CN108017383B - Soft magnetic material with high magnetic conductivity and high frequency and high impedance characteristics and preparation method thereof - Google Patents
Soft magnetic material with high magnetic conductivity and high frequency and high impedance characteristics and preparation method thereof Download PDFInfo
- Publication number
- CN108017383B CN108017383B CN201711259872.XA CN201711259872A CN108017383B CN 108017383 B CN108017383 B CN 108017383B CN 201711259872 A CN201711259872 A CN 201711259872A CN 108017383 B CN108017383 B CN 108017383B
- Authority
- CN
- China
- Prior art keywords
- soft magnetic
- magnetic material
- high frequency
- permeability
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000696 magnetic material Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 92
- 230000035699 permeability Effects 0.000 claims abstract description 47
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 15
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims description 51
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 42
- 239000001301 oxygen Substances 0.000 claims description 42
- 229910052760 oxygen Inorganic materials 0.000 claims description 42
- 239000004576 sand Substances 0.000 claims description 34
- 239000000843 powder Substances 0.000 claims description 32
- 239000007921 spray Substances 0.000 claims description 28
- 238000001816 cooling Methods 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- 238000005469 granulation Methods 0.000 claims description 17
- 230000003179 granulation Effects 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 16
- 238000004321 preservation Methods 0.000 claims description 16
- 239000002518 antifoaming agent Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 15
- 239000000654 additive Substances 0.000 claims description 14
- 238000012360 testing method Methods 0.000 claims description 14
- 239000012298 atmosphere Substances 0.000 claims description 13
- 238000003801 milling Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 230000004907 flux Effects 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 5
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 2
- 238000007493 shaping process Methods 0.000 claims description 2
- 239000013530 defoamer Substances 0.000 claims 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 26
- 239000011787 zinc oxide Substances 0.000 description 13
- 229910000859 α-Fe Inorganic materials 0.000 description 12
- 239000000203 mixture Substances 0.000 description 11
- 230000006872 improvement Effects 0.000 description 9
- 230000000996 additive effect Effects 0.000 description 8
- 238000000465 moulding Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 description 1
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000001012 protector Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2608—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
- C04B35/2633—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2658—Other ferrites containing manganese or zinc, e.g. Mn-Zn ferrites
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- 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
- H01F1/34—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 non-metallic substances, e.g. ferrites
- H01F1/36—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 non-metallic substances, e.g. ferrites in the form of particles
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3239—Vanadium oxides, vanadates or oxide forming salts thereof, e.g. magnesium vanadate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3256—Molybdenum oxides, molybdates or oxide forming salts thereof, e.g. cadmium molybdate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/608—Green bodies or pre-forms with well-defined density
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Soft Magnetic Materials (AREA)
Abstract
The invention discloses a soft magnetic material with high magnetic conductivity, high frequency and high impedance characteristics, which comprises main materials and auxiliary materials, wherein the main materials comprise: fe2O348-57 mol%, ZnO 18-25 mol%, MnO 21-28 mol%; the auxiliary materials comprise: 0.01-0.06 wt% of CaO, MoO3 0.02～0.07wt％，V2O5 0.02～0.08wt％，ZrO0.010～0.070wt％、Nb2O50.020 to 0.090 wt%. Correspondingly, the invention also provides a preparation method of the soft magnetic material with high magnetic conductivity, high frequency and high impedance. The soft magnetic material prepared by the invention has basically no attenuation between the magnetic permeability of 200KHZ and the magnetic permeability of 10KHZ, and has higher impedance than the common 10000 mu i.
Description
Technical Field
The invention relates to the field of special materials for electronic equipment, in particular to a magnetic material, and more particularly relates to a soft magnetic material with high magnetic permeability and high-frequency high-impedance characteristics.
Background
With the miniaturization development of electronic instruments and electronic equipment, matched magnetic core products are required to be smaller in volume and higher in performance. There are 4 requirements in summary: the initial magnetic conductivity requirement is high, the magnetic conductivity is high in broadband, the impedance is high in high frequency, and the magnetic conductivity is low in stress sensitivity.
The development direction of seeking for small size, low loss, high efficiency and light weight of electronic devices in a circuit is a development direction, and products with high magnetic conductivity are generally used in common-mode filters of high-frequency switching power supplies, saturated inductors, current transformers, leakage protectors, insulation transformers and signal and pulse transformers, wherein the filters of the switching power supplies and the high-frequency converters are used most widely.
With the continuous improvement of the requirement of the current electrical appliance on EMI, how to effectively reduce and inhibit the high-frequency clutter interference in a power circuit is the main task of a high-frequency filter, however, the magnetic permeability of the existing material under the condition of 10KHZ is about 10000, but the magnetic permeability of 200KHZ is only about 5000-7000, and the falling amplitude reaches 40% -50%. The prior art can not solve the high-frequency impedance characteristic of the manganese-zinc ferrite ui 10000 material, which leads to the adoption of the filter made of the existing magnetic material, and the filter has more coils, large magnetic core volume and high cost.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a soft magnetic material with high magnetic conductivity, high frequency and high impedance, and the prepared soft magnetic material has basically no attenuation between the magnetic conductivity of 200KHZ and the magnetic conductivity of 10KHZ, and has higher impedance than the general 10000 mu i.
The technical problem to be solved by the invention is to provide a method for preparing a soft magnetic material with high magnetic conductivity, high frequency and high impedance characteristics, which has the advantages of simple process, low cost and strong practicability.
In order to achieve the technical effects, the invention provides a soft magnetic material with high magnetic conductivity, high frequency and high impedance characteristics, which comprises a main material and an auxiliary material, wherein,
the main materials comprise: fe2O3 48～57mol％、ZnO 18～25mol％、MnO 21～28mol％；
The auxiliary materials comprise: 0.01-0.06 wt% of CaO, MoO3 0.02～0.07wt％，V2O5 0.02～0.08wt％， ZrO 0.010～0.070wt％、Nb2O5 0.020～0.090wt％。
As an improvement of the scheme, the coating also comprises an additive, wherein the additive comprises deionized water, a PVA solution and a defoaming agent;
the adding amount of the deionized water accounts for 10-30 wt% of the total weight of the main materials and the auxiliary materials;
the adding amount of the PVA solution accounts for 1-3 wt% of the total weight of the main material and the auxiliary material, and the concentration of the PVA solution is 0.8-1.2%;
the addition amount of the defoaming agent accounts for 0.1 to 1 weight percent of the total weight of the main material and the auxiliary materials。
As an improvement of the scheme, under the test condition of 10KHZ 0.05V, the magnetic permeability mu i of the soft magnetic material at 25 ℃ is 10000-; under the test condition of 200KHZ 0.05V, the magnetic permeability mu i of the soft magnetic material at 25 ℃ is 9500-11000 min; and satisfies mu i200KHZ/μi10KHZ＝95-96％min。
As an improvement of the proposal, the Curie temperature Tc of the soft magnetic material with high magnetic permeability, high frequency and high impedance characteristic is more than or equal to 130 ℃, and the density rho thereof is more than 5.00 multiplied by 103kg/m3And the saturation magnetic flux density Bs is more than or equal to 400mT at the temperature of 25 ℃.
Correspondingly, the invention also provides a preparation method of the soft magnetic material with high magnetic permeability, high frequency and high impedance, which comprises the following steps:
step A: proportioning the content of the main materials, adding deionized water into a sand mill for mixing and crushing, and adding a PVA solution after recycling and mixing;
and B: putting the crushed and mixed main materials into a pre-burning furnace for pre-burning;
and C: proportioning the content of the auxiliary materials of the pre-sintered main materials, then putting the powder containing the main materials and the auxiliary materials into a sand mill, adding deionized water, PVA and a defoaming agent, and carrying out secondary sand milling to prepare a ground powder material with the granularity of 0.65-0.85 mu m;
step D: carrying out spray granulation on the ground powder to prepare spray powder with the particle size of 50-200 mu m, and then carrying out compression molding on the spray powder to prepare the spray powder with the density of 3.00-3.10 g/cm3The green compact of (a);
step E: and sintering and shaping the green body in an atmosphere furnace at the temperature of 1400-1440 ℃, and cooling to obtain the soft magnetic material.
As an improvement of the above scheme, in the step a: the crushing lasts for 25-35 minutes, and the circular mixing lasts for 8-15 minutes.
As an improvement of the above scheme, in the step B: the temperature in the pre-burning furnace is controlled to be 850-950 ℃, and the heat preservation of the pre-burning furnace lasts for 2.5-3.5 hours.
As an improvement of the above scheme, in the step C: the duration time of the secondary sanding is 100-140 minutes.
As an improvement of the above scheme, in the step E: the oxygen partial pressure in the sintering atmosphere is 10-21%, and the balance is nitrogen partial pressure.
As an improvement of the above scheme, in the step E: the cooling is carried out in a controlled nitrogen-oxygen atmosphere to room temperature, wherein the oxygen content at the temperature of the cooling section 1300-sintering temperature is set to be 2-3%, the oxygen content at the temperature of the cooling section 1000-1300 is set to be 0.03-0.05%, and the oxygen content below 1000 ℃ is set to be 0.005-0.01%.
The implementation of the invention has the following beneficial effects:
the invention adopts three main components and additive combination to match, and is prepared by mixing raw materials, presintering, adding additives, molding and sintering; the main component formula is based on subsequent combined additives, the unique additive combination is adopted to promote the prepared green compact to be easy to sinter, increase the grain size, reduce air holes, grow more uniform and refined grain distribution, and simultaneously control the grain boundary porosity to generate a compact and uniform microstructure and form a higher sintering density, thereby obtaining the soft magnetic material with higher magnetic conductivity and high-frequency impedance characteristic.
Compared with the traditional mu i-10000 magnetic core, the magnetic core and the inductance element made of the soft magnetic material have the advantages that the magnetic permeability is reduced within 5 percent and is basically leveled when tested under the condition of 200 KHZ; the traditional mu i-10000 magnetic core has only 5000-7000 mu i at 200KHZ, and the falling amplitude reaches 40% -50%; the peak value of the high-frequency impedance of the product is between 600KHZ and 700KHZ, and the impedance value after the frequency of 400KHZ is 1.3 to 1.5 times higher than the impedance of the conventional ui of 10000 by taking a standard ring H25 with 15 with 8 as an example, so that the product shows excellent impedance characteristics.
Therefore, the soft magnetic material prepared by the invention has basically no attenuation in the magnetic permeability of 200KHZ and the magnetic permeability of 10KHZ, and has higher impedance than general 10000 mu i, so that the filter coil of the power circuit has the characteristics of fewer turns, lower cost, better high-frequency filtering effect and the like, can inhibit higher-frequency harmonic waves in the circuit, and maintain the cleanness of the power supply.
Besides, the soft magnetic material has better high-frequency high-impedance characteristics, the high-temperature saturation magnetic flux density Bs and the high-temperature residual magnetic flux density Br of the soft magnetic material are also greatly different, and the Curie temperature of the soft magnetic material is obviously higher than that of a conventional magnetic core.
Drawings
FIG. 1 is a frequency characteristic curve of permeability of 10 KHZ-500 KHZ between the present invention and the conventional soft magnetic material;
FIG. 2 is the impedance frequency characteristic curve of the present invention and the conventional soft magnetic material at 1 KHZ-1 MHZ.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below.
The invention provides a soft magnetic material with high magnetic conductivity, high frequency and high impedance characteristics, which comprises main materials, wherein the main materials comprise: fe2O348-57 mol%, ZnO 18-25 mol% and MnO 21-28 mol%. Preferably, the main materials comprise: fe2O3 50～55mol％、ZnO 20～25mol％、MnO 23～28mol％。
On the basis of the main materials, the soft magnetic material is also added with additives, wherein the additives comprise deionized water, PVA solution and defoaming agent;
the adding amount of the deionized water accounts for 10-30 wt% of the total weight of the main materials and the auxiliary materials;
the adding amount of the PVA solution accounts for 1-3 wt% of the total weight of the main material and the auxiliary material, and the concentration of the PVA solution is 0.8-1.2%;
the addition amount of the defoaming agent accounts for 0.1 to 1 weight percent of the total weight of the main material and the auxiliary materials。
Preference is given toIn the above-mentioned manner,the additive comprises deionized water, PVA solution and a defoaming agent;
the adding amount of the deionized water accounts for 12-15 wt% of the total weight of the main material and the auxiliary material;
the PVA solution accounts for 1.4-2 wt% of the total weight of the main material and the auxiliary material, the concentration of the PVA solution is 0.95-1%, and the concentration is percentage concentration.
The addition amount of the defoaming agent accounts for 0.1 to 0.5 weight percent of the total weight of the main material and the auxiliary materials。
The soft magnetic material with high magnetic conductivity, high frequency and high impedance is prepared by matching three main components with an additive combination, mixing raw materials, pre-burning, adding the additive, molding and sintering; the main component formula is based on subsequent combined additives, the unique additive combination is adopted to promote the prepared green compact to be easy to sinter, increase the grain size, reduce air holes, grow more uniform and refined grain distribution, and simultaneously control the grain boundary porosity to generate a compact and uniform microstructure and form a higher sintering density, thereby obtaining the soft magnetic material with higher magnetic conductivity and high-frequency impedance characteristic.
In order to further optimize the sintering process, promote the growth of crystal grains in the magnetic core, reduce air holes, improve the density and improve the compactness and uniformity of the microstructure in the magnetic core, the invention also adds auxiliary materials. Relative to the total weight of the main component, the soft magnetic material also comprises the following auxiliary materials: 0.01-0.06 wt% of CaO, MoO3 0.02～0.07wt％，V2O5 0.02～0.08wt％，ZrO 0.010～0.070wt％、Nb2O5 0.020～0.090wt％。
Preferably, the auxiliary materials include: 0.01-0.04 wt% of CaO, MoO3 0.02～0.05wt％，V2O5 0.02～0.06wt％，ZrO 0.010～0.040wt％、Nb2O5 0.020～0.060wt％。
Under the test condition of 10KHZ 0.05V, the magnetic permeability mu i of the soft magnetic material at 25 ℃ is 10000-; under the test condition of 200KHZ 0.05V, the magnetic permeability mu i of the soft magnetic material at 25 ℃ is 9500-11000 min; and satisfies mu i200KHZ/μi10KHZ＝95-96％min。
Preferably, the magnetic permeability mu i of the soft magnetic material at 25 ℃ is 10000min under the test condition of 10KHZ 0.05V; under the test condition of 200KHZ 0.05V, the magnetic permeability mu i of the soft magnetic material at 25 ℃ is 9500 min; and satisfies mu i200KHZ/μi10KHZ＝95％min。
Compared with the traditional mu i-10000 magnetic core, the magnetic core and the inductance element made of the soft magnetic material have the advantages that the magnetic permeability is reduced within 5 percent and is basically leveled when tested under the condition of 200 KHZ; the traditional mu i-10000 magnetic core has only 5000-7000 mu i at 200KHZ, and the falling amplitude reaches 40% -50%; the peak value of the high-frequency impedance of the product is between 600KHZ and 700KHZ, and the impedance value after the frequency of 400KHZ is 1.3 to 1.5 times higher than the impedance of the conventional ui of 10000 by taking a standard ring H25 with 15 with 8 as an example, so that the product shows excellent impedance characteristics. The soft magnetic material is used in various frequency converter filter circuits, can effectively inhibit various high-frequency harmonic waves and achieve the effect of purifying a power supply, and is popularized and used in various occasions such as high-frequency power supplies, high-frequency inverters, variable-frequency air conditioners, solar inverters and the like. For a filter with definite impedance requirement in a high frequency band, the soft magnetic material provided by the invention has high impedance and enough margin, so that the number of turns or the volume of a magnetic core can be reduced, the cost is reduced, and the filter has a wide market prospect.
The Curie temperature Tc of the soft magnetic material with high magnetic permeability, high frequency and high impedance characteristics is more than or equal to 130 ℃, and the density rho of the soft magnetic material is more than 5.00 multiplied by 103kg/m3And the saturation magnetic flux density Bs is more than or equal to 400mT at the temperature of 25 ℃. The soft magnetic material has better high-frequency high-impedance characteristics, the high-temperature saturation magnetic flux density Bs and the high-temperature residual magnetic flux density Br of the soft magnetic material are greatly different, and the Curie temperature of the soft magnetic material is obviously higher than that of a conventional magnetic core.
Correspondingly, the invention also provides a preparation method of the soft magnetic material with high magnetic permeability, high frequency and high impedance, which comprises the following steps:
step A: proportioning the content of the main materials, adding deionized water into a sand mill for mixing and crushing, and adding a PVA solution after recycling and mixing;
in the step A: the crushing lasts for 25-35 minutes, and the circular mixing lasts for 8-15 minutes, so that the crushing effect can be improved, and the main component process and the physical and chemical properties can be optimized.
And B: putting the crushed and mixed main materials into a pre-burning furnace for pre-burning;
in the step B: the temperature in the pre-sintering furnace is controlled to be 850-950 ℃, the heat preservation of the pre-sintering furnace lasts for 2.5-3.5 hours, the main component process and the physical and chemical properties can be further optimized, and the crystal structure of the subsequent sintering reaction is improved.
And C: proportioning the content of the auxiliary materials of the pre-sintered main materials, then putting the powder containing the main materials and the auxiliary materials into a sand mill, adding deionized water, PVA and a defoaming agent, and carrying out secondary sand milling to prepare a ground powder material with the granularity of 0.65-0.85 mu m;
in the step C: the duration time of the secondary sanding is 100-140 minutes.
Step D: carrying out spray granulation on the ground powder to prepare spray powder with the particle size of 50-200 mu m, and then carrying out compression molding on the spray powder to prepare the spray powder with the density of 3.00-3.10 g/cm3The green compact of (1).
The spray powder with the particle size of 50-200 mu m has good fluidity, and is convenient for full and uniform filling during molding and pressing; the density is 3.00-3.10 g/cm3The green body is beneficial to forming in a die with the shrinkage ratio of 80-85%.
Step E: and sintering and shaping the green body in an atmosphere furnace at the temperature of 1400-1440 ℃, and cooling to obtain the soft magnetic material.
In the step E: firstly, carrying out heat preservation sintering at the temperature of 1400-1440 ℃, and then cooling. Wherein,
for heat preservation sintering, the oxygen partial pressure in the sintering atmosphere of the heat preservation section with the highest temperature is 10-21%, the sintering tends to the atmosphere with high oxygen content, and the magnetic conductivity is improved; the balance of the other atmosphere is nitrogen partial pressure. In the existing sintering, the oxygen partial pressure of the heat preservation section is less than 10 percent.
Cooling is carried out in a controlled nitrogen-oxygen atmosphere up to room temperature. Specifically, the cooling is performed in a nitrogen-oxygen atmosphere, and according to the Nernst equation lgPO2 ═ K1/T + K2, the oxygen content in the cooling zone 1300 ℃ to the sintering temperature is set to 2 to 3%, the oxygen content in the cooling zone 1000 ℃ to 1300 ℃ is set to 0.03 to 0.05%, and the oxygen content at 1000 ℃ or less is set to 0.005 to 0.01%. The balance of the other atmosphere is nitrogen partial pressure.
Preferably, the cooling is carried out in an oxygen-nitrogen atmosphere, wherein the oxygen content in the cooling section 1300 ℃ to the sintering temperature is 3%, the oxygen content in the cooling section 1000 ℃ to 1300 ℃ is 0.03%, and the oxygen content at 1000 ℃ or less is 0.01%, according to the Nernst equation lgPO2 ═ K1/T + K2. The balance of the other atmosphere is nitrogen partial pressure.
On the basis of the component formula, the preparation method of the soft magnetic material promotes the growth of crystal grains, reduces air holes and homogenizes the distribution of the crystal grains by setting the sintering process and matching with the main formula, and the soft magnetic material with high magnetic conductivity and high impedance is sintered; the soft magnetic material prepared by the preparation method is particularly suitable for being used as a power supply clutter filtering and power supply cleaning function in various high-frequency power supplies.
The invention is further illustrated by the following specific examples
Example 1
1. Preparing materials:
weighing Fe2O351.5mo 1%; 21.3mo 1% of ZnO; MnO of 27.2mo 1%, wherein the three raw materials are Taiwan Steel Red, Hunan Jinrui Trionga and Shanghai Jinghua zinc oxide, and 15 wt% of ionized water is added into a sand mill for mixing and crushing, the crushing is carried out for 45 minutes, the mixture is circularly mixed for 10 minutes, and then 1.4 wt% of PVA solution is added for spray granulation.
2. Pre-burning:
and putting the sprayed material into a presintering furnace, and preserving heat for 3 hours at 860 ℃ for presintering.
3. Secondary sanding:
adding the following auxiliary component Nb in percentage by weight of the pre-sintering material into the pre-sintering material2O50.020 wt%, CaO 0.04 wt%, MoO30.03 wt%, V2O50.02 wt% and ZrO 0.02 wt%.
And then putting the powder into a sand mill, adding 15 wt% of deionized water into the sand mill, and performing secondary sand milling, wherein the sand milling time is 60 minutes, and the granularity of the powder is controlled to be 0.9-1.05 mu m.
4. Spray granulation and forming:
adding 1.4 wt% of PVA and 0.05 wt% of defoaming agent into the secondary sanding, and then performing spray granulation in a spray tower to obtain particles of 50-200 mu m; then molding, wherein the density of the ring blank is 3.05g/cm3Left and right;
5. and (3) sintering:
setting the proportion of oxygen and nitrogen, and respectively carrying out heat preservation for 8 hours for sintering at the temperature of 1425 ℃, wherein the oxygen partial pressure during sintering in the heat preservation section is 7 hours, 20 percent and 1 hour, 12 percent;
then, according to the Nernst equation lgPO2 ═ K1/T + K2, the oxygen content at the 1300 ℃ sintering temperature of the cooling section was set to 3%, the oxygen content at the 1000 ℃ cooling section was set to 0.03%, and the oxygen content at 1000 ℃ or less was set to 0.01%, and the mixture was cooled to room temperature.
The sintered H25 x 15 x 8 samples were subjected to inductance testing using HP4284, SY8218 testing Bs, and the specific properties are shown in table 1:
as can be seen from Table 1, the magnetic permeability at 200kHz can completely reach more than 10000, and the magnetic permeability drops by only 1.5% compared with the drop at 10KHZ, so that the soft magnetic ferrite powder has high magnetic permeability and good high-frequency characteristic.
Example 2
1. Preparing materials:
weighing Fe2O351.35mo 1%; 21.3mo 1% of ZnO; MnO of 27.45mo 1%, wherein the three raw materials are respectively Korean EG iron red, Hunan Jinrui Trimano tetroxide and Shanghai Jinghua zinc oxide, and 15 wt% of ionized water is added into a sand mill for mixing and crushing, the crushing is carried out for 45 minutes, the mixture is circularly mixed for 10 minutes, and then 1.4 wt% of PVA solution is added for spray granulation.
2. Pre-burning:
and putting the sprayed material into a presintering furnace, and preserving heat for 3 hours at 860 ℃ for presintering.
3. Secondary sanding:
adding the following auxiliary component Nb in percentage by weight of the pre-sintering material into the pre-sintering material2O50.020 wt%, CaO 0.04 wt%, MoO30.03 wt%, V2O50.02 wt% and ZrO 0.02 wt%. And then putting the powder into a sand mill, adding 15 wt% of deionized water into the sand mill, and performing secondary sand milling, wherein the sand milling time is 60 minutes, and the granularity of the powder is controlled to be 0.9-1.05 mu m.
4. Spray granulation and forming:
adding 1.5 wt% of PVA and 0.03 wt% of defoaming agent into the secondary sanding, and then performing spray granulation in a spray tower to obtain particles of 50-200 mu m; then molding, wherein the density of the ring blank is 3.05g/cm3Left and right;
5. and (3) sintering:
setting the proportion of oxygen and nitrogen, and respectively carrying out heat preservation for 8 hours for sintering at the temperature of 1425 ℃, wherein the oxygen partial pressure during sintering in the heat preservation section is 7 hours, 20 percent and 1 hour, 12 percent;
then, according to the Nernst equation lgPO2 ═ K1/T + K2, the oxygen content at the 1300 ℃ sintering temperature of the cooling section was set to 3%, the oxygen content at the 1000 ℃ cooling section was set to 0.03%, and the oxygen content at 1000 ℃ or less was set to 0.01%, and the mixture was cooled to room temperature.
The sintered H25 x 15 x 8 samples were subjected to inductance testing using HP4284, SY8218 testing Bs, and the specific properties are shown in table 2:
as can be seen from Table 2, the magnetic permeability at 200kHz can completely reach more than 10000 and is slightly larger than 10KHZ, and the magnetic ferrite powder is high-quality soft magnetic ferrite powder with high magnetic permeability and high frequency characteristic.
Example 3:
1. preparing materials:
fe was similarly weighed2O351.6mo 1%; 21.3mo 1% of ZnO; MnO of 27.1mo 1%, wherein the three raw materials are respectively Korean EG iron red, Hunan Jinrui Trimethox tetroxide and Shanghai Jinghua zinc oxide, and 15 wt% of ionized water is added into a sand mill to enterMixing and crushing, crushing for 45 minutes, circularly mixing for 10 minutes, adding 1.4 wt% PVA solution, and performing spray granulation.
2. Pre-burning:
and putting the sprayed material into a presintering furnace, and preserving heat for 3 hours at 860 ℃ for presintering.
3. Secondary sanding:
adding the following auxiliary component Nb in percentage by weight of the pre-sintering material into the pre-sintering material2O50.020 wt%, CaO 0.04 wt%, MoO30.03 wt%, V2O50.02 wt% and ZrO 0.02 wt%. And then putting the powder into a sand mill, adding 15 wt% of deionized water into the sand mill, and performing secondary sand milling, wherein the sand milling time is 60 minutes, and the granularity of the powder is controlled to be 0.9-1.05 mu m.
4. Spray granulation and forming:
adding 1.4 wt% of PVA and 0.05 wt% of defoaming agent into the secondary sanding, and then performing spray granulation in a spray tower to obtain particles of 50-200 mu m; then molding, wherein the density of the ring blank is 3.05g/cm3Left and right;
5. and (3) sintering:
setting the proportion of oxygen and nitrogen, and respectively carrying out heat preservation for 8 hours for sintering at the temperature of 1425 ℃, wherein the oxygen partial pressure during sintering in the heat preservation section is 7 hours, 20 percent and 1 hour, 12 percent;
then, according to the Nernst equation lgPO2 ═ K1/T + K2, the oxygen content at the 1300 ℃ sintering temperature of the cooling section was set to 3%, the oxygen content at the 1000 ℃ cooling section was set to 0.03%, and the oxygen content at 1000 ℃ or less was set to 0.01%, and the mixture was cooled to room temperature.
The sintered H25 x 15 x 8 samples were tested for inductance using HP4284, SY8218 for Bs, and the specific properties are shown in table 3:
as can be seen from Table 3, the magnetic permeability at 200kHz can completely reach more than 10000, the magnetic permeability at 10KHZ is only slightly dropped, and the magnetic ferrite material is a high-magnetic-permeability soft magnetic ferrite material with good high-frequency characteristics.
Example 4
1. Preparing materials:
weighing Fe2O348.05mo 1%; 25.7mo 1% of ZnO; 26.25mo 1% of MnO, wherein the three raw materials are respectively Korean EG iron red, Hunan Jinrui Trimano tetroxide and Shanghai Jinghua zinc oxide, 15 wt% of ionized water is added into a sand mill for mixing and crushing, the crushing is carried out for 45 minutes, the mixture is circularly mixed for 10 minutes, then 1.4 wt% of PVA solution is added, and the mixture is subjected to spray granulation.
2. Pre-burning:
and putting the sprayed material into a presintering furnace, and preserving heat for 3 hours at 860 ℃ for presintering.
3. Secondary sanding:
adding the following auxiliary component Nb in percentage by weight of the pre-sintering material into the pre-sintering material2O50.050 wt%, CaO 0.01 wt%, MoO30.02 wt%, V2O50.02 wt% and ZrO 0.01 wt%. And then putting the powder into a sand mill, adding 15 wt% of deionized water into the sand mill, and performing secondary sand milling, wherein the sand milling time is 60 minutes, and the granularity of the powder is controlled to be 0.9-1.05 mu m.
4. Spray granulation and forming:
adding 1.4 wt% of PVA and 0.05 wt% of defoaming agent into the secondary sanding, and then performing spray granulation in a spray tower to obtain particles of 50-200 mu m; then molding, wherein the density of the ring blank is 3.05g/cm3Left and right;
5. and (3) sintering:
setting the proportion of oxygen and nitrogen, and respectively carrying out heat preservation for 8 hours for sintering at the temperature of 1425 ℃, wherein the oxygen partial pressure during sintering in the heat preservation section is 7 hours, 20 percent and 1 hour, 12 percent;
then, according to the Nernst equation lgPO2 ═ K1/T + K2, the oxygen content at the 1300 ℃ sintering temperature of the cooling section was set to 3%, the oxygen content at the 1000 ℃ cooling section was set to 0.03%, and the oxygen content at 1000 ℃ or less was set to 0.01%, and the mixture was cooled to room temperature.
The sintered H25 x 15 x 8 samples were subjected to inductance testing using HP4284, SY8218 testing Bs, and the specific properties are shown in table 4:
as can be seen from Table 4, the magnetic permeability at 200kHz can completely reach more than 10000 and is slightly larger than 10KHZ, and the magnetic ferrite powder is high-quality soft magnetic ferrite powder with high magnetic permeability and high frequency characteristic.
Example 5:
1. preparing materials:
fe was similarly weighed2O356.8mo 1%; 20.1mo 1% of ZnO; 23.1mo 1% of MnO, wherein the three raw materials are respectively Korean EG iron red, Hunan Jinrui Trimano tetroxide and Shanghai Jinghua zinc oxide, 15 wt% of ionized water is added into a sand mill for mixing and crushing, the crushing is carried out for 45 minutes, the mixture is circularly mixed for 10 minutes, then 1.4 wt% of PVA solution is added, and the mixture is subjected to spray granulation.
2. Pre-burning:
and putting the sprayed material into a presintering furnace, and preserving heat for 3 hours at 860 ℃ for presintering.
3. Secondary sanding:
adding the following auxiliary component Nb in percentage by weight of the pre-sintering material into the pre-sintering material2O50.090 wt%, CaO 0.06 wt%, MoO30.07 wt%, V2O50.08 wt% and ZrO 0.07 wt%. And then putting the powder into a sand mill, adding 15 wt% of deionized water into the sand mill, and performing secondary sand milling, wherein the sand milling time is 60 minutes, and the granularity of the powder is controlled to be 0.9-1.05 mu m.
4. Spray granulation and forming:
adding 1.4 wt% of PVA and 0.05 wt% of defoaming agent into the secondary sanding, and then performing spray granulation in a spray tower to obtain particles of 50-200 mu m; then molding, wherein the density of the ring blank is 3.05g/cm3Left and right;
5. and (3) sintering:
setting the proportion of oxygen and nitrogen, and respectively carrying out heat preservation for 8 hours for sintering at the temperature of 1425 ℃, wherein the oxygen partial pressure during sintering in the heat preservation section is 7 hours, 20 percent and 1 hour, 12 percent;
then, according to the Nernst equation lgPO2 ═ K1/T + K2, the oxygen content at the 1300 ℃ sintering temperature of the cooling section was set to 3%, the oxygen content at the 1000 ℃ cooling section was set to 0.03%, and the oxygen content at 1000 ℃ or less was set to 0.01%, and the mixture was cooled to room temperature.
The sintered H25 x 15 x 8 samples were tested for inductance using HP4284, SY8218 for Bs, and the specific properties are shown in table 5:
as can be seen from Table 5, the magnetic permeability at 200kHz can completely reach more than 10000, the magnetic permeability at 10KHZ is only slightly dropped, and the magnetic ferrite material is a high-magnetic-permeability soft magnetic ferrite material with good high-frequency characteristics.
In conclusion, the corresponding performance of the soft magnetic ferrite powder of the present invention and the conventional typical soft magnetic ferrite powder is shown in table 6 below,
from the above, the soft magnetic material of the invention has less attenuation of high frequency magnetic permeability, the magnetic permeability of 300KHZ can reach the level of 200KHZ of the conventional material, and the soft magnetic material is a good high frequency soft magnetic material.
The soft magnetic material embodiment and the traditional soft magnetic ferrite powder comparative example are adopted to be prepared into a T25 15 10 magnetic core product through voltage sharing, an inductance coil 10TS is prepared, 1 KHZ-500 KHZ inductance and magnetic permeability and 1 KHZ-1 MHZ impedance are respectively tested under the condition of 25 ℃, the graphs are shown in figures 1 and 2, and as can be seen from figures 1 and 2, the magnetic core and the inductance coil prepared by the soft magnetic material embodiment of the invention have the advantages that the magnetic permeability of 200KHZ and the magnetic permeability of 10KHZ are basically not attenuated, the high-frequency impedance of 500KHZ is 30% higher and the high-frequency performance is greatly improved compared with the traditional magnetic core and the inductance coil.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (9)
1. A soft magnetic material with high magnetic conductivity, high frequency and high impedance is characterized by comprising a main material and an auxiliary material, wherein,
the main materials comprise: fe2O3 48～57mol％、ZnO 18～25mol％、MnO 21～28mol％；
The auxiliary materials comprise: 0.01-0.06 wt% of CaO, MoO3 0.02～0.07wt％，V2O5 0.02～0.08wt％，ZrO 0.010～0.070wt％、Nb2O5 0.020～0.090wt％；
Under the test condition of 10kHz 0.05V, the magnetic permeability mu i of the soft magnetic material at 25 ℃ is 10000-11000 min; under the test condition of 200kHz 0.05V, the magnetic permeability mu i of the soft magnetic material at 25 ℃ is 9500-11000 min; and satisfies mu i200KHZ/μi10KHZ＝95-96％min。
2. The soft magnetic material of high permeability, high frequency, high impedance characteristic of claim 1, further comprising additives comprising deionized water, PVA solution, defoamer;
the adding amount of the deionized water accounts for 10-30 wt% of the total weight of the main materials and the auxiliary materials;
the adding amount of the PVA solution accounts for 1-3 wt% of the total weight of the main material and the auxiliary material, and the concentration of the PVA solution is 0.8-1.2%;
the addition amount of the defoaming agent accounts for 0.1 to 1 weight percent of the total weight of the main material and the auxiliary materials。
3. The soft magnetic material with high permeability, high frequency and high impedance characteristics according to any of claims 1 to 2, wherein the soft magnetic material with high permeability, high frequency and high impedance characteristics has a Curie temperature Tc of 130 ℃ or more and a density p > 5.00 x 103kg/m3And the saturation magnetic flux density Bs is more than or equal to 400mT at the temperature of 25 ℃.
4. A method for preparing a soft magnetic material of high permeability, high frequency and high impedance characteristics according to any of claims 1 to 3, comprising:
step A: proportioning the content of the main materials, adding deionized water into a sand mill for mixing and crushing, and adding a PVA solution after recycling and mixing;
and B: putting the crushed and mixed main materials into a pre-burning furnace for pre-burning;
and C: proportioning the content of the auxiliary materials of the pre-sintered main materials, then putting the powder containing the main materials and the auxiliary materials into a sand mill, adding deionized water, PVA and a defoaming agent, and carrying out secondary sand milling to prepare a ground powder material with the granularity of 0.65-0.85 mu m;
step D: carrying out spray granulation on the ground powder to prepare spray powder with the particle size of 50-200 mu m, and then carrying out compression molding on the spray powder to prepare the spray powder with the density of 3.00-3.10 g/cm3The green compact of (a);
step E: and sintering and shaping the green body in an atmosphere furnace at the temperature of 1400-1440 ℃, and cooling to obtain the soft magnetic material.
5. The method for preparing a soft magnetic material with high permeability, high frequency and high impedance characteristics according to claim 4, wherein in the step A: the crushing lasts for 25-35 minutes, and the circular mixing lasts for 8-15 minutes.
6. The method for preparing a soft magnetic material with high permeability, high frequency and high impedance characteristics according to claim 4, wherein in the step B: the temperature in the pre-burning furnace is controlled to be 850-950 ℃, and the heat preservation of the pre-burning furnace lasts for 2.5-3.5 hours.
7. The method for preparing a soft magnetic material with high permeability, high frequency and high impedance characteristics according to claim 4, wherein in the step C: the duration time of the secondary sanding is 100-140 minutes.
8. A method for preparing a soft magnetic material with high permeability, high frequency and high impedance characteristics according to claim 4, wherein in the step E: the oxygen partial pressure in the sintering atmosphere is 10-21%, and the balance is nitrogen partial pressure.
9. A method for preparing a soft magnetic material with high permeability, high frequency and high impedance characteristics according to claim 4, wherein in the step E: the cooling is carried out in a controlled nitrogen-oxygen atmosphere to room temperature, wherein the oxygen content at the temperature of the cooling section 1300-sintering temperature is set to be 2-3%, the oxygen content at the temperature of the cooling section 1000-1300 is set to be 0.03-0.05%, and the oxygen content below 1000 ℃ is set to be 0.005-0.01%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711259872.XA CN108017383B (en) | 2017-12-04 | 2017-12-04 | Soft magnetic material with high magnetic conductivity and high frequency and high impedance characteristics and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711259872.XA CN108017383B (en) | 2017-12-04 | 2017-12-04 | Soft magnetic material with high magnetic conductivity and high frequency and high impedance characteristics and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108017383A CN108017383A (en) | 2018-05-11 |
| CN108017383B true CN108017383B (en) | 2021-01-15 |
Family
ID=62078432
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711259872.XA Active CN108017383B (en) | 2017-12-04 | 2017-12-04 | Soft magnetic material with high magnetic conductivity and high frequency and high impedance characteristics and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108017383B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003306376A (en) * | 2002-04-10 | 2003-10-28 | Jfe Steel Kk | MANUFACTURING METHOD OF Mn-Zn FERRITE |
| CN101106003A (en) * | 2006-07-12 | 2008-01-16 | 横店集团东磁有限公司 | Mn-Zn ferrite with ultrahigh magnetic conductivity and high Curie temperature and preparation method thereof |
| CN102063989A (en) * | 2010-10-20 | 2011-05-18 | 乳源东阳光磁性材料有限公司 | High-saturation magnetic flux, high-direct current superposition and low-loss soft magnetic material and preparation method thereof |
| CN105541316A (en) * | 2015-12-16 | 2016-05-04 | 横店集团东磁股份有限公司 | Manganese zinc ferrite material for resisting EMI and preparation method thereof |
-
2017
- 2017-12-04 CN CN201711259872.XA patent/CN108017383B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003306376A (en) * | 2002-04-10 | 2003-10-28 | Jfe Steel Kk | MANUFACTURING METHOD OF Mn-Zn FERRITE |
| CN101106003A (en) * | 2006-07-12 | 2008-01-16 | 横店集团东磁有限公司 | Mn-Zn ferrite with ultrahigh magnetic conductivity and high Curie temperature and preparation method thereof |
| CN102063989A (en) * | 2010-10-20 | 2011-05-18 | 乳源东阳光磁性材料有限公司 | High-saturation magnetic flux, high-direct current superposition and low-loss soft magnetic material and preparation method thereof |
| CN105541316A (en) * | 2015-12-16 | 2016-05-04 | 横店集团东磁股份有限公司 | Manganese zinc ferrite material for resisting EMI and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108017383A (en) | 2018-05-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107129291B (en) | With high frequency low-temperature coefficient low-loss MnZn soft magnetic ferrite and preparation method thereof | |
| CN107555984B (en) | A kind of ferritic sintering process control climate methods of high frequency wide-temperature and low-consumption MnZn | |
| CN110156451B (en) | High-impedance lean-iron manganese-zinc ferrite material and preparation method thereof | |
| CN107311637A (en) | A kind of method that low-power consumption manganese-zinc ferrite is prepared based on core shell structure crystal grain | |
| CN101575206A (en) | High-frequency high-power Ni-Zn base magnetic ferrite material and manufacturing method thereof | |
| CN104402424B (en) | High saturation magnetic flux density, high DC stacked, high-curie temperature nickel-zinc-ferrite material and preparation method thereof | |
| CN105367048A (en) | Manganese zinc ferrite material and preparation technology thereof | |
| CN110204325B (en) | Ferrite material and preparation method thereof | |
| CN110156449A (en) | A kind of high reliability Ferrite Material and preparation method thereof | |
| CN103833346B (en) | Wideband MnZn ferrite material and preparation process thereof | |
| CN107352991A (en) | A kind of core shell structure MnZn/nickel zinc complex ferrite and preparation method thereof | |
| CN107352993A (en) | A kind of high frequency Mn-Zn soft magnetic ferrite and preparation method thereof | |
| CN110655397B (en) | Wide-temperature-range high-permeability low-loss NiCuZn soft magnetic ferrite material and preparation method thereof | |
| CN108863339B (en) | Wide-temperature-range low-loss MnZn ferrite material applied to high-frequency large-magnetic-field transformer | |
| CN108610037B (en) | Manganese-zinc high-permeability material with wide temperature range and high Curie temperature superposition and preparation method thereof | |
| CN112898007A (en) | Manganese-zinc ferrite material with super-rich iron and high magnetic flux density as well as preparation method and application thereof | |
| CN114156037A (en) | Iron-silicon-chromium soft magnetic powder material | |
| CN105384435A (en) | Manganese-zinc ferrite material with quaternary formula and ultrahigh Bs and preparation method | |
| CN110436911B (en) | Soft magnetic material, preparation method thereof and application thereof in automobile electronic system | |
| CN108017383B (en) | Soft magnetic material with high magnetic conductivity and high frequency and high impedance characteristics and preparation method thereof | |
| CN111362680A (en) | High-frequency low-loss FeMnZnNi ferrite material and preparation method thereof | |
| CN111848148B (en) | High Bs nickel-zinc ferrite and preparation method thereof | |
| CN107129292A (en) | One kind prepares the ferritic ionic association alternatives of high-performance MnZn | |
| CN112979302A (en) | Manganese-zinc power ferrite material and preparation method thereof | |
| CN113284731A (en) | High-frequency large-magnetic-field soft magnetic ferrite material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 528500 building 4, No.2, shashuihexi Road, Yanghe Town, Gaoming District, Foshan City, Guangdong Province Patentee after: GUANGDONG FOSHAN JINGANG MAGNETIC INDUSTRY Co.,Ltd. Patentee after: Foshan Ceramic Research Institute Group Co.,Ltd. Address before: 528500 building 4, No.2, shashuihexi Road, Yanghe Town, Gaoming District, Foshan City, Guangdong Province Patentee before: GUANGDONG FOSHAN JINGANG MAGNETIC INDUSTRY Co.,Ltd. Patentee before: FOSHAN CERAMIC RESEARCH INSTITUTE Co.,Ltd. |
|
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 528500 building 4, No.2, shashuihexi Road, Yanghe Town, Gaoming District, Foshan City, Guangdong Province Patentee after: GUANGDONG FOSHAN JINGANG MAGNETIC INDUSTRY Co.,Ltd. Patentee after: Guangdong Foshan Ceramic Research Institute Holding Group Co., Ltd Address before: 528500 building 4, No.2, shashuihexi Road, Yanghe Town, Gaoming District, Foshan City, Guangdong Province Patentee before: GUANGDONG FOSHAN JINGANG MAGNETIC INDUSTRY Co.,Ltd. Patentee before: Foshan Ceramic Research Institute Group Co., Ltd |