Soft magnetic alloy powder and preparation method and application thereof

Abstract

The invention discloses magnetically soft alloy powder and a preparation method and application thereof, and relates to the technical field of magnetic materials. The specific preparation method comprises the following steps: firstly, in an inert atmosphere, mixing, heating and smelting various raw materials into an alloy, continuously heating to obtain mixed steam, condensing the mixed steam, and collecting to obtain alloy powder; and then organic silicon resin is used as an insulating material, the insulating material is added into a solvent, then the alloy powder is added and evenly mixed, and finally the magnetically soft alloy powder is obtained through drying. The method is simple in process and short in production period, and a soft magnetic core made of the soft magnetic alloy powder prepared through the method has the advantages of being high in initial permeability and low in magnetic core loss.

Description

Technical Field

[0001] The present invention relates to the technical field of magnetic materials, and in particular to a soft magnetic alloy powder and a preparation method and application thereof. Background Art

[0002] With the technological and market development trends of electronic technology, electronic devices are becoming increasingly miniaturized, chip-based, high-frequency, and high-power-density. This has led to increasing demands for the performance and application characteristics of magnetic materials. One-piece molded inductors, with their advantages of high inductance, high current resistance, low magnetic leakage, and a variety of sizes, have gained widespread application. Soft magnetic alloy powder is a powder material used to make magnetic cores. It is typically composed of an alloy of one or more metal elements, including iron, nickel, cobalt, and silicon. These metal elements are alloyed to form a grain structure through specific alloying processes, including melting, mechanical alloying, vapor deposition, and electrochemical deposition. Soft magnetic alloy powder can be molded into an inductor by combining it with a coil. However, during the molding process, the enameled wire may break due to high pressure after molding, potentially leading to the risk of interlayer short circuits. This requires the soft magnetic alloy powder to possess high dielectric strength to ensure that the inductor can withstand certain high voltages and reduce the risk of short circuits in one-piece molded inductors. Furthermore, a good insulation coating can improve the magnetic stability of magnetic materials made from soft magnetic alloy powder, increase magnetic permeability, and reduce eddy current losses in the magnetic material. Patent CN105149574A discloses a method for coating iron-based soft magnetic alloy powder and a method for preparing a soft magnetic composite material. The method involves oxidizing an iron-based magnetic metal powder at high temperature and then pickling it to obtain an iron-based soft magnetic alloy powder coated with a SiO2, Al2O3, or Cr2O3 oxide layer. However, when the oxidation temperature of the iron-based soft magnetic alloy powder is too low, the oxidation effect is poor. When the oxidation temperature is too high, the particles are prone to sintering and adhesion during high-temperature sintering, resulting in increased losses. Therefore, there is an urgent need to develop a soft magnetic alloy powder to improve the magnetic permeability of magnetic materials and reduce losses. Summary of the Invention

[0003] The purpose of the present invention is to provide a soft magnetic alloy powder and a preparation method and application thereof, and to prepare a soft magnetic core with high initial magnetic permeability and low core loss by using the soft magnetic alloy powder.

[0004] In order to solve the above technical problems, the present invention specifically provides the following technical solutions: The present invention discloses a method for preparing soft magnetic alloy powder, comprising: S1: In an inert atmosphere, various raw materials are mixed, heated, and melted into an alloy. The mixture is further heated to form a mixed vapor, which is then condensed and collected to obtain alloy powder. S2: Add an insulating material to a solvent, then add the alloy powder obtained in S1, mix thoroughly, and dry to obtain a soft magnetic alloy powder. The insulating material includes at least one of silicon dioxide, aluminum oxide, a silicone resin, and polytetrafluoroethylene. The silicone resin is prepared by reacting 4-(2,3-epoxypropyloxy)carbazole, γ-piperazinylpropylmethyldimethoxysilane, and 11-chloroundecanetriethoxysilane. The silicone resin has excellent high-temperature resistance. Coating the alloy powder with the silicone resin maintains good adhesion and insulation after annealing, resulting in a soft magnetic core made from the soft magnetic alloy powder having good initial permeability and low core loss.

[0005] Preferably, the raw materials in S1 are iron, nickel, manganese, chromium, aluminum and silicon.

[0006] Preferably, the mass ratio of iron to nickel is 1:1-2.

[0007] Preferably, the mass ratio of iron to manganese is 1:0.001-0.02.

[0008] Preferably, the mass ratio of iron to chromium is 1:0.001-0.02.

[0009] Preferably, the mass ratio of iron to aluminum is 1:0.001-0.02.

[0010] Preferably, the mass ratio of iron to silicon is 1:0.001-0.02.

[0011] Preferably, the solvent in S2 is acetone, and the ratio of the amount of insulating material to the solvent is 1 g: 12-120 ml; the mass ratio of the amount of alloy powder to the amount of insulating material is 1: 0.01-0.12.

[0012] The invention also discloses a soft magnetic core, comprising the soft magnetic alloy powder prepared by the method.

[0013] The invention also discloses an inductor comprising the soft magnetic core.

[0014] The present invention discloses a method for preparing soft magnetic alloy powder, comprising: In an inert atmosphere, various raw materials are mixed, heated, and melted into an alloy. Further heating is performed to produce mixed vapor, which is then condensed and collected to produce alloy powder. Insulating material is added to a solvent, followed by the alloy powder, and mixed thoroughly. Finally, the soft magnetic alloy powder is dried at 55-70°C.

[0015] Preferably, the raw materials are iron, nickel, manganese, chromium, aluminum and silicon.

[0016] Preferably, the mass ratio of iron to nickel is 1:1-2.

[0017] Preferably, the mass ratio of iron to manganese is 1:0.001-0.02.

[0018] Preferably, the mass ratio of iron to chromium is 1:0.001-0.02.

[0019] Preferably, the mass ratio of iron to aluminum is 1:0.001-0.02.

[0020] Preferably, the mass ratio of iron to silicon is 1:0.001-0.02.

[0021] Preferably, the solvent is acetone, and the ratio of the insulating material to the solvent is 1 g: 12-120 ml.

[0022] Preferably, the mass ratio of the alloy powder to the insulating material is 1:0.01-0.12.

[0023] The present invention discloses a method for preparing an organosilicon resin, comprising: 4-(2,3-Epoxypropyloxy)carbazole and γ-piperazinylpropylmethyldimethoxysilane are added to tetrahydrofuran and reacted at 60-80°C for 18-28 hours to obtain an intermediate product. 11-Chlorowecanetriethoxysilane, tetramethylammonium hydroxide pentahydrate, water, and tetrahydrofuran are added to the intermediate product and reacted at 60-80°C for 18-28 hours. After completion of the reaction, the mixture is subjected to rotary evaporation, extraction, washing, and drying to obtain a silicone resin.

[0024] Preferably, the mass ratio of 4-(2,3-epoxypropyloxy)carbazole to γ-piperazinylpropylmethyldimethoxysilane is 1:0.8-1.5.

[0025] Preferably, the ratio of the amount of 4-(2,3-epoxypropyloxy)carbazole added to tetrahydrofuran to the amount of tetrahydrofuran used is 1 g: 10-20 ml.

[0026] Preferably, the mass ratio of the intermediate product to the amount of 11-chloroundecanetriethoxysilane used is 1:0.6-1.

[0027] Preferably, the mass ratio of the intermediate product to tetramethylammonium hydroxide pentahydrate is 1:0.06-0.1.

[0028] Preferably, the mass ratio of the intermediate product to water is 1:1.2-2.

[0029] Preferably, the ratio of the intermediate product to the tetrahydrofuran added to the intermediate product is 1 g: 5.8-7.5 ml.

[0030] Preferably, the solvent used for extraction is ethyl acetate.

[0031] Preferably, the washing solvent is a saturated sodium chloride solution.

[0032] More preferably, in the preparation of soft magnetic alloy powder, on the basis of using silicone resin, poly(ethylene glycol)-lactide-poly(ethylene glycol)-maleimide can also be used. The composite use of poly(ethylene glycol)-lactide-poly(ethylene glycol)-maleimide can improve the coating adhesion and high-temperature stability of the alloy powder, thereby improving the initial magnetic permeability of the soft magnetic core made of the prepared soft magnetic alloy powder and reducing the core loss.

[0033] Preferably, the mass ratio of the silicone resin to the poly(lactide-glycol)-poly(ethylene glycol)-maleimide is 1:0.2-1.6.

[0034] Compared with the prior art, the present invention has the following beneficial effects: The present invention proposes a soft magnetic alloy powder, its preparation method, and application. First, various raw materials are mixed, heated, and melted into an alloy under an inert atmosphere. Heating is continued to produce a mixed vapor, which is then condensed and collected to produce alloy powder. Silicone resin is then used as an insulating material, added to a solvent, and the alloy powder is then added and mixed. Finally, the powder is dried to produce the soft magnetic alloy powder. The method of the present invention has a simple process and a short production cycle. Argon gas is used as a protective gas during the production process, making the soft magnetic alloy powder less susceptible to oxidation. The soft magnetic core made from the soft magnetic alloy powder produced by the present invention exhibits the advantages of high initial magnetic permeability and low core loss. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] To more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for the embodiments or the description of the prior art. Obviously, the drawings described below are merely exemplary, and those skilled in the art can derive other implementation drawings based on the provided drawings without inventive effort.

[0036] Figure 1 This is the result diagram of the initial magnetic permeability measurement; Figure 2 This is a graph showing the core loss measurement results. DETAILED DESCRIPTION

[0037] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0038] The following first describes the concepts involved in this application with reference to the accompanying drawings. It should be noted that the following description of each concept is intended only to make the content of this application easier to understand and does not limit the scope of protection of this application. At the same time, the embodiments and features in the embodiments of this application can be combined with each other unless there is a conflict. The following detailed description of this application will be made with reference to the accompanying drawings and in conjunction with the embodiments.

[0039] Example 1: Preparation of silicone resin: 4-(2,3-Epoxypropyloxy)carbazole and γ-piperazinylpropylmethyldimethoxysilane were added to tetrahydrofuran and reacted at 70°C for 20 hours to obtain an intermediate product. 11-Chloroundecanotriethoxysilane, tetramethylammonium hydroxide pentahydrate, water, and tetrahydrofuran were added to the intermediate product and reacted at 70°C for 20 hours. After completion of the reaction, the product was rotary evaporated, extracted with ethyl acetate, washed with saturated sodium chloride solution, and finally dried to obtain the silicone resin. The mass ratio of 4-(2,3-epoxypropoxy)carbazole to γ-piperazinylpropylmethyldimethoxysilane is 1:1.16, the ratio of the amount of 4-(2,3-epoxypropoxy)carbazole added to tetrahydrofuran to tetrahydrofuran is 1g:15ml, the mass ratio of the intermediate product to 11-chloroundecanetriethoxysilane is 1:0.82, the mass ratio of the intermediate product to tetramethylammonium hydroxide pentahydrate is 1:0.086, the mass ratio of the intermediate product to water is 1:1.64, and the ratio of the intermediate product to tetrahydrofuran added to the intermediate product is 1g:6.82ml.

[0040] Preparation of soft magnetic alloy powder: Under an argon atmosphere, iron, nickel, manganese, chromium, aluminum, and silicon are mixed, heated, and melted into an alloy. The alloy is further heated to produce a mixed vapor, which is condensed and collected to obtain alloy powder. Silicone resin is added to acetone, followed by the alloy powder, and finally dried at 60°C to obtain the soft magnetic alloy powder. The mass ratio of iron to nickel is 1:1, the mass ratio of iron to manganese is 1:0.01, the mass ratio of iron to chromium is 1:0.01, the mass ratio of iron to aluminum is 1:0.01, and the mass ratio of iron to silicon is 1:0.01. The ratio of silicone resin to acetone is 1g:40ml, and the mass ratio of alloy powder to silicone resin is 1:0.03.

[0041] Example 2: The preparation of the silicone resin is the same as in Example 1.

[0042] Preparation of soft magnetic alloy powder: The preparation of soft magnetic alloy powder in this embodiment is different from that in Example 1, except that the mass ratio of alloy powder to silicone resin is 1:0.06, and other conditions and parameters are the same as in Example 1.

[0043] Example 3: The preparation of the silicone resin is the same as in Example 1.

[0044] Preparation of soft magnetic alloy powder: The preparation of soft magnetic alloy powder in this embodiment is different from that in Example 1, except that the mass ratio of alloy powder to silicone resin is 1:0.015, and other conditions and parameters are the same as in Example 1.

[0045] Example 4: The preparation of the silicone resin is the same as in Example 1.

[0046] Preparation of soft magnetic alloy powder: Under an argon atmosphere, iron, nickel, manganese, chromium, aluminum, and silicon were mixed, heated, and melted to form an alloy. The alloy was further heated to produce a mixed vapor, which was condensed and collected to obtain alloy powder. Silicone resin and poly(lactic acid, polyethylene glycol) maleimide were added to acetone, followed by the alloy powder, and finally dried at 60°C to obtain the soft magnetic alloy powder. The mass ratio of iron to nickel was 1:1, the mass ratio of iron to manganese was 1:0.01, the mass ratio of iron to chromium was 1:0.01, the mass ratio of iron to aluminum was 1:0.01, and the mass ratio of iron to silicon was 1:0.01. The ratio of silicone resin to acetone was 1g:40ml, the mass ratio of alloy powder to silicone resin was 1:0.03, and the mass ratio of silicone resin to poly(lactic acid, polyethylene glycol) maleimide was 1:0.67.

[0047] Example 5: The preparation of the silicone resin is the same as in Example 1.

[0048] Preparation of soft magnetic alloy powder: The preparation of soft magnetic alloy powder in this embodiment is compared with that in Example 4, except that the mass ratio of the amount of silicone resin to poly(lactide-co-glycol) polyethylene glycol maleimide used is 1:1.33, and other conditions and parameters are the same as in Example 4.

[0049] Example 6: The preparation of the silicone resin is the same as in Example 1.

[0050] Preparation of soft magnetic alloy powder: The preparation of soft magnetic alloy powder in this embodiment is compared with that in Example 4, except that the mass ratio of the amount of silicone resin to poly(lactide-co-glycol) polyethylene glycol maleimide used is 1:0.5, and other conditions and parameters are the same as in Example 4.

[0051] Comparative Example 1: The preparation of the silicone resin is the same as in Example 1.

[0052] Preparation of soft magnetic alloy powder: The preparation of soft magnetic alloy powder in this embodiment is different from that in Example 1, except that the mass ratio of alloy powder to silicone resin is 1:0.003, and other conditions and parameters are the same as in Example 1.

[0053] Comparative Example 2: Preparation of soft magnetic alloy powder: The preparation of soft magnetic alloy powder in this embodiment is different from that in Example 4 in that silicone resin is not used. Other conditions and parameters are the same as those in Example 4.

[0054] Experimental Example 1: Soft magnetic alloy powder was pressed and annealed to form a soft magnetic core at a pressure of 1200 MPa. The soft magnetic alloy powder was then pressed into a ring-shaped sample with an outer diameter of 20 mm, an inner diameter of 12 mm, and a thickness of 5 mm at a pressure of 1200 MPa. The sample was then annealed. The ring-shaped sample was heated to 500°C at a rate of 5°C / min under a nitrogen atmosphere, held at that temperature for 1 hour, and then cooled to room temperature to obtain a ring-shaped soft magnetic core. Magnetic properties were tested by evenly winding 20 turns of primary and secondary coils on the ring-shaped soft magnetic core using copper wire. The soft magnetic alloy powder was the soft magnetic alloy powder prepared in Examples 1-6 and Comparative Examples 1-2.

[0055] The initial magnetic permeability was measured at 25°C, a frequency of 100 kHz, and a maximum magnetic flux density of 0.05T.

[0056] The results are as follows Figure 1As shown, compared with Example 2, Example 1 of the present invention, the initial magnetic permeability of the soft magnetic core made of the soft magnetic alloy powder prepared in Example 2 is higher than that in Example 1, indicating that the increase in the coating amount of the silicone resin within a certain range can improve the initial magnetic permeability of the soft magnetic alloy powder; compared with Example 3, Example 1 shows that the reduction in the coating amount of the silicone resin within a certain range will inhibit the initial magnetic permeability of the soft magnetic core made of the soft magnetic alloy powder; compared with Example 4, Example 1 shows that on the basis of using silicone resin, the use of poly (lactic acid) polyethylene glycol maleimide combined coating can further improve the initial magnetic permeability of the soft magnetic core made of soft magnetic alloy powder; compared with Example 5, Example 4 shows that the use of poly (lactic acid) polyethylene glycol maleimide Increasing the dosage within a certain range can improve the initial magnetic permeability of the soft magnetic core made of soft magnetic alloy powder; Example 4, compared with Example 6, shows that reducing the usage of poly(lactic acid) polyethylene glycol maleimide within a certain range will inhibit the initial magnetic permeability of the soft magnetic core made of soft magnetic alloy powder; Example 1, compared with Comparative Example 1, shows that the coating usage of silicone resin needs to be within an appropriate range, and too low a level will cause the initial magnetic permeability of the soft magnetic core made of soft magnetic alloy powder to decrease; Example 4, compared with Comparative Example 2, shows that silicone resin and poly(lactic acid) polyethylene glycol maleimide need to be used together, and poly(lactic acid) polyethylene glycol maleimide alone has no obvious effect on improving the initial magnetic permeability of the soft magnetic core made of soft magnetic alloy powder.

[0057] Experimental Example 2: The core loss was measured at 25°C, a frequency of 100 kHz, and a maximum magnetic flux density of 0.05 T. Other measurement conditions and methods were the same as those in Experimental Example 1.

[0058] The results are as follows Figure 2As shown, compared with Example 2, Example 1 of the present invention, the core loss of the soft magnetic alloy powder prepared in Example 2 is lower than that in Example 1, indicating that the increase in the coating amount of the silicone resin within a certain range can reduce the core loss of the soft magnetic core made of the soft magnetic alloy powder; compared with Example 3, Example 1 shows that the reduction in the coating amount of the silicone resin within a certain range will increase the core loss of the soft magnetic core made of the soft magnetic alloy powder; compared with Example 4, Example 1 shows that on the basis of using silicone resin, the use of poly (lactide) polyethylene glycol maleimide combined coating can further reduce the core loss of the soft magnetic core made of the soft magnetic alloy powder; compared with Example 5, Example 4 shows that the increase in the coating amount of the silicone resin polyethylene glycol maleimide can further reduce the core loss of the soft magnetic core made of the soft magnetic alloy powder. Increasing the usage within a certain range can reduce the core loss of the soft magnetic core made of soft magnetic alloy powder; Example 4, compared with Example 6, shows that reducing the usage of poly(lactic acid) polyethylene glycol maleimide within a certain range can also increase the core loss of the soft magnetic core made of soft magnetic alloy powder; Example 1, compared with Comparative Example 1, shows that the coating usage of silicone resin needs to be within an appropriate range, and too low a level will cause an increase in the core loss of the soft magnetic core made of soft magnetic alloy powder; Example 4, compared with Comparative Example 2, shows that silicone resin and poly(lactic acid) polyethylene glycol maleimide need to be used together, and poly(lactic acid) polyethylene glycol maleimide alone has no obvious effect on reducing the core loss of the soft magnetic core made of soft magnetic alloy powder.

[0059] The embodiments and / or implementation methods described above are only used to illustrate the preferred embodiments and / or implementation methods for realizing the technology of the present invention, and do not impose any form of limitation on the implementation methods of the technology of the present invention. Any person skilled in the art may make slight changes or modifications to other equivalent embodiments without departing from the scope of the technical means disclosed in the content of the present invention, but they should still be regarded as technologies or embodiments that are essentially the same as the present invention.

[0060] This article uses specific examples to illustrate the principles and implementation methods of this application. The description of the above embodiments is only used to help understand the method and core ideas of this application. The above is only the preferred implementation method of this application. It should be pointed out that due to the limitations of textual expression, there are objectively infinite specific structures. For ordinary technicians in this technical field, without departing from the principles of this application, they can also make several improvements, modifications or changes, and can also combine the above technical features in an appropriate manner; these improvements, modifications, changes or combinations, or the direct application of the inventive concept and technical solution to other occasions without improvement, should be regarded as the scope of protection of this application.

Claims

1. A method for preparing soft magnetic alloy powder, comprising: S1: In an inert atmosphere, various raw materials are mixed, heated, and melted into an alloy. The mixture is further heated to form a mixed vapor, which is then condensed and collected to obtain alloy powder. S2: adding an insulating material to a solvent, then adding the alloy powder obtained in S1 and mixing, and then drying to obtain a soft magnetic alloy powder; the insulating material includes at least one of silicon dioxide, aluminum oxide, silicone resin and polytetrafluoroethylene; the silicone resin is prepared by reacting 4-(2,3-epoxypropyloxy)carbazole, γ-piperazinylpropylmethyldimethoxysilane and 11-chloroundecanetriethoxysilane.

2. The method for preparing a soft magnetic alloy powder according to claim 1, wherein: The raw materials in S1 are iron, nickel, manganese, chromium, aluminum and silicon.

3. The method for preparing a soft magnetic alloy powder according to claim 2, wherein: The mass ratio of the iron and nickel used is 1:1-2.

4. The method for preparing a soft magnetic alloy powder according to claim 2, wherein: The mass ratio of the iron and manganese used is 1:0.001-0.

02.

5. The method for preparing soft magnetic alloy powder according to claim 2, wherein: The mass ratio of the iron to chromium is 1:0.001-0.

02.

6. The method for preparing soft magnetic alloy powder according to claim 2, wherein: The mass ratio of the iron to aluminum used is 1:0.001-0.

02.

7. The method for preparing soft magnetic alloy powder according to claim 2, wherein: The mass ratio of the iron to silicon is 1:0.001-0.

02.

8. The method for preparing soft magnetic alloy powder according to claim 1, wherein: The solvent in S2 is acetone, and the ratio of the amount of insulating material to the solvent is 1g:12-120ml; the mass ratio of the amount of alloy powder to the amount of insulating material is 1:0.01-0.

12.

9. A soft magnetic core comprising the soft magnetic alloy powder prepared by the method according to any one of claims 1 to 8. 10 . An inductor comprising the soft magnetic core according to claim 9 .

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