CN114068167A - Soft magnetic composite material and preparation method and application thereof - Google Patents
Soft magnetic composite material and preparation method and application thereof Download PDFInfo
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- CN114068167A CN114068167A CN202111345462.3A CN202111345462A CN114068167A CN 114068167 A CN114068167 A CN 114068167A CN 202111345462 A CN202111345462 A CN 202111345462A CN 114068167 A CN114068167 A CN 114068167A
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- 239000002131 composite material Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 99
- 238000002161 passivation Methods 0.000 claims abstract description 52
- 238000000576 coating method Methods 0.000 claims abstract description 36
- 239000011248 coating agent Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 31
- 239000006247 magnetic powder Substances 0.000 claims abstract description 30
- 238000003756 stirring Methods 0.000 claims abstract description 29
- 238000001035 drying Methods 0.000 claims abstract description 27
- 238000003825 pressing Methods 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 239000000314 lubricant Substances 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 28
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 20
- 239000004111 Potassium silicate Substances 0.000 claims description 14
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 14
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 14
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 14
- 235000019353 potassium silicate Nutrition 0.000 claims description 14
- 239000004115 Sodium Silicate Substances 0.000 claims description 13
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 13
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 13
- 229910000519 Ferrosilicon Inorganic materials 0.000 claims description 11
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 9
- 239000004327 boric acid Substances 0.000 claims description 9
- -1 orthochromate Chemical compound 0.000 claims description 9
- 229910000838 Al alloy Inorganic materials 0.000 claims description 8
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 8
- 229910000599 Cr alloy Inorganic materials 0.000 claims description 6
- 239000000788 chromium alloy Substances 0.000 claims description 6
- 235000015393 sodium molybdate Nutrition 0.000 claims description 6
- 239000011684 sodium molybdate Substances 0.000 claims description 6
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 6
- 239000012300 argon atmosphere Substances 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 229920002050 silicone resin Polymers 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910000863 Ferronickel Inorganic materials 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 21
- 230000008569 process Effects 0.000 abstract description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 229960004838 phosphoric acid Drugs 0.000 description 12
- 235000011007 phosphoric acid Nutrition 0.000 description 12
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 8
- 238000009413 insulation Methods 0.000 description 8
- 238000000137 annealing Methods 0.000 description 6
- 239000000696 magnetic material Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 6
- 239000012798 spherical particle Substances 0.000 description 6
- 229910000676 Si alloy Inorganic materials 0.000 description 4
- 238000000748 compression moulding Methods 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XEVZIAVUCQDJFL-UHFFFAOYSA-N [Cr].[Fe].[Si] Chemical compound [Cr].[Fe].[Si] XEVZIAVUCQDJFL-UHFFFAOYSA-N 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 229910002796 Si–Al Inorganic materials 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 229910000702 sendust Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229920001732 Lignosulfonate Polymers 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- PXLIDIMHPNPGMH-UHFFFAOYSA-N sodium chromate Chemical compound [Na+].[Na+].[O-][Cr]([O-])(=O)=O PXLIDIMHPNPGMH-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
Classifications
-
- 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
- H01F1/14708—Fe-Ni based alloys
- H01F1/14733—Fe-Ni based alloys in the form of particles
- H01F1/14741—Fe-Ni based alloys in the form of particles pressed, sintered or bonded together
- H01F1/1475—Fe-Ni based alloys in the form of particles pressed, sintered or bonded together the particles being insulated
-
- 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
- H01F1/147—Alloys characterised by their composition
- H01F1/14766—Fe-Si based alloys
- H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust
-
- 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
- H01F1/22—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 pressed, sintered, or bound together
- H01F1/24—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 pressed, sintered, or bound together the particles being insulated
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F27/00—Details of transformers or inductances, in general
- H01F27/24—Magnetic cores
- H01F27/255—Magnetic cores made from particles
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F27/00—Details of transformers or inductances, in general
- H01F27/34—Special means for preventing or reducing unwanted electric or magnetic effects, e.g. no-load losses, reactive currents, harmonics, oscillations, leakage fields
-
- H—ELECTRICITY
- H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
- H02K—DYNAMO-ELECTRIC MACHINES
- H02K1/00—Details of the magnetic circuit
- H02K1/02—Details of the magnetic circuit characterised by the magnetic material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F27/00—Details of transformers or inductances, in general
- H01F27/34—Special means for preventing or reducing unwanted electric or magnetic effects, e.g. no-load losses, reactive currents, harmonics, oscillations, leakage fields
- H01F2027/348—Preventing eddy currents
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Manufacturing & Machinery (AREA)
- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention provides a soft magnetic composite material and a preparation method and application thereof, wherein the preparation method comprises the following steps: (1) mixing the soft magnetic powder and the passivation solution, uniformly stirring and drying to obtain passivation powder; (2) mixing the coating liquid and the passivation powder obtained in the step (1), uniformly stirring and drying to obtain coating powder; (3) and (3) mixing a lubricant and the coated powder obtained in the step (2), uniformly stirring and grinding, pressing into a ring, and then performing heat treatment to obtain the soft magnetic composite material. The soft magnetic composite material can be used for manufacturing a switching power supply, a motor magnetic core, a charger magnetic core or a transformer magnetic core. The preparation method provided by the invention increases the resistivity of the soft magnetic composite material, reduces the eddy current loss among particles, meets the requirements of low loss and higher direct current superposition characteristics of the material, simplifies the process flow and reduces the production cost, thereby widening the application field of the soft magnetic composite material.
Description
Technical Field
The invention belongs to the technical field of magnetic materials, relates to a soft magnetic composite material, and particularly relates to a soft magnetic composite material and a preparation method and application thereof.
Background
In order to adapt to the development trend of emerging wireless charging and intelligent wearable equipment towards miniaturization and integration, the soft magnetic composite material is used as an important basic material of electronic equipment and is also an electromagnetic conversion material, and the market puts forward higher and higher requirements on the performance of the soft magnetic composite material, such as the requirement of meeting high saturation magnetization, low loss, higher direct current superposition characteristics and the like.
The soft magnetic composite material is prepared by mixing magnetic powder and an insulating agent through a powder metallurgy method, and performing pressing and annealing processes. Losses in soft magnetic materials consist of hysteresis losses, eddy current losses and residual losses. When the frequency is low, the hysteresis loss in the material dominates; the fraction of eddy current losses in the material increases with increasing frequency. In general, hysteresis loss is proportional to the frequency, and eddy current loss is proportional to the square of the frequency. Therefore, when the material is used at high frequencies, it is important to reduce eddy current losses in the material. The eddy current loss in the soft magnetic composite material includes an eddy current loss inside the particles and an eddy current loss between the particles. The soft magnetic powder is subjected to insulation treatment, so that the eddy current loss among material particles can be effectively reduced, the energy loss of the soft magnetic material is further reduced, and the purpose of energy conservation is achieved.
Wangjian et al published an article entitled Performance improvement of Fe-6.5Si soft magnetic composites with high-temperature phosphoric-silica insulation coatings, in which a sol-gel method was used to coat the surface of Fe-6.5Si with a phosphoric-silica insulation layer, and the authors emphasized that a highly heat-resistant silica insulation layer was used to protect and prevent the decomposition and crystallization of the inner phosphoric-acid insulation layer, but this experimental procedure was complicated and not easy to implement in industrial production.
CN 112185640A discloses a method for coating a magnetic powder core with sodium silicate, which comprises the steps of taking alcohol ether phosphate as a dispersant of sodium silicate, taking lignosulfonate as a dispersant of metal magnetic powder, mixing and coating dispersed sodium silicate solution and dispersed metal magnetic powder, drying, adding an adhesive and a lubricant, then carrying out compression molding, and finally carrying out high-temperature annealing treatment to obtain the magnetic powder core coated with sodium silicate. The loss of the magnetic core of the material prepared by the invention is 242-267mW/cm3(50kHz 100mT), the direct current bias performance is 29.5% -36.4%, and it can be seen that the magnetic core of the material prepared by the invention has large loss and low direct current bias, so that the application field is narrow, and the requirements of low loss and high direct current superposition characteristics of the material cannot be met.
Therefore, how to provide the soft magnetic composite material and the preparation method thereof can increase the resistivity of the soft magnetic composite material, reduce the eddy current loss among particles, meet the requirements of low loss and higher direct current superposition characteristics of the material, simplify the process flow and reduce the production cost, thereby widening the application field of the soft magnetic composite material and becoming the problem which needs to be solved by technical personnel in the field at present.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a soft magnetic composite material and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a soft magnetic composite material, comprising the steps of:
(1) mixing the soft magnetic powder and the passivation solution, uniformly stirring and drying to obtain passivation powder;
(2) mixing the coating liquid and the passivation powder obtained in the step (1), uniformly stirring and drying to obtain coating powder;
(3) and (3) mixing a lubricant and the coated powder obtained in the step (2), uniformly stirring and grinding, pressing into a ring, and then performing heat treatment to obtain the soft magnetic composite material.
According to the invention, the surface of the soft magnetic powder is passivated, a layer of passivation film is generated on the surface of the magnetic powder, the chemical activity of metal is reduced, and then the passivation film is coated, so that the decomposition and crystallization of the passivation film in the subsequent high-temperature annealing process are avoided, the functions of cementing and filling gaps are achieved, and the strength of the material is improved. According to the invention, the soft magnetic powder is subjected to insulation treatment and then is subjected to compression molding, so that the eddy current loss among material particles is effectively reduced, the energy loss of the soft magnetic material is further reduced, and the purpose of energy conservation is achieved.
Preferably, the soft magnetic powder in step (1) includes any one or a combination of at least two of iron-silicon alloy powder, iron-nickel alloy powder, iron-silicon-aluminum alloy powder or iron-silicon-chromium alloy powder, and typical but non-limiting combinations include a combination of iron-silicon alloy powder and iron-nickel alloy powder, a combination of iron-nickel alloy powder and iron-silicon-aluminum alloy powder, a combination of iron-silicon-aluminum alloy powder and iron-silicon-chromium alloy powder, a combination of iron-silicon alloy powder, iron-nickel alloy powder and iron-silicon-aluminum alloy powder, or a combination of iron-nickel alloy powder, iron-silicon-aluminum alloy powder and iron-silicon-chromium alloy powder.
Preferably, the particle shape of the soft magnetic powder in the step (1) is spherical.
Preferably, the solute in the passivating solution of step (1) comprises any one of, or a combination of at least two of, phosphoric acid, boric acid, orthochromate, manganese nitrate or sodium molybdate, and typical but non-limiting combinations include a combination of phosphoric acid and boric acid, a combination of boric acid and orthochromate, a combination of orthochromate and manganese nitrate, a combination of manganese nitrate and sodium molybdate, a combination of phosphoric acid, boric acid and orthochromate, a combination of boric acid, orthochromate and manganese nitrate, or a combination of orthochromate, manganese nitrate and sodium molybdate.
Preferably, the solute in the passivation solution in step (1) accounts for 0.1% to 2% of the mass of the soft magnetic powder, and may be, for example, 0.1%, 0.2%, 0.4%, 0.6%, 0.8%, 1%, 1.2%, 1.4%, 1.6%, 1.8%, or 2%, but is not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
Preferably, the drying temperature in step (1) is 40-80 deg.C, such as 40 deg.C, 45 deg.C, 50 deg.C, 55 deg.C, 60 deg.C, 65 deg.C, 70 deg.C, 75 deg.C or 80 deg.C, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the drying time in step (1) is 20-40min, such as 20min, 22min, 24min, 26min, 28min, 30min, 32min, 34min, 36min, 38min or 40min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the solute in the coating liquid in step (2) comprises any one of or a combination of at least two of sodium silicate, potassium silicate, aluminum oxide or silicone resin, and typical but non-limiting combinations include a combination of sodium silicate and potassium silicate, a combination of potassium silicate and aluminum oxide, a combination of aluminum oxide and silicone resin, a combination of sodium silicate, potassium silicate and aluminum oxide, a combination of potassium silicate, aluminum oxide and silicone resin, or a combination of sodium silicate, potassium silicate, aluminum oxide and silicone resin.
Preferably, the solute in the coating solution in step (2) accounts for 0.1% to 6% of the mass of the passivation powder, and may be, for example, 0.1%, 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, or 6%, but is not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
Preferably, the lubricant of step (3) comprises zinc stearate.
Preferably, the lubricant in step (3) accounts for 0.3% -0.5% of the mass of the coated powder, and may be, for example, 0.3%, 0.32%, 0.34%, 0.36%, 0.38%, 0.4%, 0.42%, 0.44%, 0.46%, 0.48%, or 0.5%, but is not limited to the enumerated values, and other unrecited values within the range of the enumerated values are also applicable.
Preferably, the pressing temperature in step (3) is 20-30 ℃, for example 20 ℃, 21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃, 26 ℃, 27 ℃, 28 ℃, 29 ℃ or 30 ℃, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the pressing pressure in step (3) is 1500-.
Preferably, the heat treatment of step (3) is performed in a nitrogen atmosphere, a helium atmosphere, or an argon atmosphere.
Preferably, the temperature of the heat treatment in step (3) is 500-850 ℃, and may be, for example, 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃, 750 ℃, 800 ℃ or 850 ℃, but is not limited to the recited values, and other unrecited values within the range of the values are also applicable.
Preferably, the time of the heat treatment in step (3) is 30-400min, such as 30min, 50min, 100min, 150min, 200min, 250min, 300min, 350min or 400min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
As a preferred technical solution of the first aspect of the present invention, the preparation method comprises the steps of:
(1) mixing the soft magnetic powder and the passivation solution, uniformly stirring, and drying at 40-80 ℃ for 20-40min to obtain passivation powder; the soft magnetic powder comprises any one or the combination of at least two of ferrosilicon powder, ferronickel powder, ferrosilicon-aluminum alloy powder or ferrosilicon-chromium alloy powder, and the particle shape is spherical; the solute in the passivation solution comprises any one or the combination of at least two of phosphoric acid, boric acid, n-chromate, manganese nitrate and sodium molybdate, and accounts for 0.1-2% of the mass of the soft magnetic powder;
(2) mixing the coating liquid and the passivation powder obtained in the step (1), uniformly stirring and drying to obtain coating powder; the solute in the coating liquid comprises any one or the combination of at least two of sodium silicate, potassium silicate, alumina and silicon resin, and the solute accounts for 0.1-6% of the mass of the passivation powder;
(3) mixing zinc stearate with the coating powder obtained in the step (2), wherein the zinc stearate accounts for 0.3-0.5% of the mass of the coating powder, uniformly stirring and grinding, pressing into a ring at 20-30 ℃, 1500-2500MPa, and then carrying out heat treatment at 500-850 ℃ for 30-400min to obtain the soft magnetic composite material; the heat treatment is performed in a nitrogen atmosphere, a helium atmosphere, or an argon atmosphere.
In a second aspect, the present invention provides a soft magnetic composite material prepared by the method of the first aspect.
In a third aspect, the present invention provides a use of the soft magnetic composite material according to the second aspect in a magnetic core of a switching power supply, a motor, a charger or a transformer.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the invention, the surface of the soft magnetic powder is passivated, so that a layer of passivation film is generated on the surface of the magnetic powder, the chemical activity of metal is reduced, and then the passivation film is coated, so that the decomposition and crystallization of the passivation film in the subsequent high-temperature annealing process are avoided, the functions of cementing and filling gaps are achieved, and the strength of the material is improved;
(2) the invention carries out insulation treatment on the soft magnetic powder and then carries out compression molding, thereby effectively reducing the eddy current loss among material particles, further reducing the energy loss of the soft magnetic material and achieving the purpose of energy saving, and the total loss is reduced to 106kW/m under the conditions of 50mT and 100kHz3When the superposed current is 10A, the direct current superposition characteristic is as high as more than 90.3 percent, and the quality factor is as high as 288, so that the requirements of low material loss, high direct current superposition characteristic and high quality factor are met;
(3) the preparation method provided by the invention is simple in process flow, convenient to operate, low in cost, high in production efficiency, green and environment-friendly, and is suitable for industrial large-scale production and application.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Example 1
The embodiment provides a soft magnetic composite material and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) adding 100g of ferrosilicon powder with spherical particle shape into a phosphoric acid passivation solution, wherein the phosphoric acid in the passivation solution accounts for 0.1 percent of the weight of the ferrosilicon powder, uniformly stirring, placing in a drying oven, and drying at 60 ℃ for 30min to obtain passivation powder;
(2) adding the passivation powder obtained in the step (1) into a mixed coating liquid of potassium silicate and silicon resin, wherein the solute in the coating liquid accounts for 6% of the mass of the passivation powder, uniformly stirring and drying to obtain a coating powder;
(3) and (3) mixing zinc stearate with the coated powder obtained in the step (2), wherein the zinc stearate accounts for 0.5% of the mass of the coated powder, uniformly stirring and grinding, pressing into a ring (26.9mm OD multiplied by 14.7mm ID multiplied by 11.2mm tall) at 25 ℃ and 1500MPa, and performing heat treatment on the obtained pressing ring for 400min at 500 ℃ in a nitrogen atmosphere to eliminate internal stress generated in the pressing process to obtain the soft magnetic composite material.
Example 2
The embodiment provides a soft magnetic composite material and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) adding 100g of iron-nickel alloy powder with spherical particle shape into a mixed passivation solution of phosphoric acid and sodium chromate, wherein the solute in the passivation solution accounts for 1% of the mass of the iron-nickel alloy powder, uniformly stirring, placing in a drying oven, and drying at 40 ℃ for 40min to obtain passivation powder;
(2) adding the passivation powder obtained in the step (1) into a potassium silicate coating liquid, wherein the potassium silicate in the coating liquid accounts for 3% of the mass of the passivation powder, uniformly stirring and drying to obtain coating powder;
(3) and (3) mixing zinc stearate with the coated powder obtained in the step (2), wherein the zinc stearate accounts for 0.4% of the mass of the coated powder, uniformly stirring and grinding, pressing into a ring (26.9mm OD multiplied by 14.7mm ID multiplied by 11.2mm tall) at 20 ℃ and 2500MPa, and performing heat treatment on the obtained compression ring for 200min at 700 ℃ in a helium atmosphere to eliminate internal stress generated in the pressing process to obtain the soft magnetic composite material.
Example 3
The embodiment provides a soft magnetic composite material and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) adding 100g of Fe-Si-Al alloy powder with spherical particle shape into a mixed passivation solution of phosphoric acid and boric acid, wherein solute in the passivation solution accounts for 2% of the weight of the Fe-Si-Al alloy powder, uniformly stirring, placing in a drying oven, and drying at 80 ℃ for 20min to obtain passivation powder;
(2) adding the passivated powder obtained in the step (1) into a sodium silicate coating solution, wherein the sodium silicate in the coating solution accounts for 0.1% of the mass of the passivated powder, uniformly stirring and drying to obtain coated powder;
(3) and (3) mixing zinc stearate with the coated powder obtained in the step (2), wherein the zinc stearate accounts for 0.3% of the mass of the coated powder, uniformly stirring and grinding the mixture, pressing the mixture into a ring (26.9mm OD multiplied by 14.7mm ID multiplied by 11.2mm tall) at the temperature of 30 ℃ and the pressure of 2000MPa, and carrying out heat treatment on the obtained compression ring for 30min at the temperature of 850 ℃ in an argon atmosphere in order to eliminate internal stress generated in the pressing process to obtain the soft magnetic composite material.
Example 4
This embodiment provides a soft magnetic composite material and a method for preparing the same, wherein the preparation method is the same as that of embodiment 1 except that the mass of phosphoric acid in the passivation solution of step (1) is changed to 3% of the mass of the iron-silicon alloy powder, and thus the details are not repeated herein.
Example 5
This embodiment provides a soft magnetic composite material and a method for preparing the same, wherein the preparation method is the same as that of embodiment 2 except that the mass of potassium silicate in the coating solution of step (2) is changed to 7% of the mass of iron-nickel alloy powder, and thus the details are not repeated herein.
Example 6
The present embodiment provides a soft magnetic composite material and a preparation method thereof, and the preparation method is the same as that of embodiment 3 except that the mass of zinc stearate in step (3) is changed to 0.2% of the mass of sendust powder, so that details are not repeated herein.
Example 7
The present embodiment provides a soft magnetic composite material and a preparation method thereof, and the preparation method is the same as that of embodiment 3 except that the mass of zinc stearate in step (3) is changed to 0.6% of the mass of sendust powder, so that details are not repeated herein.
Comparative example 1
The present comparative example provides a soft magnetic composite material and a method for preparing the same, the method comprising the steps of:
(1) adding 100g of ferrosilicon powder with spherical particle shape into a phosphoric acid passivation solution, wherein the phosphoric acid in the passivation solution accounts for 0.1 percent of the weight of the ferrosilicon powder, uniformly stirring, placing in a drying oven, and drying at 60 ℃ for 30min to obtain passivation powder;
(2) and (2) mixing zinc stearate with the passivation powder obtained in the step (1), wherein the zinc stearate accounts for 0.5% of the mass of the passivation powder, uniformly stirring and grinding the mixture, pressing the mixture into a ring (26.9mm OD multiplied by 14.7mm ID multiplied by 11.2mm tall) at 25 ℃ and 1500MPa, and performing heat treatment on the obtained pressing ring for 400min at 500 ℃ in a nitrogen atmosphere to eliminate internal stress generated in the pressing process to obtain the soft magnetic composite material.
Comparative example 2
The present comparative example provides a soft magnetic composite material and a method for preparing the same, the method comprising the steps of:
(1) adding 100g of ferrosilicon powder with spherical particle shape into a mixed coating liquid of potassium silicate and silicon resin, wherein solute in the coating liquid accounts for 6% of the weight of the ferrosilicon powder, uniformly stirring and drying to obtain coating powder;
(2) and (2) mixing zinc stearate with the coated powder obtained in the step (1), wherein the zinc stearate accounts for 0.5% of the mass of the coated powder, uniformly stirring and grinding, pressing into a ring (26.9mm OD multiplied by 14.7mm ID multiplied by 11.2mm tall) at 25 ℃ and 1500MPa, and performing heat treatment on the obtained pressing ring for 400min at 500 ℃ in a nitrogen atmosphere to eliminate internal stress generated in the pressing process to obtain the soft magnetic composite material.
Comparative example 3
The comparative example provides a soft magnetic composite material and a preparation method thereof, and the preparation method specifically comprises the following steps: mixing zinc stearate with 100g of ferrosilicon powder with spherical particle shape, wherein the zinc stearate accounts for 0.5 percent of the weight of the ferrosilicon powder, uniformly stirring and grinding the mixture, pressing the mixture into a ring (26.9mm OD multiplied by 14.7mm ID multiplied by 11.2mm tall) at the temperature of 25 ℃ and the pressure of 1500MPa, and carrying out heat treatment on the obtained pressing ring for 400min at the temperature of 500 ℃ in a nitrogen atmosphere in order to eliminate internal stress generated in the pressing process to obtain the soft magnetic composite material.
A series of performance tests were performed on the soft magnetic composite materials obtained in examples 1 to 7 and comparative examples 1 to 3, 40 turns each of the primary coil and the secondary coil, the quality factor of the product was measured by an LCR tester, the inductance test and the inductance superposition test were performed by an LCR tester under the condition that the superimposed current was 10A, the direct current superposition characteristic of the product was measured, the total loss of the product was measured by an alternating current B-H meter under the conditions of 50mT and 100kHz, and the measurement results are shown in Table 1.
TABLE 1
| Soft magnetic composite material | Quality factor | Total loss (kW/m)3) | Direct current superposition characteristics |
| Example 1 | 288 | 104 | 90.5 |
| Example 2 | 290 | 106 | 90.6 |
| Example 3 | 289 | 105 | 90.3 |
| Example 4 | 288 | 103 | 90.7 |
| Example 5 | 288 | 102 | 90.8 |
| Example 6 | 290 | 106 | 90.3 |
| Example 7 | 288 | 104 | 90.3 |
| Comparative example 1 | 220 | 320 | 80.0 |
| Comparative example 2 | 212 | 500 | 75.1 |
| Comparative example 3 | 206 | 800 | 60.9 |
As can be seen from Table 1: the soft magnetic composite materials obtained in the examples 1 to 7 meet the requirements of low loss, higher direct current superposition characteristic and high quality factor, and the total loss is reduced to 106kW/m under the conditions of 50mT and 100kHz3When the superposed current is 10A, the direct current superposition characteristic is as high as more than 90.3 percent, and the quality factor is as high as more than 288; compared with the embodiment 1, the comparative example 1 does not coat the powder, so that the passive film is decomposed and crystallized in the subsequent high-temperature annealing process, the quality factor and the direct-current superposition characteristic are obviously reduced, and the total loss is increased; comparative example 2 does not passivate the powder, resulting in higher chemical activity of the metal and also reducing the quality factor and the direct current superposition characteristic of the material; comparative example 3 directly presses the powder into a ring without passivation and coating, the quality factor and the direct current superposition characteristic are obviously reduced, and the total loss is obviously increased.
Therefore, the surface of the soft magnetic powder is passivated, a layer of passivation film is generated on the surface of the magnetic powder, the chemical activity of metal is reduced, and then the passivation film is coated, so that the decomposition and crystallization of the passivation film in the subsequent high-temperature annealing process are avoided, the functions of cementing and filling gaps are realized, and the strength of the material is improved; the invention carries out insulation treatment on the soft magnetic powder and then carries out compression molding, thereby effectively reducing the eddy current loss among material particles, further reducing the energy loss of the soft magnetic material and achieving the purpose of energy saving, and the total loss is reduced to 106kW/m under the conditions of 50mT and 100kHz3When the superposed current is 10A, the direct current superposition characteristic is as high as more than 90.3 percent, and the quality factor is as high as 288, so that the requirements of low material loss, high direct current superposition characteristic and high quality factor are met; in addition, the preparation method provided by the invention is simple in process flow, convenient to operate, low in cost, high in production efficiency, green and environment-friendly, and is suitable for industrial large-scale production and application.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing a soft magnetic composite material, characterized in that the method comprises the following steps:
(1) mixing the soft magnetic powder and the passivation solution, uniformly stirring and drying to obtain passivation powder;
(2) mixing the coating liquid and the passivation powder obtained in the step (1), uniformly stirring and drying to obtain coating powder;
(3) and (3) mixing a lubricant and the coated powder obtained in the step (2), uniformly stirring and grinding, pressing into a ring, and then performing heat treatment to obtain the soft magnetic composite material.
2. The preparation method according to claim 1, wherein the soft magnetic powder in step (1) comprises any one or a combination of at least two of ferrosilicon powder, ferronickel powder, ferrosilicon-aluminum alloy powder or ferrosilicon-chromium alloy powder;
preferably, the particle shape of the soft magnetic powder in the step (1) is spherical.
3. The preparation method according to claim 1 or 2, characterized in that the solute in the passivating solution of step (1) comprises any one or a combination of at least two of phosphoric acid, boric acid, orthochromate, manganese nitrate or sodium molybdate;
preferably, the solute in the passivation solution in the step (1) accounts for 0.1-2% of the mass of the soft magnetic powder.
4. The method according to any one of claims 1 to 3, wherein the drying temperature in step (1) is 40 to 80 ℃;
preferably, the drying time in step (1) is 20-40 min.
5. The method according to any one of claims 1 to 4, wherein the solute in the coating liquid of step (2) comprises any one of sodium silicate, potassium silicate, alumina or silicone resin or a combination of at least two thereof;
preferably, the solute in the coating liquid in the step (2) accounts for 0.1-6% of the mass of the passivation powder.
6. The production method according to any one of claims 1 to 5, wherein the lubricant of step (3) comprises zinc stearate;
preferably, the lubricant in the step (3) accounts for 0.3-0.5% of the mass of the coated powder.
7. The method according to any one of claims 1 to 6, wherein the temperature of the pressing in step (3) is 20 to 30 ℃;
preferably, the applying pressure of the pressing in the step (3) is 1500-;
preferably, the heat treatment of step (3) is performed in a nitrogen atmosphere, a helium atmosphere, or an argon atmosphere;
preferably, the temperature of the heat treatment in the step (3) is 500-850 ℃;
preferably, the time of the heat treatment in the step (3) is 30-400 min.
8. The method of any one of claims 1 to 7, comprising the steps of:
(1) mixing the soft magnetic powder and the passivation solution, uniformly stirring, and drying at 40-80 ℃ for 20-40min to obtain passivation powder; the soft magnetic powder comprises any one or the combination of at least two of ferrosilicon powder, ferronickel powder, ferrosilicon-aluminum alloy powder or ferrosilicon-chromium alloy powder, and the particle shape is spherical; the solute in the passivation solution comprises any one or the combination of at least two of phosphoric acid, boric acid, n-chromate, manganese nitrate and sodium molybdate, and accounts for 0.1-2% of the mass of the soft magnetic powder;
(2) mixing the coating liquid and the passivation powder obtained in the step (1), uniformly stirring and drying to obtain coating powder; the solute in the coating liquid comprises any one or the combination of at least two of sodium silicate, potassium silicate, alumina and silicon resin, and the solute accounts for 0.1-6% of the mass of the passivation powder;
(3) mixing zinc stearate with the coating powder obtained in the step (2), wherein the zinc stearate accounts for 0.3-0.5% of the mass of the coating powder, uniformly stirring and grinding, pressing into a ring at 20-30 ℃, 1500-2500MPa, and then carrying out heat treatment at 500-850 ℃ for 30-400min to obtain the soft magnetic composite material; the heat treatment is performed in a nitrogen atmosphere, a helium atmosphere, or an argon atmosphere.
9. A soft magnetic composite material produced by the production method according to any one of claims 1 to 8.
10. Use of the soft magnetic composite material according to claim 9 in switching power supplies, motor cores, charger cores or transformer cores.
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