CN113363067A - Iron-silicon composite magnetic powder core with surface coating structure and preparation method thereof - Google Patents
Iron-silicon composite magnetic powder core with surface coating structure and preparation method thereof Download PDFInfo
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- 239000006247 magnetic powder Substances 0.000 title claims abstract description 195
- 239000002131 composite material Substances 0.000 title claims abstract description 62
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000576 coating method Methods 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000011248 coating agent Substances 0.000 title claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 34
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 34
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 34
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 27
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 15
- -1 silicate ester Chemical class 0.000 claims abstract description 15
- 239000012670 alkaline solution Substances 0.000 claims abstract description 14
- 230000004048 modification Effects 0.000 claims abstract description 5
- 238000012986 modification Methods 0.000 claims abstract description 5
- 230000004913 activation Effects 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 118
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 73
- 238000003756 stirring Methods 0.000 claims description 52
- 238000010438 heat treatment Methods 0.000 claims description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 27
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 27
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 15
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 11
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- WOXXJEVNDJOOLV-UHFFFAOYSA-N ethenyl-tris(2-methoxyethoxy)silane Chemical compound COCCO[Si](OCCOC)(OCCOC)C=C WOXXJEVNDJOOLV-UHFFFAOYSA-N 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 47
- 239000000126 substance Substances 0.000 abstract description 4
- 230000002035 prolonged effect Effects 0.000 abstract description 3
- 239000007771 core particle Substances 0.000 abstract 1
- 239000011162 core material Substances 0.000 description 74
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical group [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 32
- 230000000694 effects Effects 0.000 description 15
- 230000008569 process Effects 0.000 description 14
- 230000005415 magnetization Effects 0.000 description 12
- 238000001035 drying Methods 0.000 description 9
- 238000000137 annealing Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910017082 Fe-Si Inorganic materials 0.000 description 2
- 229910017133 Fe—Si Inorganic materials 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- 238000001723 curing Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/14766—Fe-Si based alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses an iron-silicon composite magnetic powder core with a surface coating structure and a preparation method thereof, the method comprises the steps of firstly, dropwise adding a silane coupling agent into iron-silicon composite magnetic powder dispersed by absolute ethyl alcohol, carrying out surface activation on the iron-silicon composite magnetic powder for 1-2 h, then, slowly dropwise adding an alkaline solution, then, slowly dropwise adding silicate ester, carrying out surface modification on the activated iron-silicon composite magnetic powder by using silicate ester to obtain SiO2And a coated iron-silicon composite magnetic powder core. The iron-silicon composite magnetic powder core with the surface coating structure prepared by the method has low raw material cost, and the preparation process is clean and environment-friendly by adopting a chemical coating method. The coated composite magnetic powder core particles are insulated, so that the loss can be reduced under the condition of keeping the high frequency of the magnetic powder core, the service life is prolonged, and finally, the magnetic powder core can be widely applied in the fields of high frequency and high powerApplication is carried out.
Description
Technical Field
The invention belongs to the field of composite materials, and particularly relates to an iron-silicon composite magnetic powder core with a surface coating structure and a preparation method thereof.
Background
With the miniaturization and light weight of modern electronic devices, the electronic field puts higher requirements on the performance of the iron-based composite magnetic powder, namely, the power loss is reduced as much as possible while the working frequency is higher and higher. In the metal magnetic powder, the iron-silicon composite magnetic powder has small magnetocrystalline anisotropy constant and almost zero magnetostriction coefficient, has better direct current superposition characteristic, high frequency stability and other magnetic properties, is particularly suitable for the technical requirements of low-voltage strong current, high power density and high magnetic flux at present, and has huge commercial application prospect in the electronic component and energy industry. However, in the application field of high frequency and high power, the iron-silicon composite magnetic powder has high loss and obvious heating phenomenon, which can cause the burning loss and the failure of the magnetic powder. The current general technical scheme is that a layer of insulating material is coated on the surface of the iron-silicon composite magnetic powder, so that the resistance of the magnetic powder is improved, the loss is reduced, and the service life is prolonged. The scheme generally comprises the steps of preparing the composite material by simple processes of coating, molding, annealing, curing and the like. The annealing treatment after compression molding can eliminate various defects and internal stress introduced in the powder preparation and compression molding processes, thereby reducing loss. However, the above method is complicated to operate, and the air pollution is large in the heat treatment process steps such as annealing in industrial production. Is not good for green development requirement in general.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide the iron-silicon composite magnetic powder core with the surface coating structure.
The second purpose of the invention is to provide a preparation method of the iron-silicon composite magnetic powder core with the surface coating structure.
The purpose of the invention is realized by the following technical scheme:
a preparation method of an iron-silicon composite magnetic powder core with a surface coating structure comprises the steps of firstly, dropwise adding a silane coupling agent into iron-silicon composite magnetic powder dispersed by absolute ethyl alcohol, carrying out surface activation on the iron-silicon composite magnetic powder for 1-2 hours, then, slowly dropwise adding an alkaline solution, then, slowly dropwise adding silicate ester, carrying out surface modification on the activated iron-silicon composite magnetic powder by using silicate ester to obtain SiO2And a coated iron-silicon composite magnetic powder core.
The molecular structural formula of the silane coupling agent is generally Y-R-Si (OR)3(wherein Y is an organic functional group and SiOR is a siloxy group). Firstly, organic functional group Y of silane coupling agent and iron-silicon composite magnetic powder are dehydrated and condensed to form hydrogen bond for surface activation, and then silicon oxide group hydrolysis-polycondensation reaction of silicate ester and silane coupling agent is utilized to coat SiO on the surface of the activated iron-silicon composite magnetic powder2Finally synthesizing SiO2And a coated iron-silicon composite magnetic powder core.
Preferably, the preparation method of the iron-silicon composite magnetic powder core with the surface coating structure comprises the following steps:
(1) uniformly dispersing the iron-silicon composite magnetic powder in absolute ethyl alcohol, heating to 40-50 ℃, dropwise adding a silane coupling agent, and reacting at 40-50 ℃ for 1-2 hours;
(2) heating the solution obtained in the step (1) to 60-70 ℃, slowly dripping alkaline solution, slowly dripping silicate ester, and continuously reacting for 3-6 hours to obtain SiO2A coated iron-silicon composite magnetic powder core;
both the step (1) and the step (2) are carried out under stirring;
the speed of dripping the silane coupling agent in the step (1) is 0.2-0.3 g/min; in the step (2), the speed of slowly dripping the alkaline solution and the silicate ester is 0.03-0.04 ml/min.
Preferably, the iron-silicon composite magnetic powder in the step (1) is Fe-6.5 wt% Si;
the heating speed of the step (1) and the step (2) is 2-3 ℃/min;
and (3) in the step (2), the alkaline solution is at least one of ammonia water, NaOH solution or KOH solution.
Preferably, the ratio of the iron-silicon composite magnetic powder in the step (1) to the alkaline solution in the step (2) is 1-5 g/mL.
Preferably, the ratio of the iron-silicon composite magnetic powder in the step (1) to the alkaline solution in the step (2) is 2.5 g/mL.
Preferably, in the step (1), the concentration of the iron-silicon composite magnetic powder in the absolute ethyl alcohol is 0.017-0.03 g/mL, and the mass ratio of the iron-silicon composite magnetic powder to the silane coupling agent is (5-10): (0.6 to 1); the iron-silicon composite magnetic powder in the step (1) comprises the following steps: the silicate concentration in the step (2) is 0.8-1.6 g/mL.
Preferably, the concentration of the iron-silicon composite magnetic powder in the absolute ethyl alcohol in the step (1) is 0.025 g/mL; the iron-silicon composite magnetic powder in the step (1) comprises the following steps: the silicate concentration ratio in the step (2) was 1.25 g/mL.
Preferably, the silane coupling agent in the step (1) is at least one of vinyltris (β -methoxyethoxy) silane (a172), vinyltriethoxysilane (a151), vinyltrimethoxysilane (a171), γ -Aminopropyltriethoxysilane (APTES);
the silicate ester in the step (2) is at least one of tetraethoxysilane (tetraethoxysilane), tetramethoxysilane (methyl orthosilicate) and tetrapropoxysilane (propyl orthosilicate).
Preferably, after the reaction in the step (2) is finished, collecting by using a permanent magnet, and then filtering, washing by using absolute ethyl alcohol and vacuum drying at 35-50 ℃; and (3) the stirring speed of the step (1) and the step (2) is 200-300 rpm.
The iron-silicon composite magnetic powder core with the surface coating structure is prepared by the method.
The iron-silicon composite magnetic powder core with the surface coating structure prepared by the method has low loss under the high-frequency condition.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the method adopts a chemical coating method, adds alkaline substances as catalysts, omits the subsequent steps of mould pressing, annealing, curing and the like, and has the advantages of low cost, simple operation and environmental friendliness compared with the prior art.
(2) The iron-silicon composite magnetic powder core with the surface coating structure is insulated among particles by changing the concentration of a solvent, the concentration of an alkaline substance and the concentration of silicate ester, and compared with the raw material of the iron-silicon composite magnetic powder, the iron-silicon composite magnetic powder core with the surface coating structure has an obviously excellent high-frequency low-loss effect, namely, the loss can be reduced under the condition of keeping the high frequency of the magnetic powder core, so that the service life of the iron-silicon composite magnetic powder is prolonged, and the iron-silicon composite magnetic powder can be widely applied in the high-frequency and high-power application fields.
Drawings
FIG. 1 is a synthetic scheme of examples 1-4 of the present invention.
FIG. 2 is a synthesis scheme of example 5 of the present invention.
FIG. 3 is a synthetic scheme of examples 6-8 of the present invention.
FIG. 4 is a synthetic scheme of examples 9-12 of the present invention.
FIG. 5 shows the Fe-6.5 wt% Si magnetic powder raw material (A) and SiO obtained in example 12Comparative Scanning Electron Microscope (SEM) image of coated Fe-6.5 wt% Si magnetic powder core (B).
FIG. 6 shows the Fe-6.5 wt% Si magnetic powder raw material (A) and SiO obtained in example 52Comparative Scanning Electron Microscope (SEM) image of coated Fe-6.5 wt% Si magnetic powder core (B).
FIG. 7 shows the Fe-6.5 wt% Si magnetic powder raw material (A) and SiO obtained in example 62Comparative Scanning Electron Microscope (SEM) image of coated Fe-6.5 wt% Si magnetic powder core (B).
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
In the following examples, Fe-6.5 wt% Si magnetic powder was purchased from Yaozhou Co., Ltd, Qinghe county, Hebei province; ammonia water is purchased from Mecline, the product number is A801005-500ml, and the ammonia content is 25% -28%; the NaOH solution is purchased from Mecanne, the product number is S817976-1L, and the concentration is 0.1 mol/L; KOH solution was purchased from Michelin under the trade designation P816402-100ml with a concentration of 0.1001 mol/L. Unless otherwise specified, other starting materials for the reactions in the examples are commercially available.
Example 1
Preparation of SiO Using the synthetic scheme as shown in FIG. 12The coated Fe-6.5 wt% Si magnetic powder core comprises the following specific steps:
adding 5g of Fe-6.5 wt% Si magnetic powder into 167mL of absolute ethyl alcohol, mechanically stirring for 10 minutes at the stirring speed of 200rpm to uniformly disperse the magnetic powder, slowly heating to 50 ℃, slowly dropwise adding 0.6g of gamma-Aminopropyltriethoxysilane (APTES), and mechanically stirring for 2 hours at 50 ℃; slowly heating to 60 ℃, slowly dropwise adding 2mL of ammonia water, slowly dropwise adding 4mL of tetraethoxysilane (tetraethoxysilane) for 2h, continuously mechanically stirring to react for 6h after dropwise adding is finished, filtering after the reaction is finished, washing with absolute ethyl alcohol, and vacuum drying at 50 ℃ for 24h to obtain SiO2Coated Fe-6.5 wt% Si magnetic powder core. The speed of slow temperature rise in the experimental process is 2.5 ℃/min; the slow dropping speed of the gamma-aminopropyl triethoxysilane (APTES) is 0.25 g/min; the slow dropping speed of ammonia water and tetraethoxysilane (tetraethoxysilane) is 0.033 ml/min.
Wherein the molecular formula of the gamma-aminopropyl triethoxysilane (APTES) is C9H23NO3Si, the structural formula is as follows:
tetraethoxysilane (tetraethoxysilane) with molecular formula of C8H20O4Si, the structural formula is as follows:
as can be seen from FIG. 5, SiO obtained in example 12The surface of the coated Fe-6.5 wt% Si magnetic powder core material (B) was rough relative to the Fe-6.5 wt% Si magnetic powder raw material (A), indicating that SiO2Uniformly coating the surface of the Fe-6.5 wt% Si magnetic powder core. As can be seen from Table 1, the resistivity rho was compared with that of the Fe-6.5 wt% Si magnetic powder raw materialThe resistivity is increased by about 63 times, and the loss (P) under different conditions is reduced by increasing the resistivity10/1k(1.0T，1kHz)、P5/2k(0.5T，2kHz)、P2/5k(0.2T，5kHz)、P1/10k(0.1T, 10kHz)) was close to 13 times, and it can be seen that SiO obtained in example 1 was2Compared with the raw material of the Fe-6.5 wt% Si magnetic powder, the coated Fe-6.5 wt% Si magnetic powder core material has obviously excellent high-frequency low-loss effect. In this example SiO2The coated Fe-6.5 wt% Si magnetic powder core has a saturation magnetization M higher than that of the raw material Fe-6.5 wt% Si magnetic powdersReduced by about 4emu/g and coercive force HcBasically similar and has excellent soft magnetic performance.
Example 2
Preparation of SiO Using the synthetic scheme as shown in FIG. 12The coated Fe-6.5 wt% Si magnetic powder core comprises the following specific steps:
adding 5g of Fe-6.5 wt% Si magnetic powder into 200mL of absolute ethyl alcohol, mechanically stirring for 10 minutes at the stirring speed of 200rpm to uniformly disperse the magnetic powder, slowly heating to 50 ℃, slowly dropwise adding 0.6g of gamma-Aminopropyltriethoxysilane (APTES), mechanically stirring at 50 ℃ for 2 hours, slowly heating to 60 ℃, slowly dropwise adding 2mL of ammonia water, slowly dropwise adding 4mL of tetraethoxysilane (tetraethoxysilane) for 2 hours, continuously mechanically stirring to react for 6 hours after dropwise adding is finished, filtering after the reaction is finished, washing with absolute ethyl alcohol, and drying in vacuum at 50 ℃ for 24 hours to obtain SiO2Coated Fe-6.5 wt% Si magnetic powder core. The speed of slow temperature rise in the experimental process is 2.5 ℃/min; the slow dropping speed of the gamma-aminopropyl triethoxysilane (APTES) is 0.25 g/min; the slow dropping speed of ammonia water and tetraethoxysilane (tetraethoxysilane) is 0.033 ml/min.
Wherein the molecular formula of the gamma-aminopropyl triethoxysilane (APTES) is C9H23NO3Si, the structural formula is as follows:
tetraethoxysilane (tetraethoxysilane) with molecular formula of C8H20O4Si with the structural formula asShown below:
as can be seen from Table 1, the resistivity P is increased by nearly 83 times as compared with the Fe-6.5 wt% Si magnetic powder raw material, and the loss (P) under different conditions is reduced by increasing the resistivity10/1k(1.0T，1kHz)、P5/2k(0.5T，2kHz)、P2/5k(0.2T，5kHz)、P1/10k(0.1T, 10kHz)) was close to 17 times, and it can be seen that SiO was obtained in example 22Compared with the raw material of the Fe-6.5 wt% Si magnetic powder, the coated Fe-6.5 wt% Si magnetic powder core material has obviously excellent high-frequency low-loss effect. In this example SiO2The coated Fe-6.5 wt% Si magnetic powder core has a saturation magnetization M higher than that of the raw material Fe-6.5 wt% Si magnetic powdersReduced by about 11emu/g and coercive force HcBasically similar and has excellent soft magnetic performance.
Example 3
Preparation of SiO Using the synthetic scheme as shown in FIG. 12The coated Fe-6.5 wt% Si magnetic powder core comprises the following specific steps:
adding 5g of Fe-6.5 wt% Si magnetic powder into 250mL of absolute ethyl alcohol, mechanically stirring for 10 minutes at the stirring speed of 200rpm to uniformly disperse the magnetic powder, slowly heating to 50 ℃, slowly dropwise adding 0.6g of gamma-Aminopropyltriethoxysilane (APTES), mechanically stirring at 50 ℃ for 2 hours, slowly heating to 60 ℃, slowly dropwise adding 2mL of ammonia water, slowly dropwise adding 4mL of tetraethoxysilane (tetraethoxysilane) for 2 hours, continuously mechanically stirring to react for 6 hours after dropwise adding is finished, filtering after the reaction is finished, washing with absolute ethyl alcohol, and drying in vacuum at 50 ℃ for 24 hours to obtain SiO2Coated Fe-6.5 wt% Si magnetic powder core. The speed of slow temperature rise in the experimental process is 2.5 ℃/min; the slow dropping speed of the gamma-aminopropyl triethoxysilane (APTES) is 0.25 g/min; the slow dropping speed of ammonia water and tetraethoxysilane (tetraethoxysilane) is 0.033 ml/min.
Wherein the molecular formula of the gamma-aminopropyl triethoxysilane (APTES) is C9H23NO3Si, the structural formula is as follows:
tetraethoxysilane (tetraethoxysilane) with molecular formula of C8H20O4Si, the structural formula is as follows:
as can be seen from Table 1, the resistivity P is increased by about 75 times as compared with the raw material of Fe-6.5 wt% Si magnetic powder, and the loss (P) under different conditions is reduced by increasing the resistivity10/1k(1.0T，1kHz)、P5/2k(0.5T，2kHz)、P2/5k(0.2T，5kHz)、P1/10k(0.1T, 10kHz)) was nearly 14 times, and it can be seen that SiO was obtained in example 32Compared with the raw material of the Fe-6.5 wt% Si magnetic powder, the coated Fe-6.5 wt% Si magnetic powder core material has obviously excellent high-frequency low-loss effect. In this example SiO2The coated Fe-6.5 wt% Si magnetic powder core has a saturation magnetization M higher than that of the raw material Fe-6.5 wt% Si magnetic powdersReduced by about 9emu/g and coercive force HcBasically similar and has excellent soft magnetic performance.
Example 4
Preparation of SiO Using the synthetic scheme as shown in FIG. 12The coated Fe-6.5 wt% Si magnetic powder core comprises the following specific steps:
adding 5g of Fe-6.5 wt% Si magnetic powder into 280mL of absolute ethyl alcohol, mechanically stirring for 10 minutes at the stirring speed of 200rpm to uniformly disperse the magnetic powder, slowly heating to 50 ℃, slowly dropwise adding 0.6g of gamma-Aminopropyltriethoxysilane (APTES), mechanically stirring at 50 ℃ for 2 hours, slowly heating to 60 ℃, slowly dropwise adding 2mL of ammonia water, slowly dropwise adding 4mL of tetraethoxysilane (tetraethoxysilane) for 2 hours, continuously mechanically stirring to react for 6 hours after dropwise adding is finished, filtering after the reaction is finished, washing with absolute ethyl alcohol, and vacuum drying at 50 ℃ for 24 hours to obtain SiO2Coated Fe-6.5 wt% Si magnetic powder core. The speed of slow temperature rise in the experimental process is 2.5 ℃/min; gamma-aminopropyl trisThe speed of slowly dripping ethoxysilane (APTES) is 0.25 g/min; the slow dropping speed of ammonia water and tetraethoxysilane (tetraethoxysilane) is 0.033 ml/min.
Wherein the molecular formula of the gamma-aminopropyl triethoxysilane (APTES) is C9H23NO3Si, the structural formula is as follows:
tetraethoxysilane (tetraethoxysilane) with molecular formula of C8H20O4Si, the structural formula is as follows:
as can be seen from Table 1, the resistivity P is increased by about 56 times as compared with the Fe-6.5 wt% Si magnetic powder raw material, and the loss (P) under different conditions is reduced by increasing the resistivity10/1k(1.0T，1kHz)、P5/2k(0.5T，2kHz)、P2/5k(0.2T，5kHz)、P1/10k(0.1T, 10kHz)) was nearly 11 times, and it can be seen that SiO obtained in example 42Compared with the raw material of the Fe-6.5 wt% Si magnetic powder, the coated Fe-6.5 wt% Si magnetic powder core material has obviously excellent high-frequency low-loss effect. In this example SiO2The coated Fe-6.5 wt% Si magnetic powder core has a saturation magnetization M higher than that of the raw material Fe-6.5 wt% Si magnetic powdersReduced by about 3emu/g and coercive force HcBasically similar and has excellent soft magnetic performance.
Example 5
Preparation of SiO Using the synthetic scheme as shown in FIG. 22The coated Fe-6.5 wt% Si magnetic powder core comprises the following specific steps:
adding 5g of Fe-6.5 wt% Si magnetic powder into 200mL of absolute ethyl alcohol, mechanically stirring for 10 minutes at the stirring speed of 300rpm to uniformly disperse the magnetic powder, slowly heating to 50 ℃, slowly dropwise adding 1g of gamma-Aminopropyltriethoxysilane (APTES), mechanically stirring at 50 ℃ for 1.5 hours, slowly heating to 60 ℃, and slowly dropwise adding4mL of tetramethoxysilane (methyl orthosilicate) for 2h, continuously mechanically stirring and reacting for 6h after the dropwise addition is finished, filtering after the reaction is finished, washing with absolute ethyl alcohol, and drying in vacuum at 40 ℃ for 24h to obtain SiO2Coated Fe-6.5 wt% Si magnetic powder core. The speed of slow temperature rise in the experimental process is 2.5 ℃/min; the slow dropping speed of the gamma-aminopropyl triethoxysilane (APTES) is 0.25 g/min; tetramethoxysilane (methyl orthosilicate) was slowly added dropwise at a rate of 0.033 ml/min.
Wherein the molecular formula of the gamma-aminopropyl triethoxysilane (APTES) is C5H12O3Si, the structural formula is as follows:
tetramethoxysilane (methyl orthosilicate) with the molecular formula C4H12O4Si, the structural formula is as follows:
as can be seen from FIG. 6, the SiO produced in example 52Coated Fe-6.5 wt% Si magnetic powder core material (B) with respect to Fe-6.5 wt% Si magnetic powder raw material (A) SiO2The coating coverage rate is low, and the coating effect is poor. As can be seen from Table 1, the resistivity rho is increased by about 18 times as compared with the raw material of Fe-6.5 wt% Si magnetic powder, and the loss (P) under different conditions is reduced by increasing the resistivity10/1k(1.0T，1kHz)、P5/2k(0.5T，2kHz)、P2/5k(0.2T，5kHz)、P1/10k(0.1T, 10kHz)) only 4 times, as can be seen, due to example 5SiO2The coating effect is poor, and the prepared SiO2The coated Fe-6.5 wt% Si magnetic powder core material has no significant high frequency low loss effect compared to Fe-6.5 wt% Si magnetic powder raw material. In this example SiO2The coated Fe-6.5 wt% Si magnetic powder core has a saturation magnetization M higher than that of the raw material Fe-6.5 wt% Si magnetic powdersReduced by about 1emu/g and coercive force HcSubstantially similar.
Example 6
Preparation of SiO Using the synthetic scheme as shown in FIG. 32The coated Fe-6.5 wt% Si magnetic powder core comprises the following specific steps:
adding 5g of Fe-6.5 wt% Si magnetic powder into 200mL of absolute ethyl alcohol, mechanically stirring for 10 minutes at the stirring speed of 300rpm to uniformly disperse the magnetic powder, slowly heating to 50 ℃, slowly dropwise adding 1g of gamma-Aminopropyltriethoxysilane (APTES), mechanically stirring at 50 ℃ for 1.5 hours, slowly heating to 60 ℃, slowly dropwise adding 1mL of sodium hydroxide solution, slowly dropwise adding 4mL of tetramethoxysilane (methyl orthosilicate) for 2 hours, continuously mechanically stirring to react for 6 hours after dropwise adding is finished, filtering after the reaction is finished, washing with absolute ethyl alcohol, and drying in vacuum at 40 ℃ for 24 hours to obtain SiO2Coated Fe-6.5 wt% Si magnetic powder core. The speed of slow temperature rise in the experimental process is 2.5 ℃/min; the slow dropping speed of the gamma-aminopropyl triethoxysilane (APTES) is 0.25 g/min; the sodium hydroxide solution and tetramethoxysilane (methyl orthosilicate) were slowly added dropwise at a rate of 0.033 ml/min.
Wherein the molecular formula of the gamma-aminopropyl triethoxysilane (APTES) is C5H12O3Si, the structural formula is as follows:
tetramethoxysilane (methyl orthosilicate) with the molecular formula C4H12O4Si, the structural formula is as follows:
as can be seen from FIG. 6, the SiO produced in example 62The surface of the coated Fe-6.5 wt% Si magnetic powder core material (B) was rough relative to the Fe-6.5 wt% Si magnetic powder raw material (A), indicating that SiO2Uniformly coating the surface of the Fe-6.5 wt% Si magnetic powder core. As can be seen from Table 1, the resistivity rho is improved by nearly 66 times compared with the raw material of Fe-6.5 wt% Si magnetic powder, and the resistivity is improved, so that the resistivity is reduced under different conditionsLoss (P)10/1k(1.0T，1kHz)、P5/2k(0.5T，2kHz)、P2/5k(0.2T，5kHz)、P1/10k(0.1T, 10kHz)) is nearly 13 times, and it can be seen that SiO obtained in example 62Compared with the raw material of the Fe-6.5 wt% Si magnetic powder, the coated Fe-6.5 wt% Si magnetic powder core material has obviously excellent high-frequency low-loss effect. In this example SiO2The coated Fe-6.5 wt% Si magnetic powder core has a saturation magnetization M higher than that of the raw material Fe-6.5 wt% Si magnetic powdersReduced by about 6emu/g and coercive force HcBasically similar and has excellent soft magnetic performance.
Example 7
Preparation of SiO Using the synthetic scheme as shown in FIG. 32The coated Fe-6.5 wt% Si magnetic powder core comprises the following specific steps:
adding 5g of Fe-6.5 wt% Si magnetic powder into 200mL of absolute ethyl alcohol, mechanically stirring for 10 minutes at the stirring speed of 300rpm to uniformly disperse the magnetic powder, slowly heating to 50 ℃, slowly dropwise adding 1g of gamma-Aminopropyltriethoxysilane (APTES), mechanically stirring at 50 ℃ for 1.5 hours, slowly heating to 60 ℃, slowly dropwise adding 2mL of sodium hydroxide solution, slowly dropwise adding 4mL of tetramethoxysilane (methyl orthosilicate) for 2 hours, continuously mechanically stirring to react for 6 hours after dropwise adding is finished, filtering after the reaction is finished, washing with absolute ethyl alcohol, and drying in vacuum at 40 ℃ for 24 hours to obtain SiO2Coated Fe-6.5 wt% Si magnetic powder core. The speed of slow temperature rise in the experimental process is 2.5 ℃/min; the slow dropping speed of the gamma-aminopropyl triethoxysilane (APTES) is 0.25 g/min; the sodium hydroxide solution and tetramethoxysilane (methyl orthosilicate) were slowly added dropwise at a rate of 0.033 ml/min.
Wherein the molecular formula of the gamma-aminopropyl triethoxysilane (APTES) is C5H12O3Si, the structural formula is as follows:
tetramethoxysilane (methyl orthosilicate) with the molecular formula C4H12O4Si, the structural formula is as follows:
as can be seen from Table 1, the resistivity P is increased by nearly 87 times as compared with the raw material of Fe-6.5 wt% Si magnetic powder, and the loss (P) under different conditions is reduced by increasing the resistivity10/1k(1.0T，1kHz)、P5/2k(0.5T，2kHz)、P2/5k(0.2T，5kHz)、P1/10k(0.1T, 10kHz)) was close to 17 times, and it can be seen that SiO was obtained in example 72Compared with the raw material of the Fe-6.5 wt% Si magnetic powder, the coated Fe-6.5 wt% Si magnetic powder core material has obviously excellent high-frequency low-loss effect. In this example SiO2The coated Fe-6.5 wt% Si magnetic powder core has a saturation magnetization M higher than that of the raw material Fe-6.5 wt% Si magnetic powdersReduced by about 11emu/g and coercive force HcBasically similar and has excellent soft magnetic performance.
Example 8
Preparation of SiO Using the synthetic scheme as shown in FIG. 32The coated Fe-6.5 wt% Si magnetic powder core comprises the following specific steps:
adding 5g of Fe-6.5 wt% Si magnetic powder into 200mL of absolute ethyl alcohol, mechanically stirring for 10 minutes at the stirring speed of 300rpm to uniformly disperse the magnetic powder, slowly heating to 50 ℃, slowly dropwise adding 1g of gamma-Aminopropyltriethoxysilane (APTES), mechanically stirring at 50 ℃ for 1.5 hours, slowly heating to 60 ℃, slowly dropwise adding 3mL of sodium hydroxide solution, slowly dropwise adding 4mL of tetramethoxysilane (methyl orthosilicate) for 2 hours, continuously mechanically stirring to react for 6 hours after dropwise adding is finished, filtering after the reaction is finished, washing with absolute ethyl alcohol, and drying in vacuum at 40 ℃ for 24 hours to obtain SiO2Coated Fe-6.5 wt% Si magnetic powder core. The speed of slow temperature rise in the experimental process is 2.5 ℃/min; the slow dropping speed of the gamma-aminopropyl triethoxysilane (APTES) is 0.25 g/min; the sodium hydroxide solution and tetramethoxysilane (methyl orthosilicate) were slowly added dropwise at a rate of 0.033 ml/min.
Wherein the molecular formula of the gamma-aminopropyl triethoxysilane (APTES) is C5H12O3Si, the structural formula is as follows:
tetramethoxysilane (methyl orthosilicate) with the molecular formula C4H12O4Si, the structural formula is as follows:
as can be seen from Table 1, the resistivity P is increased by nearly 73 times as compared with the Fe-6.5 wt% Si magnetic powder raw material, and the loss (P) under different conditions is reduced by increasing the resistivity10/1k(1.0T，1kHz)、P5/2k(0.5T，2kHz)、P2/5k(0.2T，5kHz)、P1/10k(0.1T, 10kHz)) was nearly 14 times, and it can be seen that SiO was obtained in example 82Compared with the raw material of the Fe-6.5 wt% Si magnetic powder, the coated Fe-6.5 wt% Si magnetic powder core material has obviously excellent high-frequency low-loss effect. In this example SiO2The coated Fe-6.5 wt% Si magnetic powder core has a saturation magnetization M higher than that of the raw material Fe-6.5 wt% Si magnetic powdersReduced by about 2emu/g and coercive force HcBasically similar and has excellent soft magnetic performance.
Example 9
Preparation of SiO Using the synthetic scheme as shown in FIG. 42The coated Fe-6.5 wt% Si magnetic powder core comprises the following specific steps:
adding 5g of Fe-6.5 wt% Si magnetic powder into 200mL of absolute ethyl alcohol, mechanically stirring for 10 minutes at the stirring speed of 300rpm to uniformly disperse the magnetic powder, slowly heating to 50 ℃, slowly dropwise adding 1g of gamma-Aminopropyltriethoxysilane (APTES), mechanically stirring at 50 ℃ for 1.5 hours, slowly heating to 60 ℃, slowly dropwise adding 2mL of potassium hydroxide solution, slowly dropwise adding 3mL of tetrapropoxysilane (n-propyl orthosilicate) for 2 hours, continuously mechanically stirring and reacting for 6 hours after dropwise adding is finished, filtering after the reaction is finished, washing with absolute ethyl alcohol, and drying under vacuum at 40 ℃ for 24 hours to obtain SiO2Coated Fe-6.5 wt% Si magnetic powder core. The speed of slow temperature rise in the experimental process is 2.5 ℃/min; gamma-aminopropyl triethoxyThe slow dropping speed of silane (APTES) is 0.25 g/min; the potassium hydroxide solution and tetrapropoxysilane (propyl orthosilicate) were slowly added dropwise at a rate of 0.033 ml/min.
Wherein the molecular formula of the gamma-aminopropyl triethoxysilane (APTES) is C5H12O3Si, the structural formula is as follows:
tetrapropoxysilane (propyl orthosilicate) with molecular formula of C12H28O4Si, the structural formula is as follows:
as can be seen from Table 1, the resistivity P is increased by about 76 times as compared with the Fe-6.5 wt% Si magnetic powder raw material, and the loss (P) under different conditions is reduced by increasing the resistivity10/1k(1.0T，1kHz)、P5/2k(0.5T，2kHz)、P2/5k(0.2T，5kHz)、P1/10k(0.1T, 10kHz)) was nearly 14 times, and it can be seen that SiO obtained in example 92Compared with the raw material of the Fe-6.5 wt% Si magnetic powder, the coated Fe-6.5 wt% Si magnetic powder core material has obviously excellent high-frequency low-loss effect. In this example SiO2The coated Fe-6.5 wt% Si magnetic powder core has a saturation magnetization M higher than that of the raw material Fe-6.5 wt% Si magnetic powdersReduced by about 6emu/g and coercive force HcBasically similar and has excellent soft magnetic performance.
Example 10
Preparation of SiO Using the synthetic scheme as shown in FIG. 42The coated Fe-6.5 wt% Si magnetic powder core comprises the following specific steps:
adding 5g of Fe-6.5 wt% Si magnetic powder into 200mL of absolute ethyl alcohol, mechanically stirring for 10 minutes at the stirring speed of 300rpm to uniformly disperse the magnetic powder, slowly heating to 50 ℃, slowly dropwise adding 1g of gamma-Aminopropyltriethoxysilane (APTES), mechanically stirring for 1.5 hours at 50 ℃, slowly heating to 60 ℃, and slowly heating firstDropwise adding 2mL of potassium hydroxide solution, slowly dropwise adding 4mL of tetrapropoxysilane (n-propyl orthosilicate) for 2h, continuously mechanically stirring and reacting for 6h after dropwise adding is finished, filtering after the reaction is finished, washing with absolute ethyl alcohol, and vacuum drying at 40 ℃ for 24h to obtain SiO2Coated Fe-6.5 wt% Si magnetic powder core. The speed of slow temperature rise in the experimental process is 2.5 ℃/min; the slow dropping speed of the gamma-aminopropyl triethoxysilane (APTES) is 0.25 g/min; the potassium hydroxide solution and tetrapropoxysilane (propyl orthosilicate) were slowly added dropwise at a rate of 0.033 ml/min.
Wherein the molecular formula of the gamma-aminopropyl triethoxysilane (APTES) is C5H12O3Si, the structural formula is as follows:
tetrapropoxysilane (propyl orthosilicate) with molecular formula of C12H28O4Si, the structural formula is as follows:
as can be seen from Table 1, the resistivity P is increased by nearly 93 times as compared with the raw material of Fe-6.5 wt% Si magnetic powder, and the loss (P) under different conditions is reduced by increasing the resistivity10/1k(1.0T，1kHz)、P5/2k(0.5T，2kHz)、P2/5k(0.2T，5kHz)、P1/10k(0.1T, 10kHz)) was nearly 19 times, and it can be seen that SiO produced in example 102Compared with the raw material of the Fe-6.5 wt% Si magnetic powder, the coated Fe-6.5 wt% Si magnetic powder core material has obviously excellent high-frequency low-loss effect. In this example SiO2The coated Fe-6.5 wt% Si magnetic powder core has a saturation magnetization M higher than that of the raw material Fe-6.5 wt% Si magnetic powdersReduced by about 13emu/g and coercive force HcBasically similar and has excellent soft magnetic performance.
Example 11
Preparation of SiO Using the synthetic scheme as shown in FIG. 42Coated Fe-6.5 wt% Si magnetic powder coreThe method comprises the following steps:
adding 5g of Fe-6.5 wt% Si magnetic powder into 200mL of absolute ethyl alcohol, mechanically stirring for 10 minutes at the stirring speed of 300rpm to uniformly disperse the magnetic powder, slowly heating to 50 ℃, slowly dropwise adding 1g of gamma-Aminopropyltriethoxysilane (APTES), mechanically stirring at 50 ℃ for 1.5 hours, slowly heating to 60 ℃, slowly dropwise adding 2mL of potassium hydroxide solution, slowly dropwise adding 5mL of tetrapropoxysilane (n-propyl orthosilicate) for 2 hours, continuously mechanically stirring and reacting for 6 hours after dropwise adding is finished, filtering after the reaction is finished, washing with absolute ethyl alcohol, and drying under vacuum at 40 ℃ for 24 hours to obtain SiO2Coated Fe-6.5 wt% Si magnetic powder core. The speed of slow temperature rise in the experimental process is 2.5 ℃/min; the slow dropping speed of the gamma-aminopropyl triethoxysilane (APTES) is 0.25 g/min; the potassium hydroxide solution and tetrapropoxysilane (propyl orthosilicate) were slowly added dropwise at a rate of 0.033 ml/min.
Wherein the molecular formula of the gamma-aminopropyl triethoxysilane (APTES) is C5H12O3Si, the structural formula is as follows:
tetrapropoxysilane (propyl orthosilicate) with molecular formula of C12H28O4Si, the structural formula is as follows:
as can be seen from Table 1, the resistivity P is improved by nearly 78 times as compared with the Fe-6.5 wt% Si magnetic powder raw material, and the loss (P) under different conditions is reduced by improving the resistivity10/1k(1.0T，1kHz)、P5/2k(0.5T，2kHz)、P2/5k(0.2T，5kHz)、P1/10k(0.1T, 10kHz)) was close to 15 times, and it can be seen that SiO produced in example 112Compared with the raw material of the Fe-6.5 wt% Si magnetic powder, the coated Fe-6.5 wt% Si magnetic powder core material has obviously excellent high-frequency low-loss effect. In this example SiO2Coated Fe-6.5 wt% Si magnetic powder core ratio Fe-6.5 wt% Si magnetic powder raw material saturation magnetization MsReduced by about 5emu/g and coercive force HcBasically similar and has excellent soft magnetic performance.
Example 12
Preparation of SiO Using the synthetic scheme as shown in FIG. 42The coated Fe-6.5 wt% Si magnetic powder core comprises the following specific steps:
adding 5g of Fe-6.5 wt% Si magnetic powder into 200mL of absolute ethyl alcohol, mechanically stirring for 10 minutes at the stirring speed of 300rpm to uniformly disperse the magnetic powder, slowly heating to 50 ℃, slowly dropwise adding 1g of gamma-Aminopropyltriethoxysilane (APTES), mechanically stirring at 50 ℃ for 1.5 hours, slowly heating to 60 ℃, slowly dropwise adding 2mL of potassium hydroxide solution, slowly dropwise adding 6mL of tetrapropoxysilane (n-propyl orthosilicate) for 2 hours, continuously mechanically stirring for reacting for 6 hours after dropwise adding is finished, filtering after the reaction is finished, washing with absolute ethyl alcohol, and drying at 40 ℃ in vacuum for 24 hours to obtain SiO2Coated Fe-6.5 wt% Si magnetic powder core. The speed of slow temperature rise in the experimental process is 2.5 ℃/min; the slow dropping speed of the gamma-aminopropyl triethoxysilane (APTES) is 0.25 g/min; the potassium hydroxide solution and tetrapropoxysilane (propyl orthosilicate) were slowly added dropwise at a rate of 0.033 ml/min.
Wherein the molecular formula of the gamma-aminopropyl triethoxysilane (APTES) is C5H12O3Si, the structural formula is as follows:
tetrapropoxysilane (propyl orthosilicate) with molecular formula of C12H28O4Si, the structural formula is as follows:
as can be seen from Table 1, the resistivity P is improved by about 61 times as compared with the Fe-6.5 wt% Si magnetic powder raw material, and the loss (P) under different conditions is reduced by improving the resistivity10/1k(1.0T，1kHz)、P5/2k(0.5T，2kHz)、P2/5k(0.2T，5kHz)、P1/10k(0.1T, 10kHz)) is nearly 12 times, and it can be seen that SiO produced in example 122Compared with the raw material of the Fe-6.5 wt% Si magnetic powder, the coated Fe-6.5 wt% Si magnetic powder core material has obviously excellent high-frequency low-loss effect. In this example SiO2The coated Fe-6.5 wt% Si magnetic powder core has a saturation magnetization M higher than that of the raw material Fe-6.5 wt% Si magnetic powdersReduced by about 2emu/g and coercive force HcBasically similar and has excellent soft magnetic performance.
Table 1: fe-6.5 wt% Si magnetic powder raw Material and SiO obtained in examples 1 to 122Comparison of magnetic Properties of magnetic powder core Material coated with Fe-6.5 wt% Si
As can be seen from table 1 above: the Fe-Si composite magnetic powder core with the surface coating structure is prepared by the formula designed by the invention, silane coupling agent is used for modifying the surface of the magnetic powder core, hydrolysis-polycondensation reaction of silicate ester is utilized for coating the surface of the magnetic powder core, and finally the Fe-Si composite magnetic powder core with the surface coating structure is synthesized. The concentration of the Fe-6.5 wt% Si magnetic powder raw material in absolute ethyl alcohol is preferably 0.017-0.03 g/mL; most preferably 0.025 g/mL. The Fe-6.5 wt% Si magnetic powder raw material: the ratio of the alkaline solution is 1-5 g/mL; most preferably 2.5 g/mL. The Fe-6.5 wt% Si magnetic powder raw material: the concentration of silicate ester is preferably 0.8-1.6 g/mL; most preferably 1.25 g/mL.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. Iron-silicon composite magnet with surface coating structureThe preparation method of the powder core is characterized by firstly dropwise adding a silane coupling agent into the iron-silicon composite magnetic powder dispersed by absolute ethyl alcohol, carrying out surface activation on the iron-silicon composite magnetic powder for 1-2 hours, then slowly dropwise adding an alkaline solution, then slowly dropwise adding silicate ester, and carrying out surface modification on the activated iron-silicon composite magnetic powder by using silicate ester to obtain SiO2And a coated iron-silicon composite magnetic powder core.
2. The method of claim 1, comprising the steps of:
(1) uniformly dispersing the iron-silicon composite magnetic powder in absolute ethyl alcohol, heating to 40-50 ℃, dropwise adding a silane coupling agent, and reacting at 40-50 ℃ for 1-2 hours;
(2) heating the solution obtained in the step (1) to 60-70 ℃, slowly dripping alkaline solution, slowly dripping silicate ester, and continuously reacting for 3-6 hours to obtain SiO2A coated iron-silicon composite magnetic powder core;
both the step (1) and the step (2) are carried out under stirring;
the speed of dripping the silane coupling agent in the step (1) is 0.2-0.3 g/min; in the step (2), the speed of slowly dripping the alkaline solution and the silicate ester is 0.03-0.04 ml/min.
3. The production method according to claim 2, wherein the iron-silicon composite magnetic powder in the step (1) is Fe-6.5 wt% Si;
the heating speed of the step (1) and the step (2) is 2-3 ℃/min;
and (3) in the step (2), the alkaline solution is at least one of ammonia water, NaOH solution or KOH solution.
4. The preparation method according to claim 3, wherein the ratio of the iron-silicon composite magnetic powder in the step (1) to the alkaline solution in the step (2) is 1-5 g/mL.
5. The method according to claim 4, wherein the ratio of the iron-silicon composite magnetic powder in step (1) to the alkaline solution in step (2) is 2.5 g/mL.
6. The preparation method according to claim 2, 3, 4 or 5, wherein the concentration of the iron-silicon composite magnetic powder in the absolute ethyl alcohol in the step (1) is 0.017-0.03 g/mL, and the mass ratio of the iron-silicon composite magnetic powder to the silane coupling agent is (5-10): (0.6 to 1); the iron-silicon composite magnetic powder in the step (1) comprises the following steps: the silicate concentration in the step (2) is 0.8-1.6 g/mL.
7. The method according to claim 2 or 3 or 4 or 5, wherein the concentration of the iron-silicon composite magnetic powder in the absolute ethyl alcohol in the step (1) is 0.025 g/mL; the iron-silicon composite magnetic powder in the step (1) comprises the following steps: the silicate concentration ratio in the step (2) was 1.25 g/mL.
8. The method according to claim 2, 3, 4 or 5, wherein the silane coupling agent in the step (1) is at least one of vinyltris (β -methoxyethoxy) silane, vinyltriethoxysilane, vinyltrimethoxysilane, γ -aminopropyltriethoxysilane;
the silicate in the step (2) is at least one of tetraethoxysilane, tetramethoxysilane and tetrapropoxysilane.
9. The preparation method according to claim 2 or 3 or 4 or 5, characterized in that, the reaction in step (2) is continued and then collected by a permanent magnet, and then filtration, absolute ethyl alcohol washing and vacuum drying at 35-50 ℃ are carried out; and (3) the stirring speed of the step (1) and the step (2) is 200-300 rpm.
10. An iron-silicon composite magnetic powder core with a surface coating structure prepared by the method of any one of claims 1 to 9.
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| CN102824891A (en) * | 2012-09-19 | 2012-12-19 | 清华大学 | Preparation method of compact single-layer SiO2 coated on surface of magnetic nuclear material Fe3O4 |
| CN109014177A (en) * | 2018-08-31 | 2018-12-18 | 国网江苏省电力有限公司泰州供电分公司 | A kind of preparation method of insulating wrapped composite powder and transformer core |
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| CN102824891A (en) * | 2012-09-19 | 2012-12-19 | 清华大学 | Preparation method of compact single-layer SiO2 coated on surface of magnetic nuclear material Fe3O4 |
| CN109014177A (en) * | 2018-08-31 | 2018-12-18 | 国网江苏省电力有限公司泰州供电分公司 | A kind of preparation method of insulating wrapped composite powder and transformer core |
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| CN114806157A (en) * | 2022-04-29 | 2022-07-29 | 宁波京磁科技发展有限公司 | Neodymium-iron-boron magnetic composite material and preparation method thereof |
| CN114806157B (en) * | 2022-04-29 | 2023-12-01 | 宁波京磁科技发展有限公司 | Neodymium-iron-boron magnetic composite material and preparation method thereof |
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Application publication date: 20210907 |