Low-loss superfine magnetically soft alloy powder and manufacturing method and application thereof

Abstract

The invention discloses low-loss superfine soft magnetic alloy powder and a manufacturing method and application thereof, belongs to the technical field of soft magnetic materials, and particularly relates to a method for preparing superfine alloy powder by smelting iron, nickel, manganese, aluminum, silicon and chromium into alloy and adopting an evaporation condensation method. Then coating the surface of the superfine alloy powder with a phosphating film by using a medium-temperature zinc-manganese phosphating solution and a phosphating auxiliary agent, and then coating with a silicon dioxide layer to obtain coated low-loss superfine soft magnetic alloy powder; wherein the phosphating auxiliary agent at least comprises a sodium sulfonate derivative, and in the preparation of the sodium sulfonate derivative, azelaic acid dichloride and 1-octylene-3-alcohol are subjected to a reaction, and then sodium hydrogen sulfite is added for a reaction to obtain the sodium sulfonate derivative. The D50 particle size of the prepared low-loss superfine magnetically soft alloy powder ranges from 100 nm to 3000 nm; the resistivity is high, and the resistivity reaches 9.0 omega.cm or above; and the power loss is low and is lower than 320.3 mW / cm < 3 >, and the method can be used for preparing a high-performance inductor.

Description

Technical Field

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

[0002] Ultrafine soft magnetic materials typically consist of metal magnetic powder and a surface insulating coating. Compared to traditional soft magnetic materials, they exhibit superior soft magnetic properties and lower power loss in the medium- to high-frequency range, as well as improved processability. Therefore, ultrafine soft magnetic materials are widely used in inductors, transformers, and electric drive devices. With the advancement of high-frequency and high-power electronic technology, the operating frequencies of electronic devices are increasing, and conventional soft magnetic materials are unable to meet these requirements. An effective solution is to apply an insulating coating to the magnetic powder to increase its resistivity, thereby reducing the power loss of ultrafine soft magnetic materials. Insulating coatings can be broadly categorized as organic and inorganic. Organic coatings are simple to process, but they generally have poor thermal stability and may decompose during annealing. Therefore, ultrafine soft magnetic materials produced after organic insulating coatings are typically annealed at lower temperatures, making it difficult to fully release the internal stress generated during the pressing process, making it difficult to obtain ultrafine soft magnetic materials with high effective permeability. Inorganic coatings are simple to process, but they can be difficult to achieve uniform and consistent coating across the channels. They are prone to cracking and even decomposition during annealing at higher temperatures, resulting in deterioration of soft magnetic properties. Therefore, a new method for manufacturing low-loss ultrafine soft magnetic alloy powder is needed to obtain low-loss ultrafine soft magnetic alloy powder with excellent soft magnetic properties. Summary of the Invention

[0003] The purpose of the present invention is to provide low-loss ultrafine soft magnetic alloy powder and its production method and application, so as to achieve the effect of increasing the resistivity of soft magnetic materials and reducing power loss.

[0004] The technical solutions adopted by the present invention to achieve the above-mentioned purpose are: A method for producing low-loss ultrafine soft magnetic alloy powder, comprising: S1. Iron, nickel, manganese, aluminum, silicon, and chromium are smelted into an alloy at high temperature, and the alloy is heated to boiling point by evaporation-condensation method, and then steam-cooled to obtain ultrafine alloy powder with a D50 particle size of 100-3000 nm; S2, first reacting the ultrafine alloy powder with a medium-temperature zinc-manganese phosphating solution and a phosphating aid, and then reacting with 3-aminopropyltriethoxysilane and ethyl orthosilicate to obtain a low-loss ultrafine soft magnetic alloy powder; The phosphating auxiliary agent at least includes a sodium sulfonate derivative, which has a sulfonic acid group, a benzene ring and a vinyl group.

[0005] The present invention melts iron, nickel, manganese, aluminum, silicon, and chromium into an alloy, and then obtains alloy powder through an evaporation and condensation method; then, the alloy powder is phosphated using a medium-temperature zinc-manganese phosphating solution and a phosphating auxiliary agent to form a phosphating layer on the surface of the alloy powder; and then, a silicon dioxide insulating layer is coated on the surface of the alloy powder using 3-aminopropyltriethoxysilane and ethyl orthosilicate. The phosphating auxiliary agent includes a sodium sulfonate derivative, and the sodium sulfonate derivative has a large number of hydrophilic groups. The sodium sulfonate derivative can enhance the wettability of the phosphating solution on the surface of the alloy powder, thereby not only ensuring the phosphating film forming speed and obtaining a better coating effect, but also improving the soft magnetic properties, thereby increasing the resistivity of the low-loss ultrafine soft magnetic alloy powder and reducing power loss.

[0006] Preferably, 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 aluminum is 1:0.001-0.02, the mass ratio of iron to silicon is 1:0.001-0.02, and the mass ratio of iron to chromium is 0.001-0.02.

[0007] Preferably, the mass concentration of the medium-temperature zinc-manganese phosphating solution is 5-10%, and the usage ratio of the ultrafine alloy powder to the medium-temperature zinc-manganese phosphating solution is 1 g: 1-2 mL.

[0008] Preferably, the usage ratio of the ultrafine alloy powder to 3-aminopropyltriethoxysilane is 1 g: 0.1-0.5 mL.

[0009] Preferably, the volume ratio of ethyl orthosilicate to 3-aminopropyltriethoxysilane is 1:2-10.

[0010] Preferably, in the preparation of the sodium sulfonate derivative, azelaic acid chloride and 1-octen-3-ol are first reacted, and then sodium bisulfite is added to react to obtain the sodium sulfonate derivative.

[0011] Preferably, the molar ratio of azelayl chloride to 1-octen-3-ol is 1:1-2.

[0012] Preferably, the molar ratio of azelayl chloride to sodium bisulfite is 1:1-2.

[0013] Preferably, the preparation of the sodium sulfonate derivative is specifically as follows: Weigh azelayl chloride, add dichloromethane and stir to dissolve, add 1-octen-3-ol and triethylamine, stir and react for 6-12 hours, add sodium carbonate solution to adjust the pH to neutral, add sodium bisulfite and deionized water, react at 120-160°C for 2-5 hours, add methanol, filter, rotary evaporate, and dry to obtain a sodium sulfonate derivative.

[0014] More preferably, the usage ratio of azelayl chloride to dichloromethane is 1 mol: 300-400 mL.

[0015] More preferably, the molar ratio of 1-octen-3-ol to azelaic acid chloride is 1:1-2.

[0016] More preferably, the molar ratio of triethylamine to azelayl chloride is 1:1-2.

[0017] More preferably, the molar ratio of azelayl chloride to sodium bisulfite is 1:1-2.

[0018] More preferably, the usage ratio of azelayl chloride to deionized water is 1 mol: 150-200 mL.

[0019] More preferably, the volume ratio of deionized water to methanol is 1:1-2.

[0020] Preferably, the production of low-loss ultrafine soft magnetic alloy powder is specifically as follows: S1. Iron, nickel, manganese, aluminum, silicon, and chromium are smelted into an alloy at high temperature, and the alloy is heated to boiling point by evaporation-condensation method, and then steam-cooled to obtain ultrafine alloy powder with a D50 particle size of 100-3000 nm; S2. At 50-60°C, add anhydrous ethanol to the ultrafine alloy powder prepared in step S1, stir at a speed of 400-600 r / min, add 3-aminopropyltriethoxysilane and deionized water, add ethyl orthosilicate, react at 40-60°C for 2-5 hours, wash with anhydrous ethanol 2-5 times, filter, and dry to obtain low-loss ultrafine soft magnetic alloy powder.

[0021] More preferably, the mass ratio of iron to nickel in step S1 is 1:1-2.

[0022] More preferably, the mass ratio of iron to manganese in step S1 is 1:0.001-0.02.

[0023] More preferably, in step S1, the mass ratio of iron to aluminum is 1:0.001-0.02.

[0024] More preferably, in step S1, the mass ratio of iron to silicon is 1:0.001-0.02.

[0025] More preferably, the mass ratio of iron to chromium in step S1 is 0.001-0.02.

[0026] More preferably, in step S2, the ratio of the ultrafine alloy powder to anhydrous ethanol is 1 g: 5-10 mL.

[0027] More preferably, in step S2, the volume ratio of 3-aminopropyltriethoxysilane to anhydrous ethanol is 1:30-40.

[0028] More preferably, in step S2, the volume ratio of 3-aminopropyltriethoxysilane to deionized water is 1:4-8.

[0029] More preferably, in step S2, the volume ratio of ethyl orthosilicate to 3-aminopropyltriethoxysilane is 1:3-7.

[0030] Preferably, the production of low-loss ultrafine soft magnetic alloy powder is specifically as follows: S1. Iron, nickel, manganese, aluminum, silicon, and chromium are smelted into an alloy at high temperature. The metal is heated to boiling point by evaporation-condensation method, and then steam-cooled to obtain ultrafine alloy powder with a D50 particle size of 100-3000 nm. S2. At 50-60°C, the ultrafine alloy powder prepared in step S1 is added to a medium-temperature zinc-manganese phosphating solution, stirred at a rate of 100-300 r / min for 10-30 min, allowed to stand for 5-15 min, filtered, rinsed with pure water 2-5 times, and then added with anhydrous ethanol. Stirred at a speed of 400-600 r / min, 3-aminopropyltriethoxysilane and deionized water were added, and ethyl orthosilicate was added. The mixture was reacted at 40-60°C for 2-5 h, washed with anhydrous ethanol for 2-5 times, filtered, and dried to obtain a low-loss ultrafine soft magnetic alloy powder.

[0031] More preferably, the mass ratio of iron to nickel in step S1 is 1:1-2.

[0032] More preferably, the mass ratio of iron to manganese in step S1 is 1:0.001-0.02.

[0033] More preferably, in step S1, the mass ratio of iron to aluminum is 1:0.001-0.02.

[0034] More preferably, in step S1, the mass ratio of iron to silicon is 1:0.001-0.02.

[0035] More preferably, the mass ratio of iron to chromium in step S1 is 0.001-0.02.

[0036] More preferably, the mass concentration of the medium-temperature zinc-manganese phosphating solution in step S2 is 5-10%, and the usage ratio of the ultrafine alloy powder to the medium-temperature zinc-manganese phosphating solution is 1 g: 1-2 mL.

[0037] More preferably, in step S2, the ratio of the ultrafine alloy powder to anhydrous ethanol is 1 g: 5-10 mL.

[0038] More preferably, in step S2, the volume ratio of 3-aminopropyltriethoxysilane to anhydrous ethanol is 1:30-40.

[0039] More preferably, in step S2, the volume ratio of 3-aminopropyltriethoxysilane to deionized water is 1:4-8.

[0040] More preferably, in step S2, the volume ratio of ethyl orthosilicate to 3-aminopropyltriethoxysilane is 1:3-7.

[0041] Preferably, the production of low-loss ultrafine soft magnetic alloy powder is specifically as follows: S1. Iron, nickel, manganese, aluminum, silicon, and chromium are smelted into an alloy at high temperature. The metal is heated to boiling point by evaporation-condensation method, and then steam-cooled to obtain ultrafine alloy powder with a D50 particle size of 100-3000 nm. S2. At 50-60°C, the ultrafine alloy powder prepared in step S1 is added to a medium-temperature zinc-manganese phosphating solution, a phosphating aid is added, and the mixture is stirred at a rate of 100-300 r / min for 10-30 min. The mixture is allowed to stand for 5-15 min, filtered, rinsed with pure water for 2-5 times, and then anhydrous ethanol is added. The mixture is stirred at a speed of 400-600 r / min, 3-aminopropyltriethoxysilane and deionized water are added, and ethyl orthosilicate is added. The mixture is reacted at 40-60°C for 2-5 h, washed with anhydrous ethanol for 2-5 times, filtered, and dried to obtain a low-loss ultrafine soft magnetic alloy powder.

[0042] More preferably, the mass ratio of iron powder to nickel powder in step S1 is 1:1-2.

[0043] More preferably, the mass ratio of iron to manganese in step S1 is 1:0.001-0.02.

[0044] More preferably, in step S1, the mass ratio of iron to aluminum is 1:0.001-0.02.

[0045] More preferably, in step S1, the mass ratio of iron to silicon is 1:0.001-0.02.

[0046] More preferably, the mass ratio of iron to chromium in step S1 is 0.001-0.02.

[0047] More preferably, the mass concentration of the medium-temperature zinc-manganese phosphating solution in step S2 is 5-10%, and the usage ratio of the ultrafine alloy powder to the medium-temperature zinc-manganese phosphating solution is 1 g: 1-2 mL.

[0048] More preferably, in step S2, the ratio of the ultrafine alloy powder to anhydrous ethanol is 1 g: 5-10 mL.

[0049] More preferably, in step S2, the volume ratio of 3-aminopropyltriethoxysilane to anhydrous ethanol is 1:30-40.

[0050] More preferably, in step S2, the volume ratio of 3-aminopropyltriethoxysilane to deionized water is 1:4-8.

[0051] More preferably, in step S2, the volume ratio of ethyl orthosilicate to 3-aminopropyltriethoxysilane is 1:3-7.

[0052] More preferably, the phosphating aid in step S2 includes a sodium sulfonate derivative, and the mass ratio of the ultrafine alloy powder to the sodium sulfonate derivative is 1:0.01-0.03.

[0053] Preferably, in the production of low-loss ultrafine soft magnetic alloy powder, the phosphating aids include sodium sulfonate derivatives and acyl phosphite derivatives, with the mass ratio of ultrafine alloy powder to sodium sulfonate derivative being 1:0.01-0.03, and the mass ratio of ultrafine alloy powder to acyl phosphite derivative being 1:0.005-0.02. Acyl phosphite derivatives improve the stability of the phosphating solution, forming a highly effective phosphating layer, thereby optimizing the soft magnetic properties of the low-loss ultrafine soft magnetic alloy powder, further increasing its resistivity and reducing power loss.

[0054] More preferably, the preparation of the acylphospholipid derivative is specifically, Take phosphoethanolamine, add isobutyric anhydride under vacuum at 40-60°C, stir evenly, react at 80-100°C for 2-5 hours, add diethanolamine, react at 90-100°C for 6-12 hours to obtain an acyl phosphoester derivative.

[0055] More preferably, the usage ratio of isobutyric anhydride to phosphoethanolamine is 1 mL: 1-5 g.

[0056] More preferably, the mass ratio of diethanolamine to phosphoethanolamine is 1:0.5-1.0.

[0057] The invention also discloses low-loss ultrafine soft magnetic alloy powder prepared by the method.

[0058] The invention also discloses the application of low-loss ultrafine soft magnetic alloy powder in the preparation of high-performance inductors.

[0059] The invention uses iron, nickel, manganese, aluminum, silicon, and chromium to prepare alloy powder, adopts sodium sulfonate derivatives and acyl phosphite derivatives as phosphating aids to participate in the phosphating action of a medium-temperature zinc-manganese phosphating solution to assist, and forms a phosphating layer on the surface of the alloy powder; then uses 3-aminopropyltriethoxysilane and ethyl orthosilicate to coat the surface of the alloy powder with a silicon dioxide insulating layer, and produces low-loss ultrafine soft magnetic alloy powder. The invention has the following beneficial effects: the low-loss ultrafine soft magnetic alloy powder produced by the invention has a small D50 particle size of 100-3000 nm; a high resistivity of 9.0-18.2 Ω·cm; and a low power loss of 282.3-320.3 mW / cm 3, which can be used to prepare high-performance inductors. Therefore, the present invention discloses a low-loss ultrafine soft magnetic alloy powder with high resistivity and low power loss, and a manufacturing method and application thereof. BRIEF DESCRIPTION OF THE DRAWINGS

[0060] Figure 1 This is the SEM image of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1.

[0061] Figure 2 This is the iron element distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1.

[0062] Figure 3 Nickel element distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1.

[0063] Figure 4 This is the manganese element distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1.

[0064] Figure 5 This is the silicon element distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1.

[0065] Figure 6 This is the oxygen element distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1. DETAILED DESCRIPTION

[0066] The present invention will be further described in detail below in conjunction with specific embodiments. The examples provided are only for illustrating the present invention and are not intended to limit the scope of the present invention. The examples provided below can serve as a guide for further improvements by those skilled in the art and are not intended to limit the present invention in any way.

[0067] The experimental methods in the following examples are conventional methods unless otherwise specified. The materials and reagents used in the following examples are commercially available unless otherwise specified.

[0068] Example 1: Manufacturing of low-loss ultrafine soft magnetic alloy powders, including, S1. Iron, nickel, manganese, aluminum, silicon, and chromium are smelted into an alloy at high temperature. The metals are heated to boiling point using the evaporation-condensation method, and then steam-cooled to obtain an ultrafine alloy powder with a D50 particle size of 750 nm. 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 aluminum is 1:0.01; the mass ratio of iron to silicon is 1:0.01; and the mass ratio of iron to chromium is 0.01. S2. At 55°C, add anhydrous ethanol to the ultrafine alloy powder prepared in step S1, stir at 500 r / min, add 3-aminopropyltriethoxysilane and deionized water, add ethyl orthosilicate, react at 50°C for 3 hours, wash three times with anhydrous ethanol, filter, and dry to obtain low-loss ultrafine soft magnetic alloy powder. The ratio of ultrafine alloy powder to anhydrous ethanol is 1g:8.5mL; the volume ratio of 3-aminopropyltriethoxysilane to anhydrous ethanol is 1:34; the volume ratio of 3-aminopropyltriethoxysilane to deionized water is 1:6; and the volume ratio of ethyl orthosilicate to 3-aminopropyltriethoxysilane is 1:5.

[0069] Example 2: Manufacturing of low-loss ultrafine soft magnetic alloy powders, including, S1. Iron, nickel, manganese, aluminum, silicon, and chromium are smelted into an alloy at high temperature. The metals are heated to boiling point using the evaporation-condensation method, and then steam-cooled to obtain an ultrafine alloy powder with a D50 particle size of 750 nm. 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 aluminum is 1:0.01; the mass ratio of iron to silicon is 1:0.01; and the mass ratio of iron to chromium is 0.01. S2. At 55°C, the ultrafine alloy powder prepared in step S1 was added to a medium-temperature zinc-manganese phosphating solution, stirred at a rate of 200 r / min for 20 min, allowed to stand for 5 min, filtered, rinsed with pure water three times, and then added with anhydrous ethanol. The mixture was stirred at a speed of 500 r / min, 3-aminopropyltriethoxysilane and deionized water were added, and ethyl orthosilicate was added. The mixture was reacted at 50°C for 3 h, washed with anhydrous ethanol three times, filtered, and dried to obtain low-loss ultrafine soft magnetic alloy powder. Medium-temperature zinc-manganese phosphating solution was purchased from Beijing Ailsmu Technology Co., Ltd. The mass concentration of the medium-temperature zinc-manganese phosphating solution was 10%, the amount ratio of ultrafine alloy powder to medium-temperature zinc-manganese phosphating solution was 1 g:1 mL; the amount ratio of ultrafine alloy powder to anhydrous ethanol was 1 g:8.5 mL; the volume ratio of 3-aminopropyltriethoxysilane to anhydrous ethanol was 1:34; the volume ratio of 3-aminopropyltriethoxysilane to deionized water was 1:6; and the volume ratio of ethyl orthosilicate to 3-aminopropyltriethoxysilane was 1:5.

[0070] Example 3: Preparation of sodium sulfonate derivatives, comprising: Weigh azelayl chloride, add dichloromethane, and stir to dissolve. Then, add 1-octen-3-ol and triethylamine, stir and react for 8 hours. Then, add sodium carbonate solution to adjust the pH to neutral. Then, add sodium bisulfite and deionized water, react at 140°C for 3 hours, add methanol, filter, rotary evaporate, and dry to obtain the sodium sulfonate derivative. The molar ratio of azelayl chloride to dichloromethane is 1 mol:350 mL; the molar ratio of 1-octen-3-ol to azelayl chloride is 1:1.5; the molar ratio of triethylamine to azelayl chloride is 1:1.5; the molar ratio of azelayl chloride to sodium bisulfite is 1:1; the molar ratio of azelayl chloride to deionized water is 1 mol:180 mL; and the volume ratio of deionized water to methanol is 1:1.

[0071] Manufacturing of low-loss ultrafine soft magnetic alloy powders, including, S1. Iron, nickel, manganese, aluminum, silicon, and chromium are smelted into an alloy at high temperature. The metals are heated to boiling point using the evaporation-condensation method, and then steam-cooled to obtain an ultrafine alloy powder with a D50 particle size of 750 nm. 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 aluminum is 1:0.01; the mass ratio of iron to silicon is 1:0.01; and the mass ratio of iron to chromium is 0.01. S2. At 55°C, the ultrafine alloy powder prepared in step S1 is added to a medium-temperature zinc-manganese phosphating solution, and a sodium sulfonate derivative is added. The mixture is stirred at a rate of 200 r / min for 20 minutes, allowed to stand for 5 minutes, filtered, rinsed with pure water three times, and then anhydrous ethanol is added. The mixture is stirred at a speed of 500 r / min, 3-aminopropyltriethoxysilane and deionized water are added, and ethyl orthosilicate is added. The mixture is reacted at 50°C for 3 hours, washed with anhydrous ethanol three times, filtered, and dried to obtain a low-loss ultrafine soft magnetic alloy powder. Medium-temperature zinc-manganese phosphating solution was purchased from Beijing Ailsmu Technology Co., Ltd. The mass concentration of the medium-temperature zinc-manganese phosphating solution was 10%, the amount ratio of ultrafine alloy powder and medium-temperature zinc-manganese phosphating solution was 1 g:1 mL; the mass ratio of ultrafine alloy powder and sodium sulfonate derivative was 1:0.03; the amount ratio of ultrafine alloy powder and anhydrous ethanol was 1 g:8.5 mL; the volume ratio of 3-aminopropyltriethoxysilane and anhydrous ethanol was 1:34; the volume ratio of 3-aminopropyltriethoxysilane and deionized water was 1:6; and the volume ratio of ethyl orthosilicate and 3-aminopropyltriethoxysilane was 1:5.

[0072] Example 4: The only difference between this embodiment and embodiment 3 is the production of low-loss ultrafine soft magnetic alloy powder.

[0073] In this embodiment, except that the mass ratio of the ultrafine alloy powder to the sodium sulfonate salt derivative is changed to 1:0.01 in the production of the low-loss ultrafine soft magnetic alloy powder, other conditions are the same as those of Example 3.

[0074] Example 5: Preparation of acylphospholipid derivatives, comprising: To phosphoethanolamine, add isobutyric anhydride under vacuum at 50°C, stir evenly, and react at 90°C for 3 hours. Add diethanolamine and react at 95°C for 8 hours to obtain an acylphosphoester derivative. The ratio of isobutyric anhydride to phosphoethanolamine is 1 mL:2 g; the mass ratio of diethanolamine to phosphoethanolamine is 1:0.65.

[0075] Preparation of sodium sulfonate derivatives, comprising: Weigh azelayl chloride, add dichloromethane, and stir to dissolve. Then, add 1-octen-3-ol and triethylamine, stir and react for 8 hours. Then, add sodium carbonate solution to adjust the pH to neutral. Then, add sodium bisulfite and deionized water, react at 140°C for 3 hours, add methanol, filter, rotary evaporate, and dry to obtain the sodium sulfonate derivative. The molar ratio of azelayl chloride to dichloromethane is 1 mol:350 mL; the molar ratio of 1-octen-3-ol to azelayl chloride is 1:1.5; the molar ratio of triethylamine to azelayl chloride is 1:1.5; the molar ratio of azelayl chloride to sodium bisulfite is 1:1; the molar ratio of azelayl chloride to deionized water is 1 mol:180 mL; and the volume ratio of deionized water to methanol is 1:1.

[0076] Manufacturing of low-loss ultrafine soft magnetic alloy powders, including, S1. Iron, nickel, manganese, aluminum, silicon, and chromium are smelted into an alloy at high temperature. The metals are heated to boiling point using the evaporation-condensation method, and then steam-cooled to obtain an ultrafine alloy powder with a D50 particle size of 750 nm. 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 aluminum is 1:0.01; the mass ratio of iron to silicon is 1:0.01; and the mass ratio of iron to chromium is 0.01. S2. At 55°C, the ultrafine alloy powder prepared in step S1 is added to a medium-temperature zinc-manganese phosphating solution, and acyl phosphite derivatives and sodium sulfonate derivatives are added. The mixture is stirred at a rate of 200 r / min for 20 minutes, allowed to stand for 5 minutes, filtered, rinsed with pure water three times, and then anhydrous ethanol is added. The mixture is stirred at a speed of 500 r / min, 3-aminopropyltriethoxysilane and deionized water are added, and ethyl orthosilicate is added. The mixture is reacted at 50°C for 3 hours, washed with anhydrous ethanol three times, filtered, and dried to obtain low-loss ultrafine soft magnetic alloy powder. Medium-temperature zinc-manganese phosphating solution was purchased from Beijing Ailsmu Technology Co., Ltd. The mass concentration of the medium-temperature zinc-manganese phosphating solution was 10%, the amount ratio of ultrafine alloy powder to medium-temperature zinc-manganese phosphating solution was 1 g:1 mL; the mass ratio of ultrafine alloy powder to sodium sulfonate derivative was 1:0.03; the mass ratio of ultrafine alloy powder to acyl phosphide derivative was 1:0.02; the amount ratio of ultrafine alloy powder to anhydrous ethanol was 1 g:8.5 mL; the volume ratio of 3-aminopropyltriethoxysilane to anhydrous ethanol was 1:34; the volume ratio of 3-aminopropyltriethoxysilane to deionized water was 1:6; and the volume ratio of ethyl orthosilicate to 3-aminopropyltriethoxysilane was 1:5.

[0077] Example 6: The only difference between this embodiment and embodiment 5 is the production of low-loss ultrafine soft magnetic alloy powder.

[0078] In this embodiment, except that the mass ratio of the ultrafine alloy powder to the acyl phosphide derivative is changed to 1:0.005 in the production of the low-loss ultrafine soft magnetic alloy powder, other conditions are the same as those in Example 5.

[0079] Comparative Example 1: The only difference between this comparative example and Example 4 is the production of low-loss ultrafine soft magnetic alloy powder.

[0080] This embodiment is similar to the embodiment 4 except that no sodium sulfonate derivative is added in the production of the low-loss ultrafine soft magnetic alloy powder.

[0081] Experimental example: 1. Material characterization The surface morphology of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1 was observed using a scanning electron microscope, and element distribution analysis was performed using an electron probe provided in the electron microscope.

[0082] Figure 1 This is an SEM image of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1, with a scale of 100 nm. The low-loss ultrafine soft magnetic alloy powder prepared in Example 1 is in the form of round particles with a smooth surface covered with a protective layer. Figure 2 The iron element distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1, with a scale of 100 nm; Figure 3 The nickel element distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1 is shown in FIG. 1 , with a scale of 100 nm. Figure 4 The manganese element distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1, the scale is 100 nm; Figure 5 The silicon element distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1 is shown in FIG. 1 , with a scale of 100 nm. Figure 6 The oxygen element distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1, the scale is 100nm; iron, nickel, manganese, silicon and oxygen elements are evenly distributed on the surface of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1, which indicates that the low-loss ultrafine soft magnetic alloy powder prepared in Example 1 of the present invention is effectively coated with a silicon dioxide protective layer.

[0083] 2. Resistivity The resistivity (Ω·cm) of the low-loss ultrafine soft magnetic alloy powders prepared in Examples 1-6 and Comparative Example 1 was measured using a four-probe method. Resistivity (Ω·cm) = (cross-sectional area × voltage across a standard resistor × resistance of the standard resistor) / (voltage across the low-loss ultrafine soft magnetic alloy powder × distance). The resistivity measurement results are shown in Table 1.

[0084] Table 1 Resistivity (Ω·cm)

[0085] As can be seen from Table 1, the resistivity of Example 2 of the present invention is higher than that of Example 1. This is because, in the manufacture of low-loss ultrafine soft magnetic alloy powder, Example 2 first uses a medium-temperature zinc-manganese phosphating solution for phosphating treatment and then coats the silicon dioxide layer, while Example 1 does not use a medium-temperature zinc-manganese phosphating solution for phosphating treatment; the resistivity of Examples 3-4 is higher than that of Example 2. This is because, in the manufacture of low-loss ultrafine soft magnetic alloy powder, Examples 3-4 use sodium sulfonate derivatives, while Example 2 does not use sodium sulfonate derivatives; the resistivity of Example 3 is higher than that of Example 4 because the amount of sodium sulfonate derivatives used in the manufacture of low-loss ultrafine soft magnetic alloy powder is different. This shows that in the manufacture of low-loss ultrafine soft magnetic alloy powder, using an appropriate amount of sodium sulfonate derivatives to assist the phosphating effect of the medium-temperature zinc-manganese phosphating solution can improve the resistivity of the low-loss ultrafine soft magnetic alloy powder.

[0086] The higher resistivity of Examples 5-6 of the present invention than that of Example 3 and Comparative Example 1 is due to the coordinated use of acyl phosphide derivatives and sodium sulfonate derivatives in the production of the low-loss ultrafine soft magnetic alloy powder in Examples 5-6, while Example 3 only used sodium sulfonate derivatives and Comparative Example 1 only used acyl phosphide derivatives. The higher resistivity of Example 5 than in Example 6 is due to the different amounts of acyl phosphide derivatives used in the production of the low-loss ultrafine soft magnetic alloy powder. This suggests that the coordinated use of acyl phosphide derivatives and sodium sulfonate derivatives to assist in the phosphating process of a medium-temperature zinc-manganese phosphating solution in the production of the low-loss ultrafine soft magnetic alloy powder can further improve the resistivity of the low-loss ultrafine soft magnetic alloy powder.

[0087] 3. Power loss The power loss of the low-loss ultrafine soft magnetic alloy powders prepared in Examples 1-6 and Comparative Example 1 was measured at 50 kHz / 50 mT using a SY-8232B-H analyzer. The measurement results are shown in Table 2.

[0088] Table 2 Power loss (mW / cm 3 )

[0089] As can be seen from Table 2, the power loss of Example 2 of the present invention is lower than that of Example 1. This is because, in the manufacture of low-loss ultrafine soft magnetic alloy powder, Example 2 first uses a medium-temperature zinc-manganese phosphating solution for phosphating treatment and then coats the silicon dioxide layer, while Example 1 does not use a medium-temperature zinc-manganese phosphating solution for phosphating treatment; the power loss of Examples 3-4 is lower than that of Example 2. This is because, in the manufacture of low-loss ultrafine soft magnetic alloy powder, Examples 3-4 use sodium sulfonate derivatives, while Example 2 does not use sodium sulfonate derivatives; the power loss of Example 3 is lower than that of Example 4. This is because the amount of sodium sulfonate derivatives used in the manufacture of low-loss ultrafine soft magnetic alloy powder is different. This shows that in the manufacture of low-loss ultrafine soft magnetic alloy powder, using an appropriate amount of acyl phosphite derivatives to assist the phosphating effect of the medium-temperature zinc-manganese phosphating solution can reduce the power loss of the low-loss ultrafine soft magnetic alloy powder.

[0090] The power loss of Examples 5-6 of the present invention is lower than that of Example 3 and Comparative Example 1 because, in the production of low-loss ultrafine soft magnetic alloy powder, Examples 5-6 synergistically use acyl phosphoester derivatives and sodium sulfonate derivatives, while Example 3 only uses sodium sulfonate derivatives and Comparative Example 1 only uses acyl phosphoester derivatives. The power loss of Example 5 is lower than that of Example 6 because the amount of acyl phosphoester derivative used in the production of low-loss ultrafine soft magnetic alloy powder is different. This shows that in the production of low-loss ultrafine soft magnetic alloy powder, the synergistic use of acyl phosphoester derivatives and sodium sulfonate derivatives to assist the phosphating action of the medium-temperature zinc-manganese phosphating solution can further reduce the power loss of the low-loss ultrafine soft magnetic alloy powder.

[0091] The conventional operations in the operating steps of the present invention are well known to those skilled in the art and will not be described in detail here.

[0092] The embodiments described above provide a detailed description of the technical solutions of the present invention. It should be understood that the above are only specific embodiments of the present invention and are not intended to limit the present invention. Any modifications, supplements or similar substitutions made within the scope of the principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A method for producing low-loss ultrafine soft magnetic alloy powder, comprising: S1. Iron, nickel, manganese, aluminum, silicon, and chromium are smelted into an alloy at high temperature, and the alloy is heated to boiling point by evaporation-condensation method, and then steam-cooled to obtain ultrafine alloy powder with a D50 particle size of 100-3000 nm; S2, first reacting the ultrafine alloy powder with a medium-temperature zinc-manganese phosphating solution and a phosphating aid, and then reacting with 3-aminopropyltriethoxysilane and ethyl orthosilicate to obtain a low-loss ultrafine soft magnetic alloy powder; The phosphating auxiliary agent at least includes a sodium sulfonate derivative, and the sodium sulfonate derivative has a sulfonic acid group, a benzene ring and a vinyl group.

2. The method for producing low-loss ultrafine soft magnetic alloy powder according to claim 1, characterized in that: 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 aluminum is 1:0.001-0.02, the mass ratio of iron to silicon is 1:0.001-0.02, and the mass ratio of iron to chromium is 0.001-0.

02.

3. The method for producing low-loss ultrafine soft magnetic alloy powder according to claim 1, characterized in that: The mass concentration of the medium-temperature zinc-manganese phosphating solution is 5-10%, and the usage ratio of the ultrafine alloy powder to the medium-temperature zinc-manganese phosphating solution is 1g:1-2mL.

4. The method for producing low-loss ultrafine soft magnetic alloy powder according to claim 1, characterized in that: The usage ratio of the ultrafine alloy powder and 3-aminopropyltriethoxysilane is 1g:0.1-0.5mL.

5. The method for producing low-loss ultrafine soft magnetic alloy powder according to claim 1, characterized in that: The volume ratio of the ethyl orthosilicate to 3-aminopropyltriethoxysilane is 1:2-10.

6. The method for producing low-loss ultrafine soft magnetic alloy powder according to claim 1, characterized in that: In the preparation of the sodium sulfonate derivative, azelaic acid chloride and 1-octen-3-ol are first reacted, and then sodium bisulfite is added to react to obtain the sodium sulfonate derivative.

7. The method for producing low-loss ultrafine soft magnetic alloy powder according to claim 6, characterized in that: The molar ratio of azelayl chloride to 1-octen-3-ol is 1:1-2.

8. The method for producing low-loss ultrafine soft magnetic alloy powder according to claim 6, characterized in that: The molar ratio of azelayl chloride to sodium bisulfite is 1:1-2.

9. The low-loss ultrafine soft magnetic alloy powder prepared by the method according to any one of claims 1 to 8.

10. Use of the low-loss ultrafine soft magnetic alloy powder according to claim 9 in preparing high-performance inductors.

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