Low-loss ultra-fine soft magnetic alloy powder, and manufacturing method therefor and use thereof

Abstract

The present invention belongs to the technical field of soft magnetic materials, and discloses a low-loss ultra-fine soft magnetic alloy powder, and a manufacturing method therefor and the use thereof. Specifically, the manufacturing method comprises: smelting iron, nickel, manganese, aluminum, silicon and chromium into an alloy, and preparing an ultra-fine alloy powder by means of an evaporation-condensation method; and coating the surface of the ultra-fine alloy powder with a phosphating film by using a medium-temperature zinc-manganese-based phosphating solution and a phosphating aid, and subsequently coating same with a silicon dioxide layer to obtain a coated low-loss ultra-fine soft magnetic alloy powder, wherein the phosphating aid at least comprises a sodium sulfonate derivative. During the preparation of the sodium sulfonate derivative, nonanedioyl chloride and 1-octen-3-ol are first reacted, and then sodium bisulfite is added for a further reaction, so as to obtain the sodium sulfonate derivative. The low-loss ultra-fine soft magnetic alloy powder prepared in the present invention has a D50 particle size of 100-3000 nm, a high resistivity of up to 9.0 Ω·cm or more, and a low power loss below 320.3 mW / cm3, and can thus be used for preparing a high-performance inductor.

Description

Low-loss ultrafine soft magnetic alloy powder, its manufacturing method and application Technical Field

[0001] This invention relates to the field of soft magnetic materials technology, specifically to low-loss ultrafine soft magnetic alloy powder, its manufacturing method, and its applications. Background Technology

[0002] Ultrafine soft magnetic materials are typically composed of metallic magnetic powder and a surface insulating coating medium. Compared to traditional soft magnetic materials, they exhibit better soft magnetic properties and lower power loss in the mid-to-high frequency range, and also possess better processability. Therefore, ultrafine soft magnetic materials are widely used in inductors, transformers, and electric drive devices. With the development of high-frequency and high-power electronic technology, the operating frequency of electronic devices is gradually increasing, and ordinary soft magnetic materials can no longer meet the requirements. An effective solution is to improve the resistivity by insulating the magnetic powder, thereby reducing the power loss of ultrafine soft magnetic materials. Insulating coating can be broadly classified into organic coating and inorganic coating. Organic coating media have a simple coating process, but they usually have poor thermal stability and may decompose during annealing. Therefore, ultrafine soft magnetic materials obtained after organic insulating coating treatment typically have a low annealing temperature, and the internal stress generated during the pressing process is difficult to completely release, making it difficult to obtain ultrafine soft magnetic materials with high effective permeability. Inorganic coating media are simple to operate, but the channels are difficult to coat uniformly, and they are prone to cracking and detachment during annealing at higher temperatures, or even decomposition, leading to a 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 this invention is to provide low-loss ultrafine soft magnetic alloy powder, its manufacturing method and application, so as to improve the resistivity of soft magnetic materials and reduce power loss.

[0004] The technical solution adopted by the present invention to achieve the above objectives is as follows:

[0005] A method for manufacturing low-loss ultrafine soft magnetic alloy powder, including,

[0006] S1. Iron, nickel, manganese, aluminum, silicon and chromium are smelted into an alloy at high temperature. The alloy is heated to the boiling point by evaporation and condensation method, and then cooled by steam to obtain ultrafine alloy powder with a D50 particle size of 100-3000nm.

[0007] S2. The ultrafine alloy powder is first reacted with a medium-temperature zinc-manganese phosphating solution and phosphating aid, and then reacted with 3-aminopropyltriethoxysilane and tetraethyl orthosilicate to obtain low-loss ultrafine soft magnetic alloy powder.

[0008] Phosphating auxiliaries include at least sodium sulfonate derivatives, which have sulfonic acid groups, benzene rings, and vinyl groups.

[0009] This invention involves smelting iron, nickel, manganese, aluminum, silicon, and chromium into an alloy, and then obtaining alloy powder through an evaporation and condensation method. The alloy powder is then phosphated using a medium-temperature zinc-manganese phosphate solution and phosphate auxiliaries to form a phosphate layer on its surface. A silicon dioxide insulating layer is then coated onto the alloy powder surface using 3-aminopropyltriethoxysilane and tetraethyl orthosilicate. The phosphate auxiliaries include sodium sulfonate derivatives. These derivatives possess numerous hydrophilic groups, which enhance the wetting properties of the phosphate solution on the alloy powder surface. This not only ensures a faster phosphate film formation rate and achieves better coating, but also improves soft magnetic properties, thereby increasing the resistivity of the low-loss ultrafine soft magnetic alloy powder and reducing power loss.

[0010] 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.

[0011] Preferably, the mass concentration of the medium-temperature zinc-manganese phosphating solution is 5-10%, and the ratio of ultrafine alloy powder to medium-temperature zinc-manganese phosphating solution is 1g:1-2mL.

[0012] Preferably, the ratio of ultrafine alloy powder to 3-aminopropyltriethoxysilane is 1g:0.1-0.5mL.

[0013] Preferably, the volume ratio of tetraethyl orthosilicate to 3-aminopropyltriethoxysilane is 1:2-10.

[0014] Preferably, in the preparation of sodium sulfonate derivatives, azeloyl chloride and 1-octen-3-ol are reacted first, and then sodium bisulfite is added to react and obtain sodium sulfonate derivatives.

[0015] Preferably, the molar ratio of azeloyl chloride to 1-octen-3-ol is 1:1-2.

[0016] Preferably, the molar ratio of azeloyl chloride to sodium bisulfite is 1:1-2.

[0017] Preferably, the preparation of the sodium sulfonate derivative specifically involves,

[0018] Weigh azeloyl chloride, add dichloromethane and stir to dissolve, add 1-octen-3-ol and triethylamine, stir to react for 6-12 h, add sodium carbonate solution to adjust pH to neutral, add sodium bisulfite and deionized water, react at 120-160℃ for 2-5 h, add methanol, filter, rotary evaporate, dry to obtain sodium sulfonate derivative.

[0019] More preferably, the ratio of azeloyl chloride to dichloromethane is 1 mol: 300-400 mL.

[0020] More preferably, the molar ratio of 1-octen-3-ol to azeloyl chloride is 1:1-2.

[0021] More preferably, the molar ratio of triethylamine to azeloyl chloride is 1:1-2.

[0022] More preferably, the molar ratio of azeloyl chloride to sodium bisulfite is 1:1-2.

[0023] More preferably, the ratio of azeloyl chloride to deionized water is 1 mol: 150-200 mL.

[0024] More preferably, the volume ratio of deionized water to methanol is 1:1-2.

[0025] Preferably, the manufacturing of low-loss ultrafine soft magnetic alloy powder specifically involves:

[0026] S1. Iron, nickel, manganese, aluminum, silicon and chromium are smelted into an alloy at high temperature. The alloy is heated to the boiling point by evaporation and condensation method, and then cooled by steam to obtain ultrafine alloy powder with a D50 particle size of 100-3000nm.

[0027] S2. Under conditions of 50-60℃, anhydrous ethanol is added to the ultrafine alloy powder prepared in step S1, and the mixture is stirred at a speed of 400-600 r / min. 3-Aminopropyltriethoxysilane and deionized water are added, followed by tetraethyl orthosilicate. The mixture is reacted at 40-60℃ for 2-5 h, washed 2-5 times with anhydrous ethanol, filtered, and dried to obtain low-loss ultrafine soft magnetic alloy powder.

[0028] More preferably, the mass ratio of iron to nickel in step S1 is 1:1-2.

[0029] More preferably, the mass ratio of iron to manganese in step S1 is 1:0.001-0.02.

[0030] More preferably, the mass ratio of iron to aluminum in step S1 is 1:0.001-0.02.

[0031] More preferably, the mass ratio of iron to silicon in step S1 is 1:0.001-0.02.

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

[0033] More preferably, in step S2, the ratio of ultrafine alloy powder to anhydrous ethanol is 1g:5-10mL.

[0034] More preferably, in step S2, the volume ratio of 3-aminopropyltriethoxysilane to anhydrous ethanol is 1:30-40.

[0035] More preferably, in step S2, the volume ratio of 3-aminopropyltriethoxysilane to deionized water is 1:4-8.

[0036] More preferably, in step S2, the volume ratio of tetraethyl orthosilicate to 3-aminopropyltriethoxysilane is 1:3-7.

[0037] Preferably, the manufacturing of low-loss ultrafine soft magnetic alloy powder specifically involves:

[0038] S1. Iron, nickel, manganese, aluminum, silicon and chromium are smelted into an alloy at high temperature. The metal is heated to the boiling point by evaporation and condensation, and then cooled by steam to obtain ultrafine alloy powder with a D50 particle size of 100-3000nm.

[0039] S2. Under conditions of 50-60℃, the ultrafine alloy powder prepared in step S1 is added to a medium-temperature zinc-manganese phosphating solution and stirred at a rate of 100-300 r / min for 10-30 min. After standing for 5-15 min, the mixture is filtered, rinsed with pure water 2-5 times, and then anhydrous ethanol is added. The mixture is stirred at a speed of 400-600 r / min, and then 3-aminopropyltriethoxysilane and deionized water are added. Tetraethyl orthosilicate is added, and the mixture is reacted at 40-60℃ for 2-5 h. After washing with anhydrous ethanol 2-5 times, the mixture is filtered and dried to obtain low-loss ultrafine soft magnetic alloy powder.

[0040] More preferably, the mass ratio of iron to nickel in step S1 is 1:1-2.

[0041] More preferably, the mass ratio of iron to manganese in step S1 is 1:0.001-0.02.

[0042] More preferably, the mass ratio of iron to aluminum in step S1 is 1:0.001-0.02.

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

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

[0045] More preferably, in step S2, the mass concentration of the medium-temperature zinc-manganese phosphating solution is 5-10%, and the ratio of ultrafine alloy powder to medium-temperature zinc-manganese phosphating solution is 1g:1-2mL.

[0046] More preferably, in step S2, the ratio of ultrafine alloy powder to anhydrous ethanol is 1g:5-10mL.

[0047] More preferably, in step S2, the volume ratio of 3-aminopropyltriethoxysilane to anhydrous ethanol is 1:30-40.

[0048] More preferably, in step S2, the volume ratio of 3-aminopropyltriethoxysilane to deionized water is 1:4-8.

[0049] More preferably, in step S2, the volume ratio of tetraethyl orthosilicate to 3-aminopropyltriethoxysilane is 1:3-7.

[0050] Preferably, the manufacturing of low-loss ultrafine soft magnetic alloy powder specifically involves:

[0051] S1. Iron, nickel, manganese, aluminum, silicon and chromium are smelted into an alloy at high temperature. The metal is heated to the boiling point by evaporation and condensation, and then cooled by steam to obtain ultrafine alloy powder with a D50 particle size of 100-3000nm.

[0052] S2. Under conditions of 50-60℃, 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. After standing for 5-15 min, the mixture is filtered, rinsed with pure water 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 tetraethyl orthosilicate is added. The mixture is reacted at 40-60℃ for 2-5 h, washed with anhydrous ethanol 2-5 times, filtered, and dried to obtain low-loss ultrafine soft magnetic alloy powder.

[0053] More preferably, the mass ratio of iron powder to nickel powder in step S1 is 1:1-2.

[0054] More preferably, the mass ratio of iron to manganese in step S1 is 1:0.001-0.02.

[0055] More preferably, the mass ratio of iron to aluminum in step S1 is 1:0.001-0.02.

[0056] More preferably, the mass ratio of iron to silicon in step S1 is 1:0.001-0.02.

[0057] More preferably, the mass ratio of iron to chromium in step S1 is 0.001-0.02.

[0058] More preferably, in step S2, the mass concentration of the medium-temperature zinc-manganese phosphating solution is 5-10%, and the ratio of ultrafine alloy powder to medium-temperature zinc-manganese phosphating solution is 1g:1-2mL.

[0059] More preferably, in step S2, the ratio of ultrafine alloy powder to anhydrous ethanol is 1g:5-10mL.

[0060] More preferably, in step S2, the volume ratio of 3-aminopropyltriethoxysilane to anhydrous ethanol is 1:30-40.

[0061] More preferably, in step S2, the volume ratio of 3-aminopropyltriethoxysilane to deionized water is 1:4-8.

[0062] More preferably, in step S2, the volume ratio of tetraethyl orthosilicate to 3-aminopropyltriethoxysilane is 1:3-7.

[0063] 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.

[0064] Preferably, in the manufacture of low-loss ultrafine soft magnetic alloy powder, the phosphating aid includes sodium sulfonate derivatives and acyl phospholipid derivatives. The mass ratio of ultrafine alloy powder to sodium sulfonate derivative is 1:0.01-0.03, and the mass ratio of ultrafine alloy powder to acyl phospholipid derivative is 1:0.005-0.02. The acyl phospholipid derivative improves the stability of the phosphating solution, resulting in a phosphating layer with good coating effect, thereby optimizing the soft magnetic properties of the low-loss ultrafine soft magnetic alloy powder, further improving the resistivity of the low-loss ultrafine soft magnetic alloy powder, and reducing power loss.

[0065] More preferably, the preparation of acylphospholipid derivatives specifically involves,

[0066] Take ethanolamine phosphate, add isobutyric anhydride under vacuum and 40-60℃, stir evenly, react at 80-100℃ for 2-5h, add diethanolamine, react at 90-100℃ for 6-12h to obtain acylphospholipid derivative.

[0067] More preferably, the ratio of isobutyric anhydride to ethanolamine phosphate is 1 mL: 1-5 g.

[0068] More preferably, the mass ratio of diethanolamine to ethanolamine phosphate is 1:0.5-1.0.

[0069] The present invention also discloses the low-loss ultrafine soft magnetic alloy powder prepared by the above method.

[0070] This invention also discloses the application of low-loss ultrafine soft magnetic alloy powder in the preparation of high-performance inductors.

[0071] This invention involves preparing alloy powder using iron, nickel, manganese, aluminum, silicon, and chromium. Sodium sulfonate derivatives and acyl phospholipid derivatives are used as phosphating aids to assist in the phosphating process of a medium-temperature zinc-manganese phosphating solution, forming a phosphating layer on the alloy powder surface. Then, a silicon dioxide insulating layer is coated onto the alloy powder surface using 3-aminopropyltriethoxysilane and tetraethyl orthosilicate, resulting in a low-loss ultrafine soft magnetic alloy powder. Therefore, this invention provides the following advantages: the low-loss ultrafine soft magnetic alloy powder produced by this invention has a small D50 particle size (100-3000 nm); high resistivity (9.0-18.2 Ω·cm); and low power loss (282.3-320.3 mW / cm). 3 This material can be used to prepare high-performance inductors. Therefore, this invention discloses a low-loss ultrafine soft magnetic alloy powder with high resistivity and low power loss, its manufacturing method, and its applications. Attached Figure Description

[0072] Figure 1 is a SEM image of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1.

[0073] Figure 2 shows the iron distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1.

[0074] Figure 3 shows the nickel content of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1.

[0075] Figure 4 shows the manganese distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1.

[0076] Figure 5 shows the silicon element distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1.

[0077] Figure 6 shows the oxygen distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1. Embodiments of the present invention

[0078] The present invention will now be described in further detail with reference to specific embodiments. The given embodiments are merely illustrative of the invention and not intended to limit its scope. The embodiments provided below can serve as a guide for further improvements by those skilled in the art and do not constitute a limitation on the invention in any way.

[0079] Unless otherwise specified, the experimental methods used in the following examples are conventional methods. Unless otherwise specified, the materials and reagents used in the following examples are commercially available.

[0080] Example 1:

[0081] The manufacture of low-loss ultrafine soft magnetic alloy powder includes,

[0082] S1. Iron, nickel, manganese, aluminum, silicon, and chromium are smelted into an alloy at high temperature. An evaporative cooling method is used, heating the metal to its boiling point and then cooling it with steam to obtain 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.

[0083] S2. At 55℃, anhydrous ethanol was added to the ultrafine alloy powder prepared in step S1, and the mixture was stirred at 500 r / min. 3-Aminopropyltriethoxysilane and deionized water were added, followed by tetraethyl orthosilicate. The mixture was reacted at 50℃ for 3 h, washed three times with anhydrous ethanol, filtered, and dried to obtain low-loss ultrafine soft magnetic alloy powder. The volume 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 tetraethyl orthosilicate to 3-aminopropyltriethoxysilane was 1:5.

[0084] Example 2:

[0085] The manufacture of low-loss ultrafine soft magnetic alloy powder includes,

[0086] S1. Iron, nickel, manganese, aluminum, silicon, and chromium are smelted into an alloy at high temperature. An evaporative cooling method is used, heating the metal to its boiling point and then cooling it with steam to obtain 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.

[0087] S2. At 55℃, the ultrafine alloy powder prepared in step S1 is added to a medium-temperature zinc-manganese phosphating solution and stirred at 200 r / min for 20 min. After standing for 5 min, the mixture is filtered, rinsed three times with pure water, and then anhydrous ethanol is added. The mixture is stirred at 500 r / min, and then 3-aminopropyltriethoxysilane and deionized water are added. Tetraethyl orthosilicate is added, and the mixture is reacted at 50℃ for 3 h. The mixture is then washed three times with anhydrous ethanol, filtered, and dried to obtain low-loss ultrafine soft magnetic alloy powder. The 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 ratio of ultrafine alloy powder to the medium-temperature zinc-manganese phosphating solution was 1 g:1 mL; the 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 tetraethyl orthosilicate to 3-aminopropyltriethoxysilane was 1:5.

[0088] Example 3:

[0089] Preparation of sodium sulfonate derivatives, including,

[0090] Azelaic chloride was weighed and dissolved in dichloromethane by stirring. 1-Octen-3-ol and triethylamine were added, and the mixture was stirred for 8 hours. The pH was adjusted to neutral by adding sodium carbonate solution. Sodium bisulfite and deionized water were added, and the mixture was reacted at 140°C for 3 hours. Methanol was added, and the mixture was filtered, rotary evaporated, and dried to obtain the sodium sulfonate derivative. The molar ratio of azelaic chloride to dichloromethane was 1 mol: 350 mL; the molar ratio of 1-octen-3-ol to azelaic chloride was 1:1.5; the molar ratio of triethylamine to azelaic chloride was 1:1.5; the molar ratio of azelaic chloride to sodium bisulfite was 1:1; the molar ratio of azelaic chloride to deionized water was 1 mol: 180 mL; and the volume ratio of deionized water to methanol was 1:1.

[0091] The manufacture of low-loss ultrafine soft magnetic alloy powder includes,

[0092] S1. Iron, nickel, manganese, aluminum, silicon, and chromium are smelted into an alloy at high temperature. An evaporative cooling method is used, heating the metal to its boiling point and then cooling it with steam to obtain 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.

[0093] S2. At 55℃, the ultrafine alloy powder prepared in step S1 is added to a medium-temperature zinc-manganese phosphating solution, sodium sulfonate derivative is added, and the mixture is stirred at 200 r / min for 20 min, allowed to stand for 5 min, filtered, rinsed three times with pure water, and then anhydrous ethanol is added. The mixture is stirred at 500 r / min, 3-aminopropyltriethoxysilane and deionized water are added, and tetraethyl orthosilicate is added. The mixture is reacted at 50℃ for 3 h, washed three times with anhydrous ethanol, filtered, and dried to obtain low-loss ultrafine soft magnetic alloy powder. The 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 ratio of ultrafine alloy powder to the 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 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 tetraethyl orthosilicate to 3-aminopropyltriethoxysilane was 1:5.

[0094] Example 4:

[0095] The only difference between this embodiment and Embodiment 3 is the manufacturing of low-loss ultrafine soft magnetic alloy powder.

[0096] In this embodiment, the only difference is that the mass ratio of the ultrafine alloy powder to the sodium sulfonate derivative is changed to 1:0.01 in the manufacturing of the low-loss ultrafine soft magnetic alloy powder. All other conditions are the same as in Example 3.

[0097] Example 5:

[0098] Preparation of acylphospholipid derivatives, including,

[0099] Isobutyric anhydride was added to ethanolamine phosphate under vacuum at 50°C, stirred until homogeneous, and reacted at 90°C for 3 hours. Diethanolamine was then added, and the reaction was carried out at 95°C for 8 hours to obtain an acylphospholipid derivative. The ratio of isobutyric anhydride to ethanolamine phosphate was 1 mL: 2 g; the mass ratio of diethanolamine to ethanolamine phosphate was 1:0.65.

[0100] Preparation of sodium sulfonate derivatives, including,

[0101] Azelaic chloride was weighed and dissolved in dichloromethane by stirring. 1-Octen-3-ol and triethylamine were added, and the mixture was stirred for 8 hours. The pH was adjusted to neutral by adding sodium carbonate solution. Sodium bisulfite and deionized water were added, and the mixture was reacted at 140°C for 3 hours. Methanol was added, and the mixture was filtered, rotary evaporated, and dried to obtain the sodium sulfonate derivative. The molar ratio of azelaic chloride to dichloromethane was 1 mol: 350 mL; the molar ratio of 1-octen-3-ol to azelaic chloride was 1:1.5; the molar ratio of triethylamine to azelaic chloride was 1:1.5; the molar ratio of azelaic chloride to sodium bisulfite was 1:1; the molar ratio of azelaic chloride to deionized water was 1 mol: 180 mL; and the volume ratio of deionized water to methanol was 1:1.

[0102] The manufacture of low-loss ultrafine soft magnetic alloy powder includes,

[0103] S1. Iron, nickel, manganese, aluminum, silicon, and chromium are smelted into an alloy at high temperature. An evaporative cooling method is used, heating the metal to its boiling point and then cooling it with steam to obtain 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.

[0104] S2. At 55°C, the ultrafine alloy powder prepared in step S1 is added to a medium-temperature zinc-manganese phosphating solution, along with acyl phospholipid derivatives and sodium sulfonate derivatives. The mixture is stirred at 200 r / min for 20 min, allowed to stand for 5 min, filtered, and rinsed three times with pure water. Anhydrous ethanol is then added, and the mixture is stirred at 500 r / min. 3-Aminopropyltriethoxysilane and deionized water are added, along with tetraethyl orthosilicate. The mixture is reacted at 50°C for 3 h, washed three times with anhydrous ethanol, filtered, and dried to obtain low-loss ultrafine soft magnetic alloy powder. The 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 ratio of ultrafine alloy powder to the 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 acylphosphate derivative was 1:0.02; the mass 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 tetraethyl orthosilicate to 3-aminopropyltriethoxysilane was 1:5.

[0105] Example 6:

[0106] The only difference between this embodiment and Embodiment 5 is the manufacturing of low-loss ultrafine soft magnetic alloy powder.

[0107] In this embodiment, the only difference is that the mass ratio of the ultrafine alloy powder to the acylphospholipid derivative is changed to 1:0.005 in the manufacturing of the low-loss ultrafine soft magnetic alloy powder. All other conditions are the same as in Example 5.

[0108] Comparative Example 1:

[0109] The only difference between this comparative example and Example 4 is the manufacture of the low-loss ultrafine soft magnetic alloy powder.

[0110] In this embodiment, except that no sodium sulfonate derivative was added during the manufacture of the low-loss ultrafine soft magnetic alloy powder, the other conditions are the same as in Example 4.

[0111] Experimental example:

[0112] 1. Material Characterization

[0113] The surface morphology of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1 was observed using a scanning electron microscope, and elemental distribution analysis was performed using the electron probe of the microscope.

[0114] Figure 1 is an SEM image of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1, with a scale bar of 100 nm. The low-loss ultrafine soft magnetic alloy powder prepared in Example 1 is in the form of spherical particles with a smooth surface covered with a protective layer. Figure 2 shows the iron element distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1, with a scale bar of 100 nm; Figure 3 shows the nickel element distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1, with a scale bar of 100 nm; Figure 4 shows the manganese element distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1, with a scale bar of 100 nm; Figure 5 shows the silicon element distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1, with a scale bar of 100 nm; Figure 6 shows the oxygen element distribution of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1, with a scale bar of 100 nm. Iron, nickel, manganese, silicon, and oxygen elements are uniformly distributed on the surface of the low-loss ultrafine soft magnetic alloy powder prepared in Example 1, indicating that the low-loss ultrafine soft magnetic alloy powder prepared in Example 1 of this invention effectively coats a silicon dioxide protective layer.

[0115] 2. Resistivity

[0116] The resistivity (Ω·cm) of the low-loss ultrafine soft magnetic alloy powders prepared in Examples 1-6 and Comparative Example 1 was determined using the four-probe method. The resistivity (Ω·cm) = (cross-sectional area × voltage between the two ends of the standard resistor × resistance of the standard resistor) / (voltage between the two ends of the low-loss ultrafine soft magnetic alloy powder × distance). The resistivity measurement results are shown in Table 1.

[0117] Table 1 Resistivity (Ω·cm)

[0118] Treatment Number Resistivity (Ω·cm) Example 1 9.0 Example 2 12.5 Example 3 19.0 Example 4 17.8 Example 5 25.5 Example 6 23.9 Comparative Example 1 12.9

[0119] As shown in Table 1, the resistivity of Example 2 is higher than that of Example 1 because, in the manufacturing of the low-loss ultrafine soft magnetic alloy powder, Example 2 first uses a medium-temperature zinc-manganese phosphating solution for phosphating treatment before coating with a 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 because, in the manufacturing of the 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 derivative used in the manufacturing of the low-loss ultrafine soft magnetic alloy powder is different. This indicates that in the manufacturing of low-loss ultrafine soft magnetic alloy powder, using an appropriate amount of sodium sulfonate derivative 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.

[0120] The resistivity of Examples 5-6 of this invention is higher than that of Examples 3 and Comparative Example 1 because, in the manufacture of the low-loss ultrafine soft magnetic alloy powder, Examples 5-6 synergistically used acylphospholipid derivatives and sodium sulfonate derivatives, while Example 3 only used sodium sulfonate derivatives and Comparative Example 1 only used acylphospholipid derivatives. The resistivity of Example 5 is higher than that of Example 6 because the amount of acylphospholipid derivative used in the manufacture of the low-loss ultrafine soft magnetic alloy powder is different. This indicates that, in the manufacture of low-loss ultrafine soft magnetic alloy powder, the synergistic use of acylphospholipid derivatives and sodium sulfonate derivatives to assist the phosphating effect of the medium-temperature zinc-manganese phosphating solution can further improve the resistivity of the low-loss ultrafine soft magnetic alloy powder.

[0121] 3. Power loss

[0122] The power loss of the low-loss ultrafine soft magnetic alloy powders prepared in Examples 1-6 and Comparative Example 1 was measured using a SY-8232B-H analyzer at 50 kHz / 50 mT. The results are shown in Table 2.

[0123] Table 2 Power Loss (mW / cm) 3 )

[0124]

[0125] As shown in Table 2, the power loss of Example 2 is lower than that of Example 1 because, in the manufacturing of the low-loss ultrafine soft magnetic alloy powder, Example 2 first uses a medium-temperature zinc-manganese phosphating solution for phosphating treatment before coating with a 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 because, in the manufacturing of the 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 because the amount of sodium sulfonate derivative used in the manufacturing of the low-loss ultrafine soft magnetic alloy powder is different. This indicates that in the manufacturing of low-loss ultrafine soft magnetic alloy powder, using an appropriate amount of acyl phospholipid derivative 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.

[0126] The power loss of Examples 5-6 of this invention is lower than that of Examples 3 and Comparative Example 1 because, in the manufacture of the low-loss ultrafine soft magnetic alloy powder, Examples 5-6 synergistically used acylphospholipid derivatives and sodium sulfonate derivatives, while Example 3 only used sodium sulfonate derivatives and Comparative Example 1 only used acylphospholipid derivatives. The power loss of Example 5 is lower than that of Example 6 because the amount of acylphospholipid derivative used in the manufacture of the low-loss ultrafine soft magnetic alloy powder is different. This indicates that, in the manufacture of low-loss ultrafine soft magnetic alloy powder, the synergistic use of acylphospholipid derivatives and sodium sulfonate derivatives to assist the phosphating effect of the medium-temperature zinc-manganese phosphating solution can further reduce the power loss of the low-loss ultrafine soft magnetic alloy powder.

[0127] The conventional operations in the operation steps of this invention are well known to those skilled in the art and will not be described in detail here.

[0128] The embodiments described above provide a detailed explanation of the technical solution of the present invention. It should be understood that the above descriptions are merely specific embodiments of the present invention and are not intended to limit the present invention. Any modifications, additions, or similar substitutions made within the scope of the principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for manufacturing low-loss ultrafine soft magnetic alloy powder, including, S1. Iron, nickel, manganese, aluminum, silicon and chromium are smelted into an alloy at high temperature. The alloy is heated to the boiling point by evaporation and condensation method, and then cooled by steam to obtain ultrafine alloy powder with a D50 particle size of 100-3000nm. S2. The ultrafine alloy powder is first reacted with a medium-temperature zinc-manganese phosphating solution and phosphating aid, and then reacted with 3-aminopropyltriethoxysilane and tetraethyl orthosilicate to obtain low-loss ultrafine soft magnetic alloy powder. The phosphating aids include sodium sulfonate derivatives and acyl phospholipid derivatives. The sodium sulfonate derivatives have sulfonic acid groups, benzene rings, and vinyl groups. In the preparation of the sodium sulfonate derivatives, azeloyl chloride is weighed, dissolved in dichloromethane, 1-octen-3-ol and triethylamine are added, and the mixture is stirred for 6-12 hours. Sodium carbonate solution is added to adjust the pH to neutral. Sodium bisulfite and deionized water are added, and the mixture is reacted at 120-160°C for 2-5 hours. Methanol is added, the mixture is filtered, rotary evaporated, and dried to obtain the sodium sulfonate derivative. In the preparation of the acyl phospholipid derivatives, ethanolamine phosphate is taken, isobutyric anhydride is added under vacuum at 40-60°C, stirred until homogeneous, and reacted at 80-100°C for 2-5 hours. Diethanolamine is added, and the mixture is reacted at 90-100°C for 6-12 hours to obtain the acyl phospholipid derivatives.

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

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

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

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

7. The method for manufacturing low-loss ultrafine soft magnetic alloy powder according to claim 1, characterized in that, The molar ratio of azeloyl chloride and sodium bisulfite is 1:1-2.

8. Low-loss ultrafine soft magnetic alloy powder manufactured by any of the manufacturing methods described in claims 1-7.

9. The application of the low-loss ultrafine soft magnetic alloy powder described in claim 8 in the preparation of high-performance inductors.

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