CN109133905A - A kind of preparation method of high magnetic conductivity soft-magnetic ferrite - Google Patents
A kind of preparation method of high magnetic conductivity soft-magnetic ferrite Download PDFInfo
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- CN109133905A CN109133905A CN201711447150.7A CN201711447150A CN109133905A CN 109133905 A CN109133905 A CN 109133905A CN 201711447150 A CN201711447150 A CN 201711447150A CN 109133905 A CN109133905 A CN 109133905A
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- ferrite
- preparation
- magnetic
- high magnetic
- magnetic conductivity
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 33
- 230000035699 permeability Effects 0.000 claims abstract description 16
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 5
- 229910052742 iron Inorganic materials 0.000 claims abstract description 5
- 230000004048 modification Effects 0.000 claims abstract description 5
- 238000012986 modification Methods 0.000 claims abstract description 5
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 4
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 4
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 4
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 3
- 229910052802 copper Inorganic materials 0.000 claims abstract description 3
- 239000010970 precious metal Substances 0.000 claims abstract description 3
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 3
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 26
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 16
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000011787 zinc oxide Substances 0.000 claims description 13
- 239000011572 manganese Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000011777 magnesium Substances 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 239000000395 magnesium oxide Substances 0.000 claims description 8
- 229910052681 coesite Inorganic materials 0.000 claims description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 229910052682 stishovite Inorganic materials 0.000 claims description 6
- 229910052905 tridymite Inorganic materials 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 235000006748 manganese carbonate Nutrition 0.000 claims description 3
- 239000011656 manganese carbonate Substances 0.000 claims description 3
- 229940093474 manganese carbonate Drugs 0.000 claims description 3
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 3
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 2
- 238000009955 starching Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 8
- 238000009472 formulation Methods 0.000 abstract description 4
- 238000005245 sintering Methods 0.000 description 12
- 238000000498 ball milling Methods 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 239000000654 additive Substances 0.000 description 6
- 239000004615 ingredient Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 229910003962 NiZn Inorganic materials 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 238000005469 granulation Methods 0.000 description 4
- 230000003179 granulation Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000001694 spray drying Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 235000019580 granularity Nutrition 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 description 2
- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 description 2
- 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 2
- HRZMCMIZSOGQJT-UHFFFAOYSA-N [Zn].[Mn].[Mg] Chemical compound [Zn].[Mn].[Mg] HRZMCMIZSOGQJT-UHFFFAOYSA-N 0.000 description 2
- 239000002518 antifoaming agent Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000009837 dry grinding Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 description 2
- GNMQOUGYKPVJRR-UHFFFAOYSA-N nickel(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Ni+3].[Ni+3] GNMQOUGYKPVJRR-UHFFFAOYSA-N 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 2
- -1 Bi2O 3 Chemical compound 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910017706 MgZn Inorganic materials 0.000 description 1
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 1
- 229910018605 Ni—Zn Inorganic materials 0.000 description 1
- RFIJBZKUGCJPOE-UHFFFAOYSA-N [Fe].[Ni].[Zn] Chemical compound [Fe].[Ni].[Zn] RFIJBZKUGCJPOE-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical compound [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 239000011010 synthetic spinel Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
- C04B35/2625—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 magnesium
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- 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
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- 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
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- 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
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- 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
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- 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
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- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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- C04B2235/762—Cubic symmetry, e.g. beta-SiC
- C04B2235/763—Spinel structure AB2O4
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Abstract
A kind of preparation method of high magnetic conductivity soft-magnetic ferrite, uses Mn, Mg, Fe, Zn element for principal component, element Ni without precious metal, first presses MnZn ferrite formulations, prepares synthesis MnZn ferrite prefiring material, then appropriate MgO, ZnO and Fe are added in second batch2O3And modified microelement Cu, Bi, Si, Ti etc. are doped modification, synthesize the MnMgZn complex ferrite with high magnetic permeability.
Description
Technical field
The invention belongs to soft magnetic ferrite technical fields, and in particular to a kind of material low cost, preparation process are simple, but have
There is the process for preparing soft-magnetic ferrite of high magnetic permeability.
Background technique
Soft magnetic materials is mainly a kind of important electronic functional material based on MnZn, nickel-zinc ferrite.MnZn soft magnet
Oxysome magnetic conductivity with higher, generally 2000 ~ 20000, Ni Zn ferrimagnet bulk permeability is lower, generally within 2000.With
Electronic product to miniaturization, inductance element also tends to minimize, improve soft magnetic materials magnetic conductivity be reduce inductance element
The key of volume.Currently, magnetic conductivity in 2000 or more ferrites generally based on MnZn, but due to manganese-zinc ferrite need exist
Nitrogen atmosphere sintering, preparation process require stringent, high production cost, while that there are frequency of use is low not for manganese zinc material with high magnetic permeability
Foot.And nickel-zinc ferrite is needed using expensive nickel oxide as raw material, material cost is high, while the nickel zinc iron of 2000 or more magnetic conductivity
Oxysome is all very high to raw material, Recipe requirement, is difficult to stablize mass production, therefore the nickel zinc magnetic of 2000 or more magnetic conductivity
Core is expensive, and magnetic conductivity is higher reaches 3000 or more and substantially can produce without producer.Therefore magnetic conductivity is between MnZn
Between material and nickel zinc material in 2000 ~ 4000 ranges, there is inexpensive, simple process soft magnetic materials a piece of sky at present
It is white.
Since MnZn soft magnetic ferrite preparation process is stringent, height is required to physicochemical properties such as material purity, granularities, is needed simultaneously
Will be in nitrogen oxygen balance atmosphere sintering, complex process is at high cost, it is difficult to production cost be effectively reduced；NiZn soft magnetic ferrite due to
It needs with Ni2O3For raw material, material cost is high, although can reduce Ni using reducing material purity or passing through formula adjustment2O3With
Amount, but will cause material property reduce and it is unstable.Especially in the material of 2000 or more magnetic conductivity, existing Ni2O3Ferrite system
Standby technology is all difficult to steady production, therefore needs to find one kind and can reduce production cost and even improve magnetic
The formulation material of body comprehensive performance.
The present invention develops material principal component formula and microelement is modified, using unique work by selection suitable materials
Skill has been invented a kind of magnetic conductivity 2000 ~ 4000, has been sintered in air atmosphere, the manganese magnesium zinc soft magnet of nickel element without precious metal
The preparation method of oxysome.
Summary of the invention
The technical problem to be solved by the present invention is to soft magnet oxygen for magnetic conductivity in the prior art 2000 ~ 4000
Body is confined to MnZn ferrite or NiZn ferrite, all has the deficiency of high production cost, and it is low to provide a kind of manufacturing cost, uses
Roller kilns sintering has high magnetic permeability, the soft magnetic ferrite knot that comprehensive magnetic can compare favourably with similar NiZn ferrite
Preparation method.
The technical solution adopted by the present invention to solve the technical problems is as follows: a kind of preparation of high magnetic conductivity soft-magnetic ferrite
Method replaces the Ni element in NiZn ferrite using Mn, Mg element, forms the MnMgZn compound iron oxygen with high magnetic permeability
Body.In the crystal structure of ferrospinel, the trend that metal ion occupies A, B has certain tendentiousness, and sequence is
Zn2+、Cd2+、Mn2+、Fe3+、Mn3+、Fe2+、Mg2+、Cu2+、Co2+、Ti3+、Ni2+、Cr3+, ion more in front occupies A and inclines
Xiang Yueqiang；The tendency that ion more below occupies B is stronger.A small amount of Mn element mainly occupies B in ferrospinel.
Due to Mn2+With more Effect magnetic moment numbers, therefore B magnetic moments increase, Net magnetic moment increases,M sDullness is increased, magnetic conductivity increases
Add.When containing more Mn element, one side Mn element can occupy A and B, be unfavorable for Net magnetic moment increase, while Mn element
Concentration is excessive, will lead to Mn and appraises at the current rate, and a variety of valence state Mn ions occurs, material property is caused to decline, while sintered magnet holds
Easily there is surface oxidation phenomenon.Therefore, after a certain amount of Mn element is added, a certain amount of Mg element is added, due to Mg element
Not only A can take up, but also can take up B, so as to reduce the probability that Mn element occupies A, and the addition of Mg element,
Respectively replace part Zn and Fe where the position A and B, make Net magnetic moment keep do not decline.Therefore by the way that Mg element is added, balance is net
Magnetic moment reduces, it is ensured that Mn2+The variation of content influences Net magnetic moment maximum.Realizing to be formed has the MnMgZn of high magnetic conductivity compound
Ferrite.
A kind of preparation method of high magnetic conductivity soft-magnetic ferrite, uses Mn, Mg, Fe, Zn element for principal component, and be added
Cu, Bi, Si, Ti etc. are doped modification, improve material property, form high magnetic permeability MnMgZn complex ferrite.If by normal
The MnMgZn ferrite formulations and technique of rule are tested, and it is non-to reach 1000 generally between 400 ~ 800 for permeability
It is often difficult.Since manganese-zinc ferrite has a high magnetic conductivity, research is found first by MnZn ferrite formulations, with iron oxide (49 ~
54mol%), after zinc oxide (18 ~ 28mol%) and manganese carbonate (20 ~ 30mol%) prepare synthesis MnZn ferrite prefiring material, then two
Appropriate magnesia, zinc oxide and iron oxide and modified microelement are added in secondary ingredient, by high temperature sintering, these elements are mutual
It is molten into MnZn ferrite lattice, the MnMgZn ferrite of formation can keep high magnetic conductivity.
A kind of preparation method of high magnetic conductivity soft-magnetic ferrite carries out secondary match to the MnZn burning block after synthesis
Fe is added in material, supplement2O3,ZnO,MgO.Since Mg element both can take up A in ferrite lattice, it also can take up B
Feature, occupy A, B number, depend on its additional amount.The study found that therefore some addition range be it is interior, Mg element adds
Adding influences permeability less sensitive, but crystal morphology will generate variation, when MgO additive amount accounts for total ingredient (containing MnZn
Burning block): when 6 ~ 12wt%, sintered magnet crystal grain even compact, magnet strength is high, while material has high magnetic conductivity.Research
It was found that in a certain range, ZnO content increases, magnetic conductivity monotone increasing, equally in a certain range Fe2O3Content increases, magnetic
Conductance monotonic decreasing, but reach and keep after certain content stablizing, since material Curie temperature depends on iron oxide and zinc oxide
Ratio, while Fe2O3Content increase is conducive to improve material saturation flux density, therefore passes through control ZnO, Fe2O3Suitable addition
Amount, can take into account material Curie temperature and saturation flux density, and obtain high magnetic permeability.When second batch adds Fe2O3Content
(burning block containing MnZn) in 5 ~ 15 wt %, ZnO content in 6 ~ 18wt%, permeability, Curie temperature, saturation flux density are all
It is excellent.
Determine above-mentioned principal component, the influence invention further contemplates various microelements to material property, it is determined that
Add suitable modifying element and additive amount, including CuO, Bi2O 3、SiO2、TiO2.CuO, Bi of addition2O 3、SiO2It plays not
Same temperature range plays the role of solid solution to magnet sintering, can solve magnet sintering cracking, prevents manganese element that surface is precipitated,
Oxidation occurs and forms its phase substance, effect far superior to individually adds one such or two kinds effects.Bi simultaneously2O 3、
SiO2The effect of intensity can be improved with compactness magnet.And TiO2It can play in the methods of the invention and improve permeability
Permeability 10% or so can be improved in effect, suitable additive amount.Research obtains micro modifying element additive amount, with respective
The content of reference substance meter is as follows: CuO:0.2% ~ 8wt%, Bi2O 3: 0.05% ~ 0.4wt%, SiO2: 0.1% ~ 0.5wt%, TiO2:
0.05%~0.2wt%。
A kind of preparation method of high magnetic conductivity soft-magnetic ferrite, including Primary batching system, ball milling, pre-burning, two
Secondary ingredient, secondary ball milling mill, spray drying granulation, molding, sintering:
(1) various raw materials Primary batching system: are weighed by preparation MnZn burning block proportion.
(2) ball millings: it is carried out dry grinding 60 ~ 120 minutes in vibrator.
(3) pre-burning: the powder after the completion of a ball milling carries out pre-burning in kiln, and temperature is 940 ± 20 DEG C, when heat preservation
Between 120 ~ 180 minutes, preliminary synthetic spinel phase MnZn burning block.
(4) MgO, ZnO, Fe second batch: are weighed by the spinelle MgZn ferrite composition proportion2O3And modification is micro
Element is added in MnZn burning block.
(5) secondary ball milling: the material progress wet ball grinding after second batch, milling time 8 ~ 12 hours, Slurry Granularity control
System is at 1 ~ 1.5 μm.
(6) spray drying granulation: after the completion of secondary ball milling, the PVA solution that concentration is 8% is added in slurry, additive amount is
15 ~ 25%, 0.2 ~ 0.5 dispersing agent of addition, 0.05 ~ 0.2% defoaming agent, then ball milling 20 ~ 30 minutes, gained slurry is spray-dried
It is granulated, screens out thickness powder, take particle between wherein -120 mesh of 40 mesh, moisture is controlled 0.1 ~ 0.35%.
(7) it forms: 0.1 ~ 0.3% zinc stearate being added in conforming particle material, then 3.1g/cm is pressed in uniform mixing3It is raw
Base density compression moulding.
(8) be sintered: the air atmosphere sintering in roller kilns, 1150 ~ 1280 DEG C of sintering temperature keep the temperature 120 ~ 180 minutes.
The invention has the benefit that by replacing nickel oxide with manganese carbonate, magnesia, and it is modified by microelement,
The manganese magnesium zinc complex ferrite with high magnetic permeability is prepared, since without expensive nickel element, material cost significantly drops
It is low, while material has 2000 ~ 4000 magnetic conductivity, comprehensive performance is suitable with same type Ni-Zn soft magnetic ferrite.
Specific embodiment
The invention will be further described with reference to embodiments, but the present invention is not limited to these embodiments.
(1) Primary batching system: raw material is weighed by composition proportion described in table 1.
(2) ball millings: it is carried out dry grinding 60 minutes in vibrator, ball: material=4:1(weight ratio).
(3) pre-burning: the powder after the completion of a ball milling carries out pre-burning in ejection plate kiln, and temperature is 940 ± 20 DEG C, protects
120 minutes warm time.
(4) second batch: the selected micro modifying element of addition is weighed by accessory ingredient proportion.
(5) secondary ball milling: the powder after second batch carries out wet ball grinding, ball: material: water=2:1:0.5 is added 0.3%
Dispersing agent, 0.05% defoaming agent are ground 8 hours, and Slurry Granularity is controlled at 1 ~ 1.5 μm.
(6) spray drying granulation: the PVA solution that wet ball grinding slurry addition concentration is 8%, 15% ball milling 30 minutes, carry out
Spray drying granulation, moisture is controlled 0.1 ~ 0.35%.
(7) particle adjusts: the particle between 40 ~ 250 mesh of selection is taken after mist projection granulating, and 0.03 zinc stearate is added,
Particle adjusts machine, uniform mixing.
(8) form: green compact press 1.15 shrinking percentages, green compact height are calculated, by 3.1g/cm3Green density calculates substance, compacting
Molding.
(9) be sintered: the air atmosphere sintering in roller kilns, dumping stage (room temperature ~ 800 DEG C) heating rate be 150 DEG C/it is small
When, temperature rise period (800 DEG C ~ sintering temperature) heating rate is 200 DEG C/h, keeps the temperature 180 points after reaching heat preservation sintering temperature
Clock.Then furnace cooling.
Sintered magnet ring (T25*15*7) is tested and evaluated.
(1) under the conditions of the number of turns N=10Ts, with HP4284A type LCR electric bridge, frequency=1KHz is surveyed under the conditions of voltage=0.25V
Ring inductance is tried, magnet ring size is measured with digital calipers, calculates permeability.
(2) SY-8258 type B-H analyzer test sample saturation induction density Bs is used.
(3) insulating box and HP4284A type LCR bridge test Curie temperature are used.
1 MnZn burning block composition proportion of table
| Ingredient | Fe 2 O 3 | ZnO | MnCO 3 |
| Content (mol%) | 51 | 22 | 27 |
| Content (wt%) | 62.5 | 13.7 | 23.8 |
2 embodiment composition proportion of table
| Ingredient | MnZn burning block | Fe2O3 | MgO | ZnO | CuO | Bi2O 3 | CaCO 3 | SiO2 | TiO2 |
| Embodiment 1 (wt%) | 64 | 8 | 8 | 17 | 2.3 | 0.2 | 0.2 | 0.2 | 0.1 |
| Embodiment 2 (wt%) | 62 | 10 | 9 | 16 | 2.4 | 0.2 | 0 | 0.3 | 0.1 |
| Embodiment 3 (wt%) | 63 | 9 | 7 | 17 | 3.3 | 0.1 | 0.2 | 0.2 | 0.2 |
| Embodiment 4 (wt%) | 63 | 8 | 10 | 15 | 3.2 | 0.3 | 0.1 | 0.2 | 0.2 |
3 embodiment performance of table
| Project | Magnetic conductivity | Bs(25℃) | Insulation resistance | Curie temperature |
| Unit | mT | MΩ | ℃ | |
| Embodiment 1 | 2432 | 272 | >100 | >100 |
| Embodiment 2 | 2115 | 284 | >100 | >110 |
| Embodiment 3 | 2732 | 282 | >100 | >100 |
| Embodiment 4 | 2086 | 275 | >100 | >110 |
Table 2 lists embodiment performance, from Table 2, it can be seen that then the present invention is added using MnZn ferrite burning block is first synthesized
Add appropriate iron oxide, zinc oxide, magnesia, copper oxide and trace additives, the MnMgZn ferrite being prepared, tool
There is magnetic conductivity to be greater than 2000, while there is the good spy of the indexs such as saturation induction intensity and Curie temperature and insulation resistance
Property, fully meet the performance requirement of electromagnetism interference magnetic element, inductance element etc..
Specific embodiment described in the invention is only to be done to the present invention for example, the expert of correlative technology field
Or technical staff can make different degrees of modification, supplement to described specific embodiment or be substituted with similar mode, but
Without departing from the spirit of the invention or going beyond the scope defined by the appended claims.
Claims (4)
1. a kind of preparation method of high magnetic conductivity soft-magnetic ferrite: it is characterized in that using Mn, Mg, Fe, Zn element for principal component, no
Ni containing precious metal element, and Cu, Bi, Si, Ti is added etc. and is doped modification, material property is improved, high magnetic permeability is formed
MnMgZn complex ferrite.
2. the preparation method of a kind of high magnetic conductivity soft-magnetic ferrite according to claim 1, it is characterized in that first pressing MnZn iron
Oxysome formula: iron oxide (49 ~ 54mol%), zinc oxide (18 ~ 28mol%) and manganese carbonate (20 ~ 30mol%) prepare synthesis MnZn
Ferrite prefiring material.
3. the preparation method of a kind of high magnetic conductivity soft-magnetic ferrite according to claim 1, it is characterized in that in second batch
6 ~ 12wt% of middle addition magnesia, 6 ~ 18wt% of zinc oxide and 5 ~ 15 wt % of iron oxide and modified microelement CuO:0.2% ~
8wt%、Bi2O 3: 0.05% ~ 0.4wt%, SiO2: 0.1% ~ 0.5wt%, TiO2: 0.05% ~ 0.2wt% synthesizes MnMgZn compound iron oxygen
Body.
4. a kind of preparation method of high magnetic conductivity soft-magnetic ferrite according to claim 1, feature includes starching after grinding
Material granularity is controlled at 0.9 ~ 1.5 μm.
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| CN114871857A (en) * | 2022-04-19 | 2022-08-09 | 承德建龙特殊钢有限公司 | Tool for clamping metallographic specimen and specimen grinding and polishing method |
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