Soft magnetic alloy powder, and preparation method therefor and use thereof

Abstract

The present invention relates to the technical field of magnetic materials. Disclosed are a soft magnetic alloy powder, and a preparation method therefor and a use thereof. The specific preparation method comprises: first, in an inert atmosphere, mixing, heating and smelting various raw materials into an alloy, continuing to heat the alloy to obtain mixed steam, and condensing the mixed steam to collect alloy powder; and then using an organic silicone resin as an insulating material, adding the insulating material to a solvent, then adding the alloy powder and uniformly mixing same, and finally, drying the mixture to obtain a soft magnetic alloy powder. The method of the present invention is simple and involves a short production period, and a soft magnetic core made of the soft magnetic alloy powder prepared in the present invention has the advantages of high initial permeability and low magnetic core loss.

Description

A soft magnetic alloy powder, its preparation method and application Technical Field

[0001] This invention relates to the field of magnetic materials technology, specifically to a soft magnetic alloy powder, its preparation method, and its application. Background Technology

[0002] With the development trends of electronic technology and the market, electronic devices are becoming increasingly miniaturized, surface-mounted, high-frequency, and high-power-density. This has led to continuously increasing demands on the performance and application characteristics of magnetic materials. Molded inductors, with their advantages of high inductance, high current tolerance, low leakage flux, and diverse sizes, have gained widespread application. Soft magnetic alloy powder is a powder material used to prepare magnetic cores. It is typically composed of alloys of one or more metallic elements, including iron, nickel, cobalt, and silicon. These metallic elements form a crystalline structure through specific alloying processes, including melt deposition, mechanical alloying, vapor deposition, and electrochemical deposition. Soft magnetic alloy powder can be molded with a coil in a single process to obtain a molded inductor. However, during the molding process, damage to the enameled wire after high-voltage molding may lead to interlayer short circuits. This necessitates that the soft magnetic alloy powder possess high insulation and withstand voltage characteristics to ensure the inductor can withstand a certain high voltage and reduce the risk of short circuits in the molded inductor. Simultaneously, good insulation coating can improve the stability of the magnetic properties of magnetic materials prepared from soft magnetic alloy powder, increase permeability, and reduce eddy current losses. Patent CN105149574A discloses a method for coating iron-based soft magnetic alloy powder and a method for preparing soft magnetic composite materials. The method involves oxidizing iron-based magnetic metal powder at high temperature, followed by acid washing, to obtain iron-based soft magnetic alloy powder coated with SiO2, Al2O3, or Cr2O3 oxide layers. However, when the oxidation temperature of the iron-based soft magnetic alloy powder is too low, the oxidation effect deteriorates; when the oxidation temperature is too high, the particles are prone to sintering and sticking during high-temperature sintering, leading to increased losses. Therefore, there is an urgent need to develop a soft magnetic alloy powder to improve the permeability of magnetic materials and reduce losses. Summary of the Invention

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

[0004] To solve the above-mentioned technical problems, the present invention specifically provides the following technical solution:

[0005] This invention discloses a method for preparing soft magnetic alloy powder, comprising:

[0006] S1: Under an inert atmosphere, various raw materials are mixed, heated and melted into an alloy. The mixture is then heated to form mixed steam. The mixed steam is condensed and collected to obtain alloy powder.

[0007] S2: The insulating material is added to the solvent, followed by the alloy powder obtained in S1, and mixed thoroughly. The mixture is then dried to obtain a soft magnetic alloy powder. The insulating material includes at least one of silicon dioxide, alumina, silicone resin, and polytetrafluoroethylene. The silicone resin is prepared by reacting 4-(2,3-epoxypropoxy)carbazole, γ-piperazinylpropylmethyldimethoxysilane, and 11-chloroundecanetriethoxysilane. Silicone resin has excellent high-temperature resistance. Coating the alloy powder with silicone resin results in good adhesion and good insulating coating even after annealing, thus giving the soft magnetic core made from the prepared soft magnetic alloy powder good initial permeability and low core loss.

[0008] Preferably, the raw materials in S1 are iron, nickel, manganese, chromium, aluminum and silicon.

[0009] Preferably, the mass ratio of iron to nickel used is 1:1-2.

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

[0011] Preferably, the mass ratio of iron to chromium used is 1:0.001-0.02.

[0012] Preferably, the mass ratio of iron to aluminum used is 1:0.001-0.02.

[0013] Preferably, the mass ratio of iron to silicon used is 1:0.001-0.02.

[0014] Preferably, the solvent in S2 is acetone, and the ratio of the amount of insulating material to the amount of 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.

[0015] The present invention also discloses a soft magnetic core comprising soft magnetic alloy powder prepared by the above method.

[0016] The present invention also discloses an inductor comprising the aforementioned soft magnetic core.

[0017] This invention discloses a method for preparing soft magnetic alloy powder, comprising:

[0018] Under an inert atmosphere, various raw materials are mixed, heated, and melted into an alloy. Heating continues to produce mixed steam, which is then condensed and collected to obtain alloy powder. Insulating material is added to a solvent, followed by the alloy powder, which is then mixed thoroughly. Finally, the mixture is dried at 55-70°C to obtain soft magnetic alloy powder.

[0019] Preferably, the raw materials are iron, nickel, manganese, chromium, aluminum and silicon.

[0020] Preferably, the mass ratio of iron to nickel used is 1:1-2.

[0021] Preferably, the mass ratio of iron to manganese used is 1:0.001-0.02.

[0022] Preferably, the mass ratio of iron to chromium used is 1:0.001-0.02.

[0023] Preferably, the mass ratio of iron to aluminum used is 1:0.001-0.02.

[0024] Preferably, the mass ratio of iron to silicon used is 1:0.001-0.02.

[0025] Preferably, the solvent is acetone, and the ratio of insulating material to solvent is 1g:12-120ml.

[0026] Preferably, the mass ratio of alloy powder to insulating material is 1:0.01-0.12.

[0027] This invention discloses a method for preparing organosilicon resin, comprising:

[0028] 4-(2,3-epoxypropoxy)carbazole and γ-piperazinylpropylmethyldimethoxysilane were added to tetrahydrofuran and reacted at 60-80℃ for 18-28 h to obtain an intermediate product. 11-chloroundecanetriethoxysilane, tetramethylammonium hydroxide pentahydrate, water, and tetrahydrofuran were added to the intermediate product, and the reaction was carried out at 60-80℃ for 18-28 h. After the reaction was completed, the product was obtained by rotary evaporation, extraction, washing, and drying to obtain an organosilicon resin.

[0029] Preferably, the mass ratio of 4-(2,3-epoxypropoxy)carbazole to γ-piperazinylpropylmethyldimethoxysilane is 1:0.8-1.5.

[0030] Preferably, the ratio of the amount of 4-(2,3-epoxypropoxy)carbazole added to tetrahydrofuran to the amount of tetrahydrofuran is 1g:10-20ml.

[0031] Preferably, the mass ratio of the intermediate product to 11-chloroundecanetriethoxysilane used is 1:0.6-1.

[0032] Preferably, the mass ratio of the intermediate product to tetramethylammonium hydroxide pentahydrate is 1:0.06-0.1.

[0033] Preferably, the mass ratio of the intermediate product to water used is 1:1.2-2.

[0034] Preferably, the ratio of the intermediate product to the tetrahydrofuran added to the intermediate product is 1g:5.8-7.5ml.

[0035] Preferably, the solvent used for extraction is ethyl acetate.

[0036] Preferably, the solvent used for washing is a saturated sodium chloride solution.

[0037] More preferably, in the preparation of soft magnetic alloy powder, in addition to using organosilicon resin, polyethylene glycol maleimide can also be used. The combined use of polyethylene glycol maleimide can improve the coating adhesion and high-temperature stability of the alloy powder, thereby increasing the initial permeability of the soft magnetic core made from the prepared soft magnetic alloy powder and reducing the core loss.

[0038] Preferably, the mass ratio of the amount of silicone resin to polyethylene glycol maleimide is 1:0.2-1.6.

[0039] Compared with the prior art, the present invention has the following advantages:

[0040] This invention proposes a soft magnetic alloy powder, its preparation method, and its application. First, various raw materials are mixed and heated to form an alloy under an inert atmosphere. Heating continues to produce mixed steam, which is then condensed and collected to obtain alloy powder. Next, silicone resin is used as an insulating material and added to a solvent. The alloy powder is then added and mixed thoroughly, and finally dried to obtain the soft magnetic alloy powder. This invention features a simple process, short production cycle, and argon protection during production, preventing oxidation of the soft magnetic alloy powder. Furthermore, the soft magnetic core made from the powder prepared by this invention has the advantages of high initial permeability and low core loss. Attached Figure Description

[0041] To more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are merely exemplary, and those skilled in the art can derive other embodiments based on the provided drawings without creative effort.

[0042] Figure 1 shows the results of the initial magnetic permeability measurement.

[0043] Figure 2 shows the results of the core loss measurement. Embodiments of the present invention

[0044] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0045] The concepts involved in this application will first be described with reference to the accompanying drawings. It should be noted that the following descriptions of various concepts are only for the purpose of making the content of this application easier to understand and do not constitute a limitation on the scope of protection of this application; furthermore, the embodiments and features in the embodiments of this application can be combined with each other unless otherwise specified. This application will now be described in detail with reference to the accompanying drawings and embodiments.

[0046] Example 1:

[0047] Preparation of organosilicon resin: 4-(2,3-epoxypropoxy)carbazole and γ-piperazinylpropylmethyldimethoxysilane were added to tetrahydrofuran and reacted at 70°C for 20 h to obtain an intermediate product. 11-chloroundecanetriethoxysilane, tetramethylammonium hydroxide pentahydrate, water, and tetrahydrofuran were added to the intermediate product, and the reaction was carried out at 70°C for 20 h. After the reaction was completed, the product was subjected to rotary evaporation, extraction with ethyl acetate, washing with saturated sodium chloride solution, and finally drying to obtain the organosilicon resin. The mass ratio of 4-(2,3-epoxypropoxy)carbazole to γ-piperazinylpropylmethyldimethoxysilane used was 1:1.16; the mass ratio of 4-(2,3-epoxypropoxy)carbazole added to tetrahydrofuran to tetrahydrofuran was 1 g:15 ml; the mass ratio of the intermediate product to 11-chloroundecanetriethoxysilane used was 1:0.82; the mass ratio of the intermediate product to tetramethylammonium hydroxide pentahydrate used was 1:0.086; the mass ratio of the intermediate product to water used was 1:1.64; and the mass ratio of the intermediate product to tetrahydrofuran added to the intermediate product was 1 g:6.82 ml.

[0048] Preparation of soft magnetic alloy powder: Under an argon atmosphere, iron, nickel, manganese, chromium, aluminum, and silicon were mixed and heated to form an alloy. The alloy was further heated to obtain mixed steam, which was then condensed and collected to obtain alloy powder. Organosilicon resin was added to acetone, followed by the alloy powder, and then dried at 60°C to obtain 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, the mass ratio of iron to silicon was 1:0.01, the mass ratio of organosilicon resin to acetone was 1 g:40 ml, and the mass ratio of alloy powder to organosilicon resin was 1:0.03.

[0049] Example 2:

[0050] The preparation of the silicone resin is the same as in Example 1.

[0051] Preparation of soft magnetic alloy powder: The preparation of soft magnetic alloy powder in this embodiment differs from that in Example 1 in that the mass ratio of alloy powder to organosilicon resin is 1:0.06, while other conditions and parameters are the same as in Example 1.

[0052] Example 3:

[0053] The preparation of the silicone resin is the same as in Example 1.

[0054] Preparation of soft magnetic alloy powder: The preparation of soft magnetic alloy powder in this embodiment differs from that in Example 1 in that the mass ratio of alloy powder to organosilicon resin is 1:0.015, while other conditions and parameters are the same as in Example 1.

[0055] Example 4:

[0056] The preparation of the silicone resin is the same as in Example 1.

[0057] Preparation of soft magnetic alloy powder: Iron, nickel, manganese, chromium, aluminum, and silicon were mixed and heated to form an alloy under an argon atmosphere. The alloy was further heated to obtain mixed steam, which was then condensed and collected to obtain alloy powder. Organosilicon resin and polyethylene glycol maleimide were added to acetone, followed by the alloy powder, and then dried at 60°C to obtain soft magnetic alloy powder. The mass ratios of iron and nickel were 1:1, iron and manganese were 1:0.01, iron and chromium were 1:0.01, iron and aluminum were 1:0.01, iron and silicon were 1:0.01, the ratio of organosilicon resin to acetone was 1 g:40 ml, the mass ratio of alloy powder to organosilicon resin was 1:0.03, and the mass ratio of organosilicon resin to polyethylene glycol maleimide was 1:0.67.

[0058] Example 5:

[0059] The preparation of the silicone resin is the same as in Example 1.

[0060] Preparation of soft magnetic alloy powder: The preparation of soft magnetic alloy powder in this embodiment differs from that in Example 4 in that the mass ratio of organosilicon resin to polyethylene glycol maleimide is 1:1.33, while other conditions and parameters are the same as in Example 4.

[0061] Example 6:

[0062] The preparation of the silicone resin is the same as in Example 1.

[0063] Preparation of soft magnetic alloy powder: The preparation of soft magnetic alloy powder in this embodiment differs from that in Example 4 in that the mass ratio of organosilicon resin to polyethylene glycol maleimide is 1:0.5, while other conditions and parameters are the same as in Example 4.

[0064] Comparative Example 1:

[0065] The preparation of the silicone resin is the same as in Example 1.

[0066] Preparation of soft magnetic alloy powder: The preparation of soft magnetic alloy powder in this embodiment differs from that in Example 1 in that the mass ratio of alloy powder to organosilicon resin is 1:0.003, while other conditions and parameters are the same as in Example 1.

[0067] Comparative Example 2:

[0068] Preparation of soft magnetic alloy powder: The preparation of soft magnetic alloy powder in this embodiment differs from that in Example 4 in that silicone resin was not used, while other conditions and parameters are the same as in Example 4.

[0069] Experimental Example 1:

[0070] Soft magnetic alloy powder was pressed and annealed to form a soft magnetic core at a pressure of 1200 MPa. The 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. Annealing was then performed, and 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 h, and then cooled to room temperature to obtain the ring-shaped soft magnetic core. Twenty turns of primary and secondary coils were uniformly wound onto the ring-shaped soft magnetic core for magnetic performance testing. The soft magnetic alloy powder used was the same as that prepared in Examples 1-6 and Comparative Examples 1-2.

[0071] The initial permeability was measured at 25℃, 100kHz, and a maximum magnetic flux density of 0.05T.

[0072] As shown in Figure 1, compared with Example 2, the initial permeability of the soft magnetic core made from the soft magnetic alloy powder prepared in Example 2 is higher than that in Example 1, indicating that increasing the amount of silicone resin coating within a certain range can improve the initial permeability of the soft magnetic alloy powder. Compared with Example 3, Example 1 shows that decreasing the amount of silicone resin coating within a certain range will inhibit the initial permeability of the soft magnetic core made from the soft magnetic alloy powder. Compared with Example 4, Example 1 shows that using polyethylene glycol maleimide co-coating on the basis of silicone resin can further improve the initial permeability of the soft magnetic core made from the soft magnetic alloy powder. Compared with Example 5, Example 4 shows that polyethylene glycol maleimide co-coating can further improve the initial permeability of the soft magnetic core made from the soft magnetic alloy powder. Increasing the amount of amine used within a certain range can improve the initial permeability of soft magnetic cores made from soft magnetic alloy powder. Compared with Example 6, Example 4 shows that reducing the amount of polyethylene glycol maleimide used within a certain range will suppress the initial permeability of soft magnetic cores made from soft magnetic alloy powder. Compared with Comparative Example 1, Example 1 shows that the amount of silicone resin used for coating needs to be within a suitable range; too low an amount will cause a decrease in the initial permeability of soft magnetic cores made from soft magnetic alloy powder. Compared with Comparative Example 2, Example 4 shows that silicone resin and polyethylene glycol maleimide need to be used together; polyethylene glycol maleimide alone has no significant effect on improving the initial permeability of soft magnetic cores made from soft magnetic alloy powder.

[0073] Experimental Example 2:

[0074] The core loss was measured at 25℃, 100kHz, and a maximum magnetic flux density of 0.05T. Other measurement conditions and methods were the same as in Experiment 1.

[0075] As shown in Figure 2, compared with Example 2, the core loss of the soft magnetic alloy powder prepared in Example 2 is lower than that in Example 1, indicating that increasing the amount of silicone resin used for coating within a certain range can reduce the core loss of the soft magnetic core made of soft magnetic alloy powder. Compared with Example 3, Example 1 shows that decreasing the amount of silicone resin used for coating within a certain range will increase the core loss of the soft magnetic core made of soft magnetic alloy powder. Compared with Example 4, Example 1 shows that using polyethylene glycol maleimide co-coating on the basis of silicone resin can further reduce the core loss of the soft magnetic core made of soft magnetic alloy powder. Compared with Example 5, Example 4 shows that polyethylene glycol maleimide co-coating can further reduce the core loss of the soft magnetic core made of soft magnetic alloy powder. Increasing the amount of amine used within a certain range can reduce the core loss of soft magnetic cores made of soft magnetic alloy powder. Example 4, compared to Example 6, shows that decreasing the amount of polyethylene glycol maleimide used within a certain range will also increase the core loss of soft magnetic cores made of soft magnetic alloy powder. Example 1, compared to Comparative Example 1, shows that the amount of silicone resin used for coating needs to be within a suitable range; too low a amount will increase the core loss of soft magnetic cores made of soft magnetic alloy powder. Example 4, compared to Comparative Example 2, shows that silicone resin and polyethylene glycol maleimide need to be used together; polyethylene glycol maleimide alone has no significant effect on reducing the core loss of soft magnetic cores made of soft magnetic alloy powder.

[0076] The embodiments and / or implementation methods described above are merely preferred embodiments and / or implementation methods for implementing the technology of the present invention, and are not intended to limit the implementation methods of the technology of the present invention in any way. Any person skilled in the art can make some modifications or alterations 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 the technology or embodiments that are substantially the same as the present invention.

[0077] This document uses specific examples to illustrate the principles and implementation methods of this application. The descriptions of the above embodiments are only for the purpose of helping to understand the methods and core ideas of this application. The above descriptions are only preferred embodiments of this application. It should be noted that due to the limitations of written expression, while there are objectively infinite specific structures, those skilled in the art can make several improvements, modifications, or changes without departing from the principles of this application, 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 situations without modification, should all be considered within the scope of protection of this application.

Claims

1. A method for preparing soft magnetic alloy powder, comprising: S1: Under an inert atmosphere, various raw materials are mixed, heated and melted into an alloy. The mixture is then heated to form mixed steam. The mixed steam is condensed and collected to obtain alloy powder. S2: Add the insulating material to the solvent, then add the alloy powder obtained in S1 and mix well, then dry to obtain soft magnetic alloy powder; the insulating material is an organosilicon resin; the organosilicon resin is prepared by reacting 4-(2,3-epoxypropoxy)carbazole, γ-piperazinylpropylmethyldimethoxysilane and 11-chloroundecanetriethoxysilane. The raw materials in S1 are iron, nickel, manganese, chromium, aluminum, and silicon; the mass ratio of iron to nickel is 1:1-2; the mass ratio of iron to manganese is 1:0.001-0.02; the mass ratio of iron to chromium is 1:0.001-0.02; the mass ratio of iron to aluminum is 1:0.001-0.02; and the mass ratio of iron to silicon is 1:0.001-0.

02. The mass ratio of alloy powder to insulating material used in S2 is 1:0.01-0.

12.

2. The method for preparing soft magnetic alloy powder according to claim 1, characterized in that, The solvent in S2 is acetone, and the ratio of insulating material to solvent is 1g:12-120ml.

3. A soft magnetic core comprising soft magnetic alloy powder prepared by any one of the methods described in claims 1-2.

4. An inductor comprising the soft magnetic core as described in claim 3.

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