CN111383810A - Preparation method of amorphous alloy magnetic powder core - Google Patents
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- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
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Abstract
The invention relates to the technical field of soft magnetic alloy, and provides a preparation method of an amorphous alloy magnetic powder core aiming at the problem that alloy magnetic powder cannot achieve both high magnetic conductivity and low power consumption. The preparation method has the advantages of simple preparation process and stable performance, and the obtained magnetic conductivity is more than 70, and the power consumption is less than 450kW/m3The amorphous alloy magnetic powder core.
Description
Technical Field
The invention relates to the technical field of soft magnetic alloy, in particular to a preparation method of an amorphous alloy magnetic powder core.
Background
The magnetic powder core is a novel composite electronic material, which is a soft magnetic material formed by mixing and pressing alloy powder and an insulating medium. The special soft magnetic performance of the magnetic powder core is hard to be compared with other soft magnetic materials, so that the magnetic powder core is widely applied and provides conditions for the development and innovation of the soft magnetic materials. The amorphous material has good direct current bias performance, low loss and good magnetic conductivity stability under the broadband condition, but the direct current bias performance is relative to the broadband conditionFor the iron powder core, the magnetic permeability of the amorphous magnetic powder core is low. Mu in the current marketa80-alloy magnetic powder core with power consumption PcvAt 500kW/m3Left and right.
One aspect of the current research on amorphous materials is to improve the properties of the raw powder material itself, for example by adding or replacing some of the trace elements Cr 87]、Co[88]、Nb[89]、Cu[90]、Mo[91]The isoelement improves the saturation magnetic induction intensity and the magnetic permeability of the material, but increases the cost; on the other hand, the preparation process of the magnetic powder core is optimized, for example, a patent with the name of "a preparation method of low-loss amorphous magnetic powder core" with the patent number of CN104575913B discloses a preparation method of low-loss amorphous magnetic powder core, aiming at providing a preparation method of low-loss amorphous magnetic powder core with low loss and good direct current superposition performance. The amorphous magnetic powder core with the magnetic conductivity of 60-90 and better strength is prepared by adding a proper high-temperature-resistant insulating material, selecting a proper insulating coating method, and performing compression molding and high-temperature annealing process. The product of the invention not only has low loss, but also has the loss lower than 500mW/cm under the condition of 100kHz/100mT3(ii) a And the method has better direct current superposition performance, and the direct current superposition performance is between 65 and 70 percent under the condition of 100Oe magnetic field intensity, but the method has complicated steps, and the magnetic conductivity and the power consumption can be further optimized. There is a need to provide an ideal solution.
Disclosure of Invention
The invention provides a preparation method of an amorphous alloy magnetic powder core, aiming at overcoming the problem that the alloy magnetic powder core cannot achieve both high magnetic conductivity and low power consumption.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an amorphous alloy magnetic powder core comprises the following steps:
1) adding iron-based amorphous powder into a phosphoric acid solution for reaction to form a layer of compact passivation film on the surface of powder particles, wherein the addition amount of phosphoric acid is 0.1-1.0 wt% of the iron-based amorphous powder;
2) uniformly mixing the passivated iron-based amorphous powder with an inorganic insulating material to obtain composite powder, wherein the addition amount of the inorganic insulating material is 0.1-2.0 wt% of the iron-based amorphous powder;
3) adding the composite powder into the diluted adhesive solution to fully mix the adhesive and the composite powder, and drying, wherein the addition amount of the adhesive is 0.5-5.0 wt% of the composite powder;
4) adding a release agent into the product obtained in the step 3) to increase the fluidity of the composite powder, wherein the addition amount of the release agent is 0.1-0.8 wt% of the composite powder;
5) pressing and molding the product obtained in the step 4), wherein the molding pressure is 1400-2200MPa, and obtaining a magnetic core blank;
6) and placing the magnetic core blank at a high temperature protected by inert atmosphere for annealing to obtain the amorphous alloy magnetic powder core finished product.
The invention adopts iron-based amorphous powder as a raw material, and firstly uses phosphoric acid solution to passivate the powder: the passivation process may increase the resistivity. And then using an inorganic insulating material as an insulating coating agent for coating: the insulating coating can effectively improve the resistivity of the magnetic powder core, so that the eddy current loss is greatly reduced, and the electromagnetic conversion efficiency and the use frequency of the magnetic powder core are improved. Although the resistivity of the inorganic substance is high, the inorganic substance has weak adhesiveness, so that it is necessary to add a binder to the magnetic powder, and the binder can also increase the resistivity of the magnetic powder core and reduce the eddy current loss of the magnetic core. Then, a release agent is added to the composite powder to increase the fluidity of the composite powder. And then pressing to obtain the magnetic core blank. And finally, annealing at a high temperature protected by inert atmosphere: residual internal stress exists in the green magnetic powder core after compression molding, which can increase the difficulty degree of magnetic domain movement and reduce the magnetic performance of the magnetic powder core, so the magnetic conductivity of the magnetic powder core is improved by annealing treatment. The annealing is carried out under inert gas, so that the magnetic powder core can be prevented from being oxidized. The amorphous alloy magnetic powder core prepared by the invention has higher magnetic conductivity and lower power consumption.
Preferably, the annealing temperature in the step 6) is 460-630 ℃, and the heating rate is 1-4 ℃/min. The internal stress cannot be better eliminated when the annealing temperature is too low; proper annealing temperature can not only reduce the magnetic performance deterioration caused by internal stress, but also reduce the defects in the magnetic powder core and improve the performance; too high annealing temperature may cause crystallization of amorphous powder, resulting in changes in the properties of the magnetic powder core.
Preferably, the annealing temperature in the step 6) is 500-590 ℃, and the heating rate is 1-3 ℃/min. The experimental results show that: within the annealing temperature range of 460-590 ℃, the magnetic conductance of the magnetic powder core is increased and then decreased, and the loss of the magnetic powder core is decreased and then increased. The annealing at the temperature of 460 and 500 ℃ is not enough to eliminate the internal stress in the magnetic powder core, and the annealing treatment is carried out on the amorphous magnetic powder core at the temperature of 590 and 630 ℃, so that the magnetic permeability of the magnetic powder core is reduced because the temperature is close to the crystallization temperature of the amorphous material.
Preferably, the amount of the phosphoric acid added in step 1) is 0.2-0.7 wt% of the iron-based amorphous powder, and the solvent of the phosphoric acid solution is selected from one of water, ethanol and acetone. The phosphoric acid reacts with the surface of the powder particle size to generate a layer of passivation film, and when the powder particle size is determined, the total specific surface area of the powder is determined. When the content of phosphoric acid is too high, the thickness of a passivation film generated on the surface of the powder increases, so that the magnetic component of the powder itself decreases, and the inductance of the prepared green compact decreases. The preferred amount of phosphoric acid in the present invention can form a thin and uniform passivation film.
Preferably, the addition amount of the inorganic insulating material in the step 2) is 0.1-1.0 wt% of the iron-based amorphous powder, and the inorganic insulating material comprises one or a mixture of more of alumina, silica, kaolin, mica powder and magnesium oxide. The magnetic powder core prepared by using one or a mixture of more of alumina, silica, kaolin, mica powder and magnesium oxide as a coating agent has higher magnetic conductivity, lower loss and better comprehensive magnetic property. The amorphous magnetic powder core has excellent magnetism due to the proper content of the coating agent. When the content of the coating agent is increased, the coating layer on the surface of the powder particle is thick, and the density of the magnetic powder core is decreased. When the content of the capping agent exceeds 1.0 wt%, the magnetic density of the magnetic powder core is reduced, so that the magnetic permeability value of the amorphous magnetic powder core is reduced. The higher the resistivity of the magnetic powder core, the smaller the eddy current loss. Since the magnetic powder core contains a magnetic powder part with lower resistivity and a non-magnetic part with higher resistivity (such as a coating agent, a binding agent and the like), the loss of the amorphous magnetic powder core generally shows a trend of decreasing when the content of the coating agent is gradually increased from low. When the content of the covering agent is increased from 0.1 wt% to 2.0 wt%, the electrical resistivity of the amorphous magnetic powder core increases as the content of the covering agent increases, and thus the eddy current loss of the amorphous magnetic powder core decreases, so that the total loss of the amorphous magnetic powder core shows a tendency of decreasing.
Preferably, the addition amount of the adhesive in the step 3) is 1.0-3.5 wt% of the composite powder, and the adhesive is one or a mixture of more of silicone resin, epoxy resin, silicone resin, phenolic resin, polyimide and cyanate resin. The optimal addition amount of the binder can form a thin uniform coating layer on the surface of the iron-based amorphous powder, so that complete coating of the powder surface can be realized, accumulation and waste are avoided, and the auxiliary material cost is saved.
Preferably, in the step 4), the addition amount of the release agent is 0.2-0.6 wt% of the composite powder, and the release agent is selected from one of zinc stearate, magnesium stearate or aluminum stearate.
Preferably, the molding pressure in the step 5) is 1600-2100 MPa. During the pressing process of the magnetic powder core, the forming pressure can cause the performance of the magnetic powder core to generate large change. If the pressure is too small, the air gaps in the pressed magnetic powder core are more, the density is smaller, and the magnetic conductivity is small. The molding pressure of the magnetic powder core is properly increased, so that the powder particles are displaced in the pressing process, and the gaps in the magnetic powder core are reduced, so that the density of the magnetic powder core is increased, the magnetic conductivity of the magnetic powder core is improved, the volume fraction of magnetic substances in the magnetic powder core can be increased, the coercive force is reduced, and the loss is reduced. When the pressure is overlarge, on one hand, the insulation coating layer is cracked due to the overlarge pressure, and the magnetic particles are exposed to increase the loss of the magnetic powder core; on the other hand, the excessive pressure can cause certain damage to the die and reduce the service life of the die.
Therefore, the invention has the following beneficial effects: (1) the invention provides a preparation method of an amorphous magnetic powder core, which has simple process and stable performance, and the obtained magnetic conductivity is more than 70, and the power consumption is less than 450kW/m3The amorphous alloy magnetic powder core; (2) the annealing temperature is preferably 460-630 ℃, so that the internal stress in the magnetic powder core can be reduced, the structure of the raw material powder can not be changed, the performance of the magnetic powder core can not be changed, and the performance of the magnetic powder core can be optimized; (3) the preferable addition amount of the binder is 1.0-3.5 wt% of the composite powder, and a thin uniform coating layer is better formed on the surface of the iron-based amorphous powder, so that complete coating on the surface of the powder can be realized, accumulation and waste are avoided, and the auxiliary material cost is saved.
Drawings
FIG. 1 is an SEM image of a crushed amorphous ribbon.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
In the present invention, unless otherwise specified, all the raw materials and equipment used are commercially available or commonly used in the art, and the methods in the examples are conventional in the art unless otherwise specified. The raw material iron-based amorphous powder used in the examples was amorphous ribbon crushed powder having main components of Fe, Si and B, and the SEM image of the crushed powder is shown in fig. 1.
Example 1
1) Adding phosphoric acid diluted by acetone into the amorphous strip crushed powder, wherein the phosphoric acid accounts for 0.3 wt% of the amorphous powder, the acetone accounts for 10 wt% of the amorphous powder, and stirring at 80 ℃ until the mixture is dried;
2) adding an inorganic insulating agent-mica powder and kaolin mixed powder (the mass ratio of mica powder to kaolin is 1:2) which accounts for 0.2 wt% of the mass of the amorphous powder into the dried powder, and uniformly mixing the amorphous powder and the inorganic insulating agent by a ball milling method to obtain composite powder;
3) adding silicone resin accounting for 1.4 wt% of the composite powder as a bonding agent, diluting the silicone resin with acetone, drying, adding zinc stearate accounting for 0.4 wt% of the composite powder as a release agent, and pressing under the pressure of 1800Mpa to form a magnetic ring with the diameter of 12.76 x 7.66 x 4.8mm (the outer diameter x the inner diameter x the height);
4) placing the pressed magnetic ring in N2Annealing at 550 ℃ for 20min in the atmosphere, wherein the heating rate is 3.0 ℃/min, and obtaining the finished product of the magnetic powder core.
Example 2
1) Adding phosphoric acid diluted by distilled water into the amorphous strip crushed powder, wherein the phosphoric acid accounts for 0.1 wt% of the amorphous powder, and the distilled water accounts for 10 wt% of the amorphous powder, and stirring at 150 ℃ until the mixture is dried;
2) adding an inorganic insulating agent-alumina accounting for 0.1 wt% of the amorphous powder into the dried powder, and uniformly mixing the amorphous powder and the inorganic insulating agent by a ball milling method to obtain composite powder;
3) adding polyimide which accounts for 5 wt% of the composite powder as an adhesive, diluting the polyimide with acetone, drying, adding magnesium stearate which accounts for 0.1 wt% of the composite powder as a release agent, and pressing under the pressure of 1400MPa to form a magnetic ring which is 12.76 x 7.66 x 4.8mm (outer diameter x inner diameter x height);
4) placing the pressed magnetic ring in N2Annealing at 460 ℃ for 20min in the atmosphere, wherein the heating rate is 1.0 ℃/min, and obtaining the finished product of the magnetic powder core.
Example 3
1) Adding phosphoric acid diluted by ethanol into the amorphous strip crushed powder, wherein the phosphoric acid accounts for 1 wt% of the amorphous powder, and the ethanol accounts for 10 wt% of the amorphous powder, and stirring at 120 ℃ until the mixture is dried;
2) adding 2 wt% of inorganic insulating agent-silicon dioxide of the mass of the amorphous powder into the dried powder, and uniformly mixing the amorphous powder and the inorganic insulating agent by a ball milling method to obtain composite powder;
3) adding epoxy resin accounting for 0.5 wt% of the composite powder as a bonding agent, diluting the epoxy resin with acetone, drying, adding aluminum stearate accounting for 0.8 wt% of the composite powder as a release agent, and pressing under 2200Mpa pressure to obtain a magnetic ring with 12.76 x 7.66 x 4.8mm (outer diameter x inner diameter x height);
4) placing the pressed magnetic ring in N2Annealing at 630 ℃ for 20min in the atmosphere, wherein the heating rate is 4.0 ℃/min, and obtaining the finished product of the magnetic powder core.
Example 4
1) Adding phosphoric acid diluted by acetone into the amorphous strip crushed powder, wherein the phosphoric acid accounts for 0.2 wt% of the amorphous powder, the acetone accounts for 10 wt% of the amorphous powder, and stirring at 80 ℃ until the mixture is dried;
2) adding an inorganic insulating agent kaolin accounting for 0.4 wt% of the weight of the amorphous powder into the dried powder, and uniformly mixing the amorphous powder and the inorganic insulating agent by a ball milling method to obtain composite powder;
3) adding silicone resin accounting for 1 wt% of the composite powder as an adhesive, diluting the silicone resin with acetone, drying, adding zinc stearate accounting for 0.2 wt% of the composite powder as a release agent, and pressing under 1600Mpa to form a magnetic ring with 12.76 x 7.66 x 4.8mm (outer diameter x inner diameter x height);
4) placing the pressed magnetic ring in N2Annealing at 500 deg.C for 20min in the atmosphere, and heating at 3.0 deg.C/min to obtain the final product.
Example 5
1) Adding phosphoric acid diluted by acetone into the amorphous strip crushed powder, wherein the phosphoric acid accounts for 0.7 wt% of the amorphous powder, the acetone accounts for 10 wt% of the amorphous powder, and stirring at 80 ℃ until the mixture is dried;
2) adding an inorganic insulating agent-magnesium oxide accounting for 1 wt% of the weight of the amorphous powder into the dried powder, and uniformly mixing the amorphous powder and the inorganic insulating agent by a ball milling method to obtain composite powder;
3) adding phenolic resin accounting for 3.5 wt% of the composite powder as a bonding agent, diluting the phenolic resin with acetone, drying, adding zinc stearate accounting for 0.6 wt% of the composite powder as a release agent, and pressing under 2100MPa to obtain a magnetic ring with the diameter of 12.76 x 7.66 x 4.8mm (the outer diameter x the inner diameter x the height);
4) placing the pressed magnetic ring in N2Annealing at 590 ℃ for 20min in the atmosphere, wherein the heating rate is 3.0 ℃/min, and obtaining the finished product of the magnetic powder core.
The test method comprises the following steps: for testing inductance L, quality factor Q (the higher the quality factor, the lower the energy representing the magnetic powder core loss, the better the magnetic performance) and direct current superposition characteristic (DCB @50Oe), a copper wire with the diameter of 0.4mm is uniformly wound on a magnetic ring for 30 turns under the test conditions of 100kHz, 1V and 25 ℃. Test Power consumption PcvUniformly winding 30 turns to 5 turns on a magnetic ring by using a copper wire with the diameter of 0.4mm under the test conditions of 100kHz and 100mT, 25 ℃. The test results are shown in the following table:
as can be seen from the above embodiments: the preparation method of the amorphous magnetic powder core provided by the invention has the advantages of simple process and stable performance by optimizing and screening the preparation process of the magnetic powder core, and the obtained amorphous magnetic powder core has the magnetic conductivity of more than 70 and the power consumption of less than 450kW/m3The amorphous alloy magnetic powder core. A permeability of more than 60 and a loss of less than 500mW/cm, as compared with that of the above-mentioned reference3The improvement is realized, and the steps are simpler. In addition, the power consumption and the magnetic conductivity of the invention can be adjusted in a small range, and more requirements can be met.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. The preparation method of the amorphous alloy magnetic powder core is characterized by comprising the following steps:
1) adding iron-based amorphous powder into a phosphoric acid solution for reaction to form a layer of compact passivation film on the surface of powder particles, wherein the addition amount of phosphoric acid is 0.1-1.0 wt% of the iron-based amorphous powder;
2) uniformly mixing the passivated iron-based amorphous powder with an inorganic insulating material to obtain composite powder, wherein the addition amount of the inorganic insulating material is 0.1-2.0 wt% of the iron-based amorphous powder;
3) adding the composite powder into the diluted adhesive solution to fully mix the adhesive and the composite powder, and drying, wherein the addition amount of the adhesive is 0.5-5.0 wt% of the iron-based amorphous powder;
4) adding a release agent into the product obtained in the step 3) to increase the fluidity of the composite powder, wherein the addition amount of the release agent is 0.1-0.8 wt% of the composite powder;
5) pressing and molding the product obtained in the step 4), wherein the molding pressure is 1400-2200MPa, and obtaining a magnetic core blank;
6) and placing the magnetic core blank at a high temperature protected by inert atmosphere for annealing to obtain the amorphous alloy magnetic powder core finished product.
2. The method as claimed in claim 1, wherein the annealing temperature in step 6) is 460-630 ℃ and the heating rate is 1-4 ℃/min.
3. The method as claimed in claim 2, wherein the annealing temperature in step 6) is 500-590 ℃, and the heating rate is 1-3 ℃/min.
4. The method for preparing an amorphous alloy magnetic powder core according to claim 1, wherein the amount of phosphoric acid added in step 1) is 0.2-0.7 wt% of the iron-based amorphous powder, and the solvent of the phosphoric acid solution is selected from one of water, ethanol or acetone.
5. The method for preparing an amorphous alloy magnetic powder core according to claim 1, wherein the amount of the inorganic insulating material added in step 2) is 0.1-1.0 wt% of the iron-based amorphous powder, and the inorganic insulating material comprises one or a mixture of more of alumina, silica, kaolin, mica powder and magnesium oxide.
6. The method for preparing the amorphous alloy magnetic powder core according to claim 1, wherein the addition amount of the adhesive in the step 3) is 1.0-3.5 wt% of the composite powder, and the adhesive is one or a mixture of more of silicone resin, epoxy resin, silicone resin, phenolic resin, polyimide and cyanate resin.
7. The method for preparing the amorphous alloy magnetic powder core according to claim 1, wherein the addition amount of the release agent in the step 4) is 0.2-0.6 wt% of the composite powder, and the release agent is selected from one of zinc stearate, magnesium stearate or aluminum stearate.
8. The method as claimed in claim 1, 2 or 3, wherein the forming pressure in step 5) is 1600-2100 MPa.
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| CN113744948A (en) * | 2021-09-01 | 2021-12-03 | 横店集团东磁股份有限公司 | Amorphous magnetic powder core precursor particle, amorphous magnetic powder core, preparation method of amorphous magnetic powder core and inductance device |
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Application publication date: 20200707 |