CN115719667A - Low-loss amorphous nano soft magnetic composite material for MHz frequency and preparation method thereof - Google Patents
Low-loss amorphous nano soft magnetic composite material for MHz frequency and preparation method thereof Download PDFInfo
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- CN115719667A CN115719667A CN202211426033.3A CN202211426033A CN115719667A CN 115719667 A CN115719667 A CN 115719667A CN 202211426033 A CN202211426033 A CN 202211426033A CN 115719667 A CN115719667 A CN 115719667A
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Abstract
The invention discloses a low-loss amorphous nano soft magnetic composite material for MHz frequency, which has the density higher than that of a common amorphous soft magnetic composite material by more than 10%, the magnetic conductivity higher than that of the common amorphous soft magnetic composite material by more than 15% and the loss lower than that of the common amorphous soft magnetic composite material by more than 30%, and is an excellent power soft magnetic composite material applied to MHz frequency. The invention relates to an amorphous nano soft magnetic composite material prepared by hot-press molding at 250-550 ℃, which consists of amorphous soft magnetic composite powder with the particle size of 2-30 mu m, nano soft magnetic powder and low-melting-point glass. The amorphous soft magnetic composite material has great application potential in the fields of wide band gap semiconductor switch power supplies, inductive devices and the like.
Description
Technical Field
The invention relates to a high-frequency low-loss amorphous nano soft magnetic composite material for MHz frequency and a preparation method thereof. The material can be applied to MHz high-frequency soft magnetic devices and has great potential in the aspects of wide-band-gap semiconductor switching power supplies, radio frequency inductors and the like.
Background
The iron-based amorphous soft magnetic composite material is an important soft magnetic material, has excellent direct current bias performance and low loss characteristic, and can be widely used as electric and electronic equipment such as inductors, switching power supplies, transformers, motors and the like. However, amorphous powder is difficult to form or has a low forming density during the pressing of soft magnetic composite materials due to its high hardness and nearly spherical shape. This requires more binder and higher compaction pressure, while too much non-magnetic forming agent causes magnetic dilution of the material, and high forming pressure can seriously damage the insulating layer and generate large internal stress during pressing, thereby reducing the permeability of the soft magnetic composite material and increasing the magnetic loss (Pcv). Also, annealing at too high a temperature can cause crystallization of the amorphous phase. Therefore, compared to crystalline materials, amorphous iron-based soft magnetic composites have a relatively low permeability, limiting their further applications.
In order to adjust the compressibility of the amorphous soft magnetic composite material and improve the magnetic performance of the amorphous soft magnetic composite material, the nanoscale soft magnetic particles are added into the amorphous powder, so that the compressibility of the amorphous soft magnetic composite material is improved, and the magnetic performance of the amorphous soft magnetic composite material is improved. The added soft magnetic nanoparticles are composed of nano soft magnetic metal and low-melting-point glass, and the low-melting-point glass is coated on the surface of the nano metal and has low melting point and cohesiveness. The mixed powder is prepared into the soft magnetic powder core by a hot-press molding process, and the glass phase on the soft magnetic nano particles is gradually softened under the action of hot pressure, so that the soft magnetic composite material with high compression density is obtained, and the soft magnetic material has the characteristics of high strength, high magnetic conductivity and low loss.
Disclosure of Invention
The invention aims to provide an amorphous nano soft magnetic composite material with high magnetic permeability and low loss for MHz. The amorphous nano soft magnetic powder core is prepared by taking amorphous soft magnetic powder as a base, uniformly mixing the amorphous soft magnetic powder with nano soft magnetic metal @ amorphous glass with a certain proportion of grain diameter of about 10-200nm after insulation coating, and then carrying out high-temperature high-pressure forming, annealing and other processes. When the powder is pressed above the glass transition temperature, the spherical amorphous powder is softened and deformed, and meanwhile, the low-melting-point nano particles are melted to fill gaps, so that the density of the powder is increased, and the soft magnetic performance is improved.
According to some embodiments of the present invention, the specific preparation method of the amorphous nano soft magnetic composite material comprises the following steps:
(1) Carrying out insulation coating treatment on the amorphous soft magnetic powder;
(2) Uniformly mixing the powder obtained in the step (1) with nano soft magnetic composite powder with a certain proportion of particles of about 10-200 nm;
(3) Pressing and molding the mixed powder obtained in the step (2) at the temperature of 250-550 ℃, wherein the pressing pressure is 500-2500 MPa;
(4) And (4) annealing the soft magnetic green body obtained in the step (3) at the temperature of 300-550 ℃ by nitrogen to obtain the high-frequency (applicable to MHz frequency) low-loss amorphous nano soft magnetic composite material.
Furthermore, the grain diameter of the amorphous soft magnetic powder is 2-30 microns, the nano soft magnetic composite powder is prepared by a sol-gel method and subsequent hydrogen reduction, and is a nano composite powder with a core-shell structure, the core is Fe or Co nano particles, and the shell is P 2 O 5 、Bi 2 O 3 、B 2 O 3 、SiO 2 And PbO, etc., and the melting point of the low-melting glass is usually 350 to 550 ℃.
Further, the insulating coating is usually a phosphate coating, a silane coating, siO 2 One or more of the coatingsAnd (4) performing composite coating.
Further, the mass ratio of the addition amount of the nano soft magnetic composite powder to the amorphous soft magnetic powder is 1-15: 100.
furthermore, the hot pressing temperature is preferably 350-500 ℃, the pressure is preferably 1000-2500 Mpa, and the pressing time is preferably 10-30 min.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, the amorphous soft magnetic composite material with high density, high magnetic permeability and low loss is prepared by insulating amorphous powder, uniformly mixing the amorphous powder with low-melting-point nano soft magnetic powder and performing hot press molding, and the problems that the existing amorphous soft magnetic composite material is difficult to mold due to high amorphous particle hardness, and the existing amorphous soft magnetic composite material has low molding density, low magnetic permeability, high loss and the like are solved.
(2) Compared with amorphous soft magnetic composite materials formed by cold pressing and other modes, the amorphous soft magnetic composite material prepared by the process has the characteristics of high density, high magnetic permeability and low loss. The magnetic conductivity between 1MHz and 200MHz is 25-45, the loss between 20mT/1MHz and 30mT/1MHz is less than 160kW/m 3 And 450kW/m 3 This property is difficult to achieve in other materials (its density is higher than that of the ordinary amorphous soft magnetic composite material by more than 10%, its magnetic permeability is higher by more than 15%, and its loss is lower by more than 30%). Therefore, the material can be well applied to the field of MHz high frequency.
Drawings
FIG. 1 is an SEM photograph of an uncoated amorphous powder (a) and an uncoated amorphous powder (b) of example 1 and a TEM photograph of a coated amorphous powder (c) as a nanopowder.
Fig. 2 is XRD patterns before and after annealing of the amorphous soft magnetic composite magnetic powder core of example 1.
FIG. 3 is a cross-sectional SEM of an amorphous nano soft magnetic composite magnetic powder core of the present invention and its elemental distribution diagram.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of protection of the invention is not limited thereto:
the nano soft magnetic composite powder adopted in the invention is prepared by a sol-gel method and subsequent hydrogen reduction, wherein one specific preparation method comprises the following steps:
adding metal nitrate (metal is Fe or Co), anhydrous glucose and at least one of boric acid, ethyl orthosilicate, phosphate, lead acetate and bismuth nitrate into anhydrous ethanol, uniformly mixing, dropwise adding ammonia water and deionized water into the mixture, reacting to gel, drying at 100-200 ℃ for 4-20h, calcining the gel product at 300-700 ℃ for 0.5-4 h, fully grinding the calcined product, and then reducing by hydrogen at 300-700 ℃ for 1-4 h to obtain the magnetic nano powder. The hydrogen reduction is typically carried out at a nitrogen to hydrogen ratio of N 2 :H 2 An atmosphere of =0.1 to 0.1. The mass ratio of the metal nitrate to the anhydrous glucose is preferably 1:4 to 1:1.
example 1
Weighing 4g 5um amorphous soft magnetic powder, adding 1wt% silane solution, ultrasonically stirring, and mixing the obtained soft magnetic composite powder with 6wt% Fe @ P 2 O 5 -SiO 2 -B 2 O 3 And uniformly grinding the nano powder in a mortar. And filling the soft magnetic composite powder into a mold, pressing for 20min at 350 ℃/1000Mpa, removing the magnetic ring after completely cooling to room temperature, and then placing the magnetic ring in a tube furnace for nitrogen annealing at 300 ℃ for 1h.
Example 2
Weighing 8g 10um amorphous soft magnetic powder, adding 4wt% of silane solution, ultrasonically stirring, and mixing the obtained soft magnetic composite powder with 5wt% of Fe @ Bi 2 O 3 -SiO 2 -B 2 O 3 The nano powder is evenly mixed in a mortar. And filling the soft magnetic composite powder into a mold, pressing for 10min at 400 ℃/1500Mpa, removing the magnetic ring after completely cooling to room temperature, and then placing the magnetic ring in a tube furnace for nitrogen annealing at 400 ℃ for 1h.
Example 3
Weighing 10g 20um amorphous soft magnetic powder, adding the amorphous soft magnetic powder into phosphating solution for treatment, adding a proper amount of tetraethoxysilane into the obtained powder, and ultrasonically stirring the obtained powder and 8wt% of Co @ Bi 2 O 3 -PbO-B 2 O 3 The nano powder is put into a mortar and mixed evenly. WhileThen filling the soft magnetic composite powder into a mould, pressing for 20min at 450 ℃/2000Mpa, removing the magnetic ring after completely cooling to room temperature, and then placing the magnetic ring in a tube furnace for nitrogen annealing for 1h at 450 ℃.
Example 4
Weighing 6g of 25um amorphous soft magnetic powder, adding phosphating solution for treatment to obtain soft magnetic composite powder and 10wt% of Co @ SiO 2 -PbO-B 2 O 3 And (3) putting the nano powder into a mortar for grinding and mixing. Then filling the soft magnetic composite powder into a mould, pressing for 10min at 500 ℃/2500Mpa, removing the magnetic ring after completely cooling to room temperature, and then placing the magnetic ring in a tube furnace for nitrogen annealing at 500 ℃ for 1h.
Example 5
Weighing 10g 30um amorphous soft magnetic powder, adding phosphating solution for treatment to obtain soft magnetic composite powder and 15wt% of Co @ Bi 2 O 3 -PbO-B 2 O 3 And (3) putting the nano powder into a mortar for grinding and mixing. Then filling the soft magnetic composite powder into a mould, pressing for 20min at 420 ℃/2000Mpa, removing the magnetic ring after completely cooling to room temperature, and then placing the magnetic ring in a tube furnace for nitrogen annealing for 1h at 500 ℃.
Example 6
Weighing 8g 15um amorphous soft magnetic powder, phosphorizing, adding 4wt% silane solution, ultrasonically stirring to obtain soft magnetic composite powder and 6wt% Fe @ Bi 2 O 3 -PbO-P 2 O 5 The nano powder is put into a mortar and mixed evenly. And filling the soft magnetic composite powder into a mold, pressing for 30min at the temperature of 420 ℃/1500Mpa, removing the magnetic ring after completely cooling to the room temperature, and then placing the magnetic ring in a tube furnace for nitrogen annealing at the temperature of 400 ℃ for 1h.
Example 7
Weighing 5g 20um amorphous soft magnetic powder, adding a proper amount of tetraethoxysilane, ultrasonically stirring, and then mixing the obtained soft magnetic composite powder with 8wt% of Fe @ Bi 2 O 3 -PbO-P 2 O 5 The nano powder is put into a mortar and mixed evenly. Then filling the soft magnetic composite powder into a mould, pressing for 12min at 350 ℃ and 1500Mpa, removing the magnetic ring after completely cooling to room temperature, and then placing the magnetic ring in a tube furnace for nitrogen annealing for 1h at 350 ℃.
Example 8
Weighing 4g 15um amorphous soft magnetic powder, adding 6wt% silane solution, ultrasonically stirring to obtain soft magnetic composite powder and 10wt% Fe @ Bi 2 O 3 -PbO-SiO 2 And (3) putting the nano powder into a mortar for grinding and mixing. And then filling the soft magnetic composite powder into a mold, preserving heat at 450 ℃ under 1800MPa, maintaining pressure for 30min, removing the magnetic ring after completely cooling to room temperature, and then placing the magnetic ring in a tube furnace for nitrogen annealing at 450 ℃ for 1h.
Example 9
Weighing 20g 30um amorphous soft magnetic powder, adding 6wt% silane solution, and ultrasonically stirring to obtain soft magnetic composite powder and 15wt% Fe @ Bi 2 O 3 -PbO-P 2 O 5 And (3) putting the nano powder into a mortar for grinding and mixing. And then filling the soft magnetic composite powder into a mold, preserving heat at 360 ℃ and 1600MPa, maintaining the pressure for 25min, removing the magnetic ring after the soft magnetic composite powder is completely cooled to room temperature, and then placing the magnetic ring in a tubular furnace for nitrogen annealing at 400 ℃ for 1h.
Example 10
Weighing 20g 25um amorphous soft magnetic powder, phosphorizing, adding 5wt% silane solution, ultrasonically stirring to obtain soft magnetic composite powder and 12wt% Fe @ Bi 2 O 3 -PbO-B 2 O 3 And (3) putting the nano powder into a mortar for grinding and mixing. And then filling the soft magnetic composite powder into a mold, preserving heat at 360 ℃ and 1900MPa, maintaining pressure for 15min, removing the magnetic ring after completely cooling to room temperature, and then placing the magnetic ring in a tube furnace for nitrogen annealing at 450 ℃ for 1h.
Table 1 shows the comparison of the properties of the amorphous nano soft magnetic composite magnetic powder cores of the examples
Claims (8)
1. Low-loss amorphous nano soft magnet for MHz frequencyThe composite material is characterized in that amorphous soft magnetic powder with the particle size of 2-30 um is used as a raw material, and the amorphous soft magnetic powder is prepared by uniformly mixing with nano soft magnetic composite powder consisting of nano soft magnetic powder and low-melting-point glass after being subjected to insulation coating; the density of the soft magnetic composite material exceeds 5.6g/cm 3 。
2. The low loss amorphous nano soft magnetic composite material for MHz frequencies according to claim 1, characterized in that the preparation method comprises:
(1) Carrying out insulation coating treatment on the amorphous soft magnetic powder;
(2) Uniformly mixing the insulated and coated powder with nano soft magnetic composite powder in a certain proportion;
(3) Pressing and molding the mixed powder obtained in the step (2) at the temperature of 250-550 ℃, wherein the pressing pressure is 500-2500 MPa, and the pressing time is 2-30 min;
(4) And (4) annealing the soft magnetic green body obtained in the step (3) at the temperature of 300-550 ℃ in nitrogen to obtain the low-loss amorphous nano soft magnetic composite material for MHz frequency.
3. Low loss amorphous nano soft magnetic composite for MHz frequencies according to claim 1 or 2, characterized in that: the nano soft magnetic composite powder is nano particles with a core-shell structure, the core is Fe or Co nano particles, the shell is low-melting-point glass, and the melting point of the nano soft magnetic composite powder is 350-550 ℃.
4. The low loss amorphous nano soft magnetic composite for MHz frequency according to claim 3, wherein said low melting glass is selected from B 2 O 3 、P 2 O 5 、SiO 2 、Bi 2 O 3 And PbO.
5. The low-loss amorphous nano soft magnetic composite material for MHz according to claim 1 or 2, wherein the mass ratio of the nano soft magnetic composite powder to the amorphous soft magnetic powder is 1-15: 100.
6. a low loss amorphous nano soft magnetic composite material for MHz frequency according to claim 1 or 2, wherein the nano soft magnetic composite powder is prepared by sol-gel method and subsequent hydrogen reduction, and the particle size of its nano particles is between 10-200 nm.
7. The low loss amorphous nano soft magnetic composite for MHz frequencies according to claim 1 or 2, characterized in that the insulating coating is a phosphate coating, silane coating, siO 2 One or more composite coatings of the coating.
8. The low-loss amorphous nano soft magnetic composite material for MHz frequency according to claim 1 or 2, wherein the material has a complex permeability of more than 30 at 1 MHz-200 MHz frequency, and magnetic loss of less than 160kW/m at 20mT/1MHz and 30mT/1MHz, respectively 3 And 450kW/m 3 。
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