A soft magnetic alloy powder and its preparation method and application

Abstract

The present invention discloses a soft magnetic alloy powder and a preparation method and application thereof, and relates to the technical field of magnetic materials. The specific preparation method comprises: firstly, in an inert atmosphere, various raw materials are mixed, heated and melted into an alloy, and then the mixed steam is obtained by further heating, and the mixed steam is condensed and collected to obtain the alloy powder; then, an organic silicone resin is used as an insulating material, the insulating material is added to a solvent, and then the alloy powder is added and mixed, and finally the soft magnetic alloy powder is obtained by drying. The method of the present invention has a simple process and a short production cycle, and the soft magnetic core made of the soft magnetic alloy powder prepared by the present invention has the advantages of high initial magnetic permeability and low magnetic core loss.

Description

Technical Field

[0001] The 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 development trend of electronic technology and the market, electronic devices are miniaturized, chip-type, high-frequency, and high-power density. The requirements for the performance and application characteristics of magnetic materials are constantly increasing. One-piece molded inductors have been widely used for their advantages such as high inductance, high current resistance, small magnetic leakage, and diversified sizes. Soft magnetic alloy powder is a powder material used to prepare magnetic cores. It is usually composed of an alloy of one or more metal elements, including iron, nickel, cobalt, and silicon. These metal elements are formed into a grain structure through a specific alloying process, including melting, mechanical alloying, vapor deposition, and electrochemical deposition. Soft magnetic alloy powder can be formed with the coil in one step to obtain an one-piece molded inductor. However, during the molding process, the inductor may cause the risk of interlayer short circuit due to the damage of the enameled wire after high-pressure molding. This requires the soft magnetic alloy powder to have high insulation withstand voltage characteristics to ensure that the inductor can withstand a certain high voltage and reduce the risk of short circuit of the one-piece molded inductor. At the same time, good insulation coating can also improve the stability of the magnetic properties of magnetic materials prepared from soft magnetic alloy powders, improve the magnetic permeability, and reduce the eddy current loss of magnetic materials. Patent CN105149574A discloses a method for coating iron-based soft magnetic alloy powder and a method for preparing soft magnetic composite materials, wherein the iron-based magnetic metal powder is oxidized at high temperature and then pickled to obtain an iron-based soft magnetic alloy powder with a surface coated with SiO2, Al2O3 or Cr2O3 oxide layer. However, when the oxidation temperature of the iron-based soft magnetic alloy powder is low, the oxidation effect will be poor. When the oxidation temperature is high, the particles are prone to sintering and adhesion during high-temperature sintering, resulting in increased losses. Therefore, the prior art urgently needs 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:

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

[0006] S1: In an inert atmosphere, various raw materials are mixed, heated and melted into an alloy, and further heated to form a mixed vapor, and the mixed vapor is condensed and collected to obtain alloy powder;

[0007] S2: Add the insulating material to the solvent, then add the alloy powder obtained in S1 and mix well, and then dry to obtain the 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 the reaction of 4-(2,3-epoxypropoxy)carbazole, γ-piperazinepropylmethyldimethoxysilane and 11-chloroundecanetriethoxysilane. The silicone resin has good high temperature resistance. The alloy powder is coated with the silicone resin, and it still has good adhesion and good insulation coating after annealing, so that the soft magnetic core made of the prepared soft magnetic alloy powder has 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 is 1:1-2.

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

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

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

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

[0014] Preferably, the solvent in S2 is acetone, and the usage ratio of the insulating material to the solvent is 1 g: 12-120 ml; the mass ratio of the alloy powder to the insulating material is 1: 0.01-0.12.

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

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

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

[0018] In an inert atmosphere, various raw materials are mixed, heated and melted into an alloy, and then heated to obtain mixed steam, which is condensed and collected to obtain alloy powder. Insulating materials are added to the solvent, followed by the alloy powder, and finally 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 is 1:1-2.

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

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

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

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

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

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

[0027] The present invention discloses a method for preparing an organosilicon resin, comprising:

[0028] 4-(2,3-epoxypropoxy)carbazole and γ-piperazinylpropylmethyldimethoxysilane are added to tetrahydrofuran, and reacted at 60-80°C for 18-28h to obtain an intermediate product. 11-Chloroundecanetriethoxysilane, tetramethylammonium hydroxide pentahydrate, water and tetrahydrofuran are added to the intermediate product, and reacted at 60-80°C for 18-28h. After the reaction is completed, the organic silicone resin is obtained by rotary evaporation, extraction, washing and drying.

[0029] Preferably, the mass ratio of 4-(2,3-epoxypropyloxy)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 used is 1 g: 10-20 ml.

[0031] Preferably, the mass ratio of the intermediate product to 11-chloroundecanetriethoxysilane 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 is 1:1.2-2.

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

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

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

[0037] More preferably, in the preparation of soft magnetic alloy powder, on the basis of using silicone resin, poly(ethylene glycol)-lactide-maleimide can also be used. The composite use of poly(ethylene glycol)-lactide-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.

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

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

[0040] The present invention proposes a soft magnetic alloy powder and a preparation method and application thereof. First, various raw materials are mixed, heated and melted into an alloy under an inert atmosphere, and the mixed steam is further heated to obtain a mixed steam, and the mixed steam is condensed and collected to obtain an alloy powder; then, an organic silicone resin is used as an insulating material, the insulating material is added to a solvent, and then the alloy powder is added and mixed, and finally the soft magnetic alloy powder is obtained by drying. The method of the present invention has a simple process and a short production cycle. Argon protection is used in the production process, and the soft magnetic alloy powder is not easily oxidized. The soft magnetic core made of the soft magnetic alloy powder prepared by the present invention has the advantages of high initial magnetic permeability and low magnetic core loss. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] In order to more clearly illustrate the implementation methods of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for the implementation methods or the description of the prior art. Obviously, the drawings in the following description are only exemplary, and for ordinary technicians in this field, other implementation drawings can be derived from the provided drawings without creative work.

[0042] Figure 1 This is the result diagram of the initial magnetic permeability measurement;

[0043] Figure 2 This is a graph showing the results of core loss measurement. DETAILED DESCRIPTION

[0044] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. 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 creative work are within the scope of protection of the present invention.

[0045] The following first describes the concepts involved in the present application in conjunction with the accompanying drawings. It should be noted that the following description of each concept is only to make the content of the present application easier to understand, and does not limit the scope of protection of the present application; at the same time, the embodiments and features in the embodiments of the present application can be combined with each other in the absence of conflict. The present application will be described in detail with reference to the accompanying drawings and in conjunction with the embodiments.

[0046] Embodiment 1:

[0047] Preparation of silicone resin: 4-(2,3-epoxypropoxy)carbazole and γ-piperazinylpropylmethyldimethoxysilane were added to tetrahydrofuran and reacted at 70°C for 20 hours to obtain an intermediate product. 11-Chloroundecanetriethoxysilane, tetramethylammonium hydroxide pentahydrate, water and tetrahydrofuran were added to the intermediate product and reacted at 70°C for 20 hours. After the reaction, the silicone resin was obtained by rotary evaporation, extraction with ethyl acetate and washing with saturated sodium chloride solution, and finally drying. The mass ratio of 4-(2,3-epoxypropoxy)carbazole to γ-piperazinepropylmethyldimethoxysilane is 1:1.16, the mass ratio 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 mass ratio of the intermediate product to tetrahydrofuran added to the intermediate product is 1g:6.82ml.

[0048] Preparation of soft magnetic alloy powder: In an argon atmosphere, iron, nickel, manganese, chromium, aluminum and silicon are mixed, heated and melted into an alloy, the alloy is further heated to obtain a mixed vapor, and the mixed vapor is condensed and collected to obtain an alloy powder. Silicone resin is added to acetone, and then the alloy powder is added and mixed, and finally dried at 60°C to obtain a 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, 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.

[0049] Embodiment 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 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.

[0052] Embodiment 3:

[0053] The preparation of 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 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.

[0055] Embodiment 4:

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

[0057] Preparation of soft magnetic alloy powder: In an argon atmosphere, iron, nickel, manganese, chromium, aluminum and silicon are mixed, heated and melted into an alloy, the alloy is further heated to obtain a mixed vapor, and the mixed vapor is condensed and collected to obtain an alloy powder. Silicone resin and poly(lactic acid) polyethylene glycol maleimide are added to acetone, and then the alloy powder is added and mixed, and finally dried at 60°C to obtain a 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, the mass ratio of iron to silicon is 1:0.01, the mass ratio of silicone resin to acetone is 1g:40ml, the mass ratio of alloy powder to silicone resin is 1:0.03, and the mass ratio of silicone resin to poly(lactic acid) polyethylene glycol maleimide is 1:0.67.

[0058] Embodiment 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 is compared with that in Example 4, except that the mass ratio of the amount of silicone resin to poly(lactide-glycol) polyethylene glycol maleimide used is 1:1.33, and other conditions and parameters are the same as in Example 4.

[0061] Embodiment 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 is compared with that in Example 4, except that the mass ratio of the amount of silicone resin to poly(ethylene glycol)-lactide-poly(ethylene glycol)-maleimide used is 1:0.5, and 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 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.

[0067] Comparative Example 2:

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

[0069] Experimental Example 1:

[0070] The soft magnetic alloy powder is pressed and annealed to form a soft magnetic core at a pressure of 1200MPa. The soft magnetic alloy powder is pressed into a ring sample with an outer diameter of 20mm, an inner diameter of 12mm, and a thickness of 5mm at a pressure of 1200MPa, and then annealed. The ring sample is heated to 500℃ at a rate of 5℃ / min in a nitrogen atmosphere, and then cooled to room temperature for 1 hour to obtain a ring-shaped soft magnetic core. Copper wire is used to evenly wind 20 turns of primary and secondary coils on the ring-shaped soft magnetic core, and the magnetic performance test can be performed. The soft magnetic alloy powder is the soft magnetic alloy powder prepared in Example 1-6 and Comparative Example 1-2.

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

[0072] The results are as follows Figure 1 As 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)-poly(ethylene glycol)-maleimide combined coating can further improve the initial magnetic permeability of the soft magnetic core made of the soft magnetic alloy powder; compared with Example 5, Example 4 shows that the use of poly(lactic acid)-poly(ethylene 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(lactide-ethylene 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(lactide-ethylene glycol) maleimide need to be used together, and poly(lactide-ethylene glycol) maleimide alone has no obvious effect on improving the initial magnetic permeability of the soft magnetic core made of soft magnetic alloy powder.

[0073] Experimental Example 2:

[0074] 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.

[0075] The results are as follows Figure 2 As 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 silicone resin 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 the reduction in the coating amount of silicone resin 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 on the basis of using silicone resin, the use of poly(lactic acid)-poly(ethylene glycol)-maleimide combined coating 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 the 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 usage of the silicone resin coating 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.

[0076] 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 are not intended to limit the implementation methods of the technology of the present invention in any form. Any technical personnel in this field 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.

[0077] 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 its 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 and the objective existence of infinite specific structures, ordinary technicians in this technical field 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 concept and technical solution of the invention 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, and further heated to form a mixed vapor, and the mixed vapor is 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 is an organic silicone resin; the organic silicone resin is prepared by reacting 4-(2,3-epoxypropoxy)carbazole, γ-piperazinepropylmethyldimethoxysilane 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; the mass ratio of iron to silicon is 1:0.001-0.02; The mass ratio of the alloy powder to the insulating material in S2 is 1:0.01-0.

12.

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

3. A soft magnetic core, comprising soft magnetic alloy powder prepared by the method according to any one of claims 1-2. An inductor comprising the soft magnetic core according to claim 3.

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