Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a preparation method of a high-superposition low-loss sendust magnetic powder core, wherein powder component adjustment and particle size optimization are performed on the magnetic powder core, and the prepared sendust magnetic powder core is low in loss and high in direct current bias performance.
In order to achieve the above purpose, the technical scheme provided by the invention is as follows:
a high-superposition low-loss sendust magnetic powder core comprises the following components in parts by weight:
1 to 50 percent of gas atomized Fe-Si-Al powder;
2 to 70 percent of gas atomized Fe-Si-Al powder;
wherein, the aerosolised sendust powder 1 consists of the following components in percentage by weight: 5.4% of Al, 9.6% of Si and 81% of Fe; the aerosolized sendust 2 consists of the following components in weight content: 5.0-6.0% of Al, 7.8-9.0% of Si and the balance of Fe.
Preferably, the gas atomized sendust powder 1 is selected from a granularity interval of-200 to +400 meshes, and the gas atomized sendust powder 2 is selected from a granularity interval of-400 meshes.
The preparation method of the high-superposition low-loss sendust magnetic powder core comprises the following specific steps:
Step one: atomizing and pulverizing: weighing the raw materials according to the component proportion, putting the raw materials into a vacuum intermediate frequency furnace for smelting, pouring the smelted molten steel into atomizing equipment, and simultaneously, impacting the molten steel with high-pressure nitrogen to prepare gas atomized Fe-Si-Al powder 1 and gas atomized Fe-Si-Al powder 2;
Step two: particle size ratio: the method comprises the steps of (1) screening the gas-atomized Fe-Si-Al powder 1 and the gas-atomized Fe-Si-Al powder 2 according to the particle size of a region, selecting the powder particle sizes required by the gas-atomized Fe-Si-Al powder 1 and the gas-atomized Fe-Si-Al powder 2, carrying out particle size proportioning, and mixing according to a proportion to obtain raw powder to be passivated;
Step three: insulating coating: adding the prepared passivation solution into the raw powder to be passivated in the second step, uniformly stirring, then parching on a heating furnace, cooling to form passivated powder, adding 1.0wt.% of organic silicon resin acetone solution into the passivated powder, uniformly stirring, heating, parching, then placing in an oven for drying, taking out, and cooling to obtain the iron-silicon-aluminum powder with the insulation coating completed;
Step four: and (5) press forming: adding a release agent and auxiliary materials into the iron-silicon-aluminum powder subjected to insulating coating, uniformly stirring, and pressing into a ring shape to obtain a ring-shaped sample;
Step five: and (3) heat treatment: placing the annular sample in a tube furnace for heat treatment under a protective atmosphere to obtain a magnetic core;
step six: impregnating and spraying: and (3) placing the magnetic core into an immersion liquid prepared by mixing epoxy resin and acetone in proportion, immersing for a certain time, cleaning, placing into an oven for baking, and then placing into a coating machine for spraying to obtain the high-superposition low-loss sendust magnetic powder core.
Preferably, in the third step, the passivation solution comprises the following components in percentage by mass: weak acid 0.1-0.3%, sodium nitrate solution 0.2-0.8%, nano-oxide powder 0.3-5%, deionized water for the rest, and controlling pH value of passivation solution to 4-7. The sodium nitrate solution is 80-90% sodium nitrate solution which is commercially available.
Preferably, the weak acid is one or more of oxalic acid, acetic acid and boric acid.
Preferably, the nano-oxide powder is one or more of zinc oxide powder, aluminum oxide powder and silicon dioxide powder.
Preferably, in the third step, the temperature of the oven is 150-200 ℃ and the drying time is 20-30 min.
Preferably, in the fourth step, the auxiliary material is glass powder, and the release agent is one or more of zinc stearate, calcium stearate and paraffin wax.
Preferably, in the fourth step, the mass ratio of the iron-silicon-aluminum powder, the release agent and the glass powder which are subjected to insulating coating is 100:0.6:0.2, and the molding pressure is 800-1200 MPa.
Preferably, in the fifth step, the annealing temperature is 600-700 ℃, the heating rate is 10 ℃/min, the heat preservation time is 1 hour, the annealing atmosphere is one or a mixture of a plurality of gases selected from hydrogen, nitrogen and argon, and the annealing is rapidly cooled after the heat preservation is finished.
Compared with the prior art, the technical scheme provided by the invention has the following remarkable effects: the invention relates to a high-superposition low-loss sendust magnetic powder core, which comprises aerosolised sendust powder 1 and aerosolised sendust powder 2, wherein the powder of the two components is screened by different granularities, and sendust powder with better comprehensive performance is selected; in the preparation method of the magnetic powder core, a passivation method is optimized to form a main composite insulating layer and an auxiliary composite insulating layer, so that the insulating layers are more uniform and compact, the concentration and the pH value of passivation solution are controlled pertinently, the magnetic powder with different components is effectively subjected to corrosion passivation, sodium nitrate is used as an oxidizing salt to perform in-situ passivation on the magnetic powder, the reaction is mild, the main insulating layer is effectively formed, nano oxidized powder is used for carrying out auxiliary insulating layer, the gap of the main insulating layer is repaired, and the iron-silicon-aluminum metal magnetic powder core with high superposition and low loss performance, wherein the magnetic permeability is about 60, the magnetic core loss is below 150mW/cm 3, and the direct current superposition characteristic can reach 68.5% maximally.
Detailed Description
The low-loss sendust core insulation cladding method will be described in connection with examples.
Example 1:
the embodiment 1 discloses a high-superposition low-loss sendust magnetic powder core, which comprises the following components in parts by weight:
1% of aerosolised Fe-Si-Al powder;
2% of aerosolised Fe-Si-Al powder;
wherein, the aerosolised sendust powder 1 consists of the following components in percentage by weight: 5.4% of Al, 9.6% of Si and 81% of Fe; the aerosolized sendust 2 consists of the following components in weight content: 5.0% of Al, 8.2% of Si and the balance of Fe.
The embodiment 1 also discloses a preparation method of the high-superposition low-loss sendust magnetic powder core, which comprises the following specific steps:
Step one: smelting the gas-atomized sendust powder 1 and the gas-atomized sendust powder 2 by adopting a vacuum gas-atomization smelting furnace;
step two: sieving out the gas atomized Fe-Si-Al powder 1 in the step one to obtain powder of-200 to +400 meshes, and sieving out the gas atomized Fe-Si-Al powder 2 to obtain powder of-400 meshes according to the following steps: 1, mixing powder and feeding to form raw powder to be passivated;
Step three: preparing a passivation solution with pH of 5 according to the proportion of 0.1% of acetic acid, 0.8% of sodium nitrate solution, 0.3% of nano zinc dioxide powder and the balance of deionized water, pouring raw powder to be passivated into the passivation solution, heating in a water bath at 90 ℃, stirring until the solution is evaporated to dryness, adding the passivated powder into 1.0wt.% of organic silicon resin acetone solution, stirring uniformly, heating and parching to dryness, then placing in a baking oven at 180 ℃ for 20min, taking out and cooling;
step four: the cooled powder is added with zinc stearate and glass powder with the mass ratio of 0.6wt% and 0.2wt% and is evenly mixed, and pressed and molded under the molding pressure of 1200 MPa.
Step five: placing the sample in an argon atmosphere furnace at 600 ℃ for sintering for 1 hour to obtain a magnetic core;
Step six: and (3) placing the magnetic core into 40% epoxy resin acetone impregnation liquid, soaking for a certain time, cleaning, placing into an oven for baking, and then placing into a coating machine for spraying to obtain the iron-silicon-aluminum metal magnetic powder core.
Comparative example 1:
The embodiment 1 discloses a high-superposition low-loss sendust magnetic powder core, which consists of the following components in percentage by weight:
1% of aerosolised Fe-Si-Al powder;
2% of gas atomized Fe-Si-Al powder;
wherein, the aerosolised sendust powder 1 consists of the following components in percentage by weight: 5.4% of Al, 9.6% of Si and 81% of Fe; the aerosolized sendust 2 consists of the following components in weight content: 5.0% of Al, 8.2% of Si and the balance of Fe.
The embodiment 1 also discloses a preparation method of the high-superposition low-loss sendust magnetic powder core, which comprises the following specific steps:
Step one: smelting the gas-atomized sendust powder 1 and the gas-atomized sendust powder 2 by adopting a vacuum gas-atomization smelting furnace;
Step two: sieving out the gas atomized Fe-Si-Al powder 1 in the step one to obtain powder of-200 to +400 meshes, and sieving out the gas atomized Fe-Si-Al powder 2 to obtain powder of-400 meshes according to the following steps: 9, mixing powder and feeding to form raw powder to be passivated;
step three: preparing a passivation solution with the pH value of 5 according to the proportion of 0.1 percent of acetic acid, 0.8 percent of sodium nitrate solution, 0.3 percent of nano zinc dioxide powder and the balance of deionized water, pouring raw powder to be passivated into the passivation solution, heating in a water bath at 90 ℃, stirring until the solution is evaporated to dryness, adding the passivated powder into 1.0wt.% of organic silicon resin acetone solution, stirring uniformly, heating and parching to dryness, then placing in a baking oven at 180 ℃ for drying for 20min, taking out and cooling;
step four: the cooled powder is added with zinc stearate and glass powder with the mass ratio of 0.6wt% and 0.2wt% and is evenly mixed, and pressed and molded under the molding pressure of 1200 MPa.
Step five: placing the sample in an argon atmosphere furnace at 600 ℃ for sintering for 1 hour to obtain a magnetic core;
Step six: and (3) placing the magnetic core into 40% epoxy resin acetone impregnation liquid, soaking for a certain time, cleaning, placing into an oven for baking, and then placing into a coating machine for spraying to obtain the iron-silicon-aluminum metal magnetic powder core.
Example 2:
The embodiment 1 discloses a high-superposition low-loss sendust magnetic powder core, which consists of the following components in percentage by weight:
1% of aerosolised Fe-Si-Al powder;
2% of gas atomized Fe-Si-Al powder;
wherein, the aerosolised sendust powder 1 consists of the following components in percentage by weight: 5.4% of Al, 9.6% of Si and 81% of Fe; the aerosolized sendust 2 consists of the following components in weight content: 5.0% of Al, 8.9% of Si and the balance of Fe.
The embodiment 1 also discloses a preparation method of the high-superposition low-loss sendust magnetic powder core, which comprises the following specific steps:
Step one: smelting the gas-atomized sendust powder 1 and the gas-atomized sendust powder 2 by adopting a vacuum gas-atomization smelting furnace;
Step two: sieving out the gas atomized Fe-Si-Al powder 1 in the step one to obtain powder of-200 to +400 meshes, and sieving out the gas atomized Fe-Si-Al powder 2 to obtain powder of-400 meshes according to the following steps: mixing and feeding to form raw powder to be passivated;
Step three: preparing a passivation solution with the pH value of 4 according to the proportion of 0.3 percent of acetic acid, 0.5 percent of sodium nitrate solution, 0.5 percent of nano silicon dioxide powder and the balance of deionized water, pouring the raw powder to be passivated into the passivation solution, heating in a water bath at 90 ℃, stirring until the solution is evaporated to dryness, adding the passivated powder into 0.9wt.% of organic silicon resin acetone solution, stirring uniformly, heating and parching to dryness, then placing in a baking oven at 150 ℃ for drying for 30min, taking out and cooling;
step four: the cooled powder is added with zinc stearate and glass powder with the mass ratio of 0.6wt% and 0.2wt% and is evenly mixed, and pressed and molded under the molding pressure of 1200 MPa.
Step five: placing the sample in an argon atmosphere furnace at 600 ℃ for sintering for 1 hour to obtain a magnetic core;
Step six: and (3) placing the magnetic core into 40% epoxy resin acetone impregnation liquid, soaking for a certain time, cleaning, placing into an oven for baking, and then placing into a coating machine for spraying to obtain the iron-silicon-aluminum metal magnetic powder core.
Comparative example 2:
The embodiment 1 discloses a high-superposition low-loss sendust magnetic powder core, which consists of the following components in percentage by weight:
1% of aerosolised sendust powder;
2% of gas atomized Fe-Si-Al powder;
wherein, the aerosolised sendust powder 1 consists of the following components in percentage by weight: 5.4% of Al, 9.6% of Si and 81% of Fe; the aerosolized sendust 2 consists of the following components in weight content: 5.0% of Al, 8.9% of Si and the balance of Fe.
The embodiment 1 also discloses a preparation method of the high-superposition low-loss sendust magnetic powder core, which comprises the following specific steps:
Step one: smelting the gas-atomized sendust powder 1 and the gas-atomized sendust powder 2 by adopting a vacuum gas-atomization smelting furnace;
Step two: sieving out the gas atomized Fe-Si-Al powder 1 in the step one to obtain powder of-200 to +400 meshes, and sieving out the gas atomized Fe-Si-Al powder 2 to obtain powder of-400 meshes according to the following steps of 9:1, mixing powder and feeding to form raw powder to be passivated;
Step three: preparing a passivation solution with the pH value of 4 according to the proportion of 0.3 percent of acetic acid, 0.5 percent of sodium nitrate solution, 0.5 percent of nano silicon dioxide powder and the balance of deionized water, pouring the raw powder to be passivated into the passivation solution, heating in a water bath at 90 ℃, stirring until the solution is evaporated to dryness, adding the passivated powder into 0.9wt.% of organic silicon resin acetone solution, stirring uniformly, heating and parching to dryness, then placing in a baking oven at 150 ℃ for drying for 30min, taking out and cooling;
step four: the cooled powder is added with zinc stearate and glass powder with the mass ratio of 0.6wt% and 0.2wt% and is evenly mixed, and pressed and molded under the molding pressure of 1200 MPa.
Step five: placing the sample in an argon atmosphere furnace at 600 ℃ for sintering for 1 hour to obtain a magnetic core;
Step six: and (3) placing the magnetic core into 40% epoxy resin acetone impregnation liquid, soaking for a certain time, cleaning, placing into an oven for baking, and then placing into a coating machine for spraying to obtain the iron-silicon-aluminum metal magnetic powder core.
The sendust core samples obtained in example 1, example 2 and comparative examples 1 and 2 were subjected to performance test, wherein the DC-Bias graph of the sendust core sample of example 1 is shown in fig. 1, the loss graph of the sendust core sample of example 1 is shown in fig. 2, and the specific test results of each example and comparative example are shown in table 1 below:
Table 1: test data of magnetic permeability, magnetic core loss and DC superposition characteristic performance of each Fe-Si-Al metal magnetic powder core sample
Group of |
Permeability (20 khz,1.0 v) |
Pcv(mW/cm3)(50kHz/100mT) |
DC-Bias(100Oe) |
Example 1 |
59.1 |
148 |
68.1% |
Comparative example 1 |
57.5 |
225 |
71% |
Example 2 |
58.8 |
144 |
68.5% |
Comparative example 2 |
59.2 |
124 |
60.2% |
The test result shows that the permeability of the sendust magnetic powder core prepared by the method is about 60, the magnetic core loss is controllable to be below 150mW/cm 3, the direct current superposition characteristic is as high as 68.5%, and the comprehensive performance is excellent, so that the sendust magnetic powder core with high superposition performance and low loss can be obtained by the method, and the sendust magnetic powder core can be applied to devices such as an output inductance line filter, a power factor corrector and the like.
The present embodiment is only illustrative of the present patent and does not limit the scope of protection thereof, and those skilled in the art can make local changes thereto, and the equivalent replacement of the present patent is considered to be within the scope of protection of the present patent as long as the spirit of the present patent is not exceeded.