1.5% of the mass of the FeSiAl/MnZn ferrite composite magnetic powder, and the mass of the lubricant is 0.2-1.5% of the mass of the FeSiAl/MnZn ferrite composite magnetic powder.
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