CN104973858A - Sintered permanent magnetic ferrite material and preparation method thereof - Google Patents

Sintered permanent magnetic ferrite material and preparation method thereof Download PDF

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Publication number
CN104973858A
CN104973858A CN201510280427.6A CN201510280427A CN104973858A CN 104973858 A CN104973858 A CN 104973858A CN 201510280427 A CN201510280427 A CN 201510280427A CN 104973858 A CN104973858 A CN 104973858A
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ball milling
sintered permanent
permanent magnet
preparation
magnet materials
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郭超阳
杨武国
李军华
吴云飞
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Hengdian Group DMEGC Magnetics Co Ltd
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Hengdian Group DMEGC Magnetics Co Ltd
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Abstract

The invention discloses a sintered permanent magnetic ferrite material and a preparation method thereof. The sintered permanent magnetic ferrite material has a chemical formula of A1-X-yCaxBiy(FE12-zZnz)nO19, wherein A is one or more than one element of Sr and Ba. x, y, z and n are molar ratios, wherein x is 0-0.08, y is 0.01-0.05, z is 0.01-0.1, and n is 0.97-1.0.The material is prepared from the specific processes of material blending, pre-sintering, ball milling, forming, and sintering. According to the invention, ion substitution of Ca, Bi, Zn and the like is carried out; the ball milling process is adjusted; the addition of secondary addition materials is controlled; and grain size and material orientation degree are controlled during a production process. The method has the following advantages: 1, ion substitution is carried out, wherein the substitution is realized mainly with Ca, Bi, and Zn, such that cost is reduced; 2, graded ball milling is combined with secondary ball milling, such that single-domain particles with a uniform size are obtained; material orientation degree is improved; and Br is increased; 3, secondary addition materials are controlled, and appropriate sintering curve temperatures are adopted, such that grains are refined, and sintering density is improved.

Description

A kind of sintered permanent magnet materials and preparation method thereof
Technical field
The present invention relates to ferrite permanent-magnet materials correlative technology field, refer in particular to a kind of sintered permanent magnet materials and preparation method thereof.
Background technology
Ferrite is that one has ferromagnetic metal oxide, is to be formed by the oxide compound of iron and other batching sintering.It is as one of electronic functional material, is widely used in the consumption such as manufacture and automobile, household electrical appliance, nucleus magnetic resonance of the electric installations such as motor, transformer, electronic instrument or the manufacture of medical facilities; Also apply to the fields such as the manufacture of the aerospace equipment such as the information equipments such as mobile telephone, computer, network appliance and aircraft, rocket, satellite simultaneously.
Recent two decades comes, in permanent-magnet ferrite material, breakthrough progress is achieved with the Japanese permanent-magnet ferrite manufacturer that TDK company is representative, the contour performance permanent-magnet ferrite product of FB9, FB12 series that released one after another, at the beginning of 2010, releases again more high performance FB13B/FB14H series product.Its technical characteristics is all based on Sr ferrite, combines substitutional ion by La-Co, thus the coercive force of Ferrite Material (Hcj) and residual flux density (Br) are highly improved.But these products, in order to obtain excellent performance further, must add more expensive rare earth element and rare metal Co etc., its production cost affects very large by factors such as material price such as rare earths.
China is rare earth big country, assume responsibility for the role of global rare earth supply in the past decades, but rare earth mining belongs to heavy polluted industry, adds that government lacks management and control always, exploits for a long time to have paid ceaselessly and destroys self natural surroundings and the cost consuming own resource.Within 2011, State Council has issued " the some suggestions about promoting rare-earth trade Sustainable Healthy Development ", has made a series of Important Adjustment, has caused rare earth price also to soar all the way thus, produce great effect to permanent magnet material industry to Rare-earth Industry.
Summary of the invention
There is above-mentioned deficiency to overcome in prior art in the present invention, provides a kind of low cost, high Br, high performance sintered permanent magnet materials and preparation method thereof.
To achieve these goals, the present invention is by the following technical solutions:
A kind of sintered permanent magnet materials, its chemical formula is A 1-x-yca xbi y(Fe 12-zzn z) no 19, wherein, A represents one or more elements in Sr, Ba, and x, y, z, n represent mol ratio, and x is 0 ~ 0.08, y be 0.01 ~ 0.05, z be 0.01 ~ 0.1, n is 0.97 ~ 1.0.
The present invention is added to basis with Ca, Bi, Zn combination, adds Zn replacement of fe, can improve ferrite saturation magnetization Ms, obtain high Br value.But add too much Zn, the reduction of magnetocrystalline anisotropy field can be made, cause Hcj sharply to decline.Ca to A replace be conducive to promoting sintering time crystal grain orientation degree, thus increase Br, but it is too low to add Ca, then sintered magnet can not high densification, and Br declines; Crystal grain will be caused too to grow up if too high, and produce abnormal grain, Hcj is declined.In addition, in formula, once add a small amount of Bi effectively can improve Br, but also effect of fluxing, reduce sintering temperature, increase density.The present invention utilizes Ca, Bi etc. to the replacement of A and Zn to the replacement of Fe, does not need to add expensive La, Co, just can make low cost, high Br, high performance permanent-magnet ferrite.
As preferably, described A represents Sr, and its starting compound comprises Fe 2o 3, SrCO 3, CaCO 3, ZnO and Bi 2o 3.
In addition, present invention also offers the preparation method of above-mentioned sintered permanent magnet materials, concrete operation step is as follows:
(1) prepare burden: by chemical formula A 1-x-ybi xca y(Fe 12-zzn z) no 19starting compound mixes by composition, adds primary material compound by weight percentage, is pulverized and mixed after mixing by wet ball-milling mode;
(2) pre-burning: after being dried by above-mentioned raw materials, be pressed into closely knit bulk, carry out pre-burning in air atmosphere, a heating and heat preservation, secondary temperature elevation is incubated, and lowers the temperature after three heating and heat preservation, broken with centrifugal crusher after the cooling of pre-burning body, obtain Preburning material;
(3) ball milling: take above-mentioned Preburning material, and add secondary addition material and dispersion agent in quality proportioning mode, adopt wet method mode to carry out secondary ball milling after mixing;
(4) shaping: above-mentioned slip vacuum pump is dewatered, shaping in magnetic field;
(5) sinter: gained magnet in step (4) is sintered in oxygen-enriched environment.
The present invention utilizes Ca, Bi etc. to the replacement of A and Zn to the replacement of Fe, by adjustment ball-milling technology and the interpolation controlling secondary addition material, in preparation process, the size of crystal grain and the orientation degree of material are controlled simultaneously, thus obtain a kind of low cost, high Br, high performance permanent-magnet ferrite product.
As preferably, in step (1), undertaken being pulverized and mixed 3 ~ 8h by wet ball-milling mode after mixing, the mean particle size of ball milling disposed slurry particle is less than 0.8um.Require the weight ratio controlling suitable water, material powder and steel ball during ball milling, if add water excess, will to cause pulverizing rear granular size uneven; After ball milling, if Slurry Granularity is excessive after mixed, in burn-in process, easily cause pre-burning insufficient, generate the ferritic content of M phase too low; If material grain is meticulous, then a Ball-milling Time also must be longer, causes Sr in compound to run off too much.
As preferably, in step (2), closely knit bulk is depressed at 5 ~ 10MP, in air atmosphere, carry out pre-burning, be warming up to 120 DEG C of insulation 1h, then be warming up to 300 DEG C of insulation 1h, and then be warming up to 1150 DEG C ~ 1250 DEG C, be incubated after 1 ~ 3 hour and lower the temperature, with the broken 5min of centrifugal crusher after the cooling of pre-burning body, obtain Preburning material.Pressure-controlling, at 5 ~ 10MP, to increase material inter-granular contact areas, contributes to solid state reaction and carries out; The reaction times of the pre-burning long or too high excessive grain that will cause of temperature is grown up, otherwise then reaction is carried out insufficient, is difficult to obtain premium quality product.
As preferably, in step (3), secondary addition material comprises CaCO 3, SiO 2, Al 2o 3, H 3bO 3, Cr 2o 3, dispersion agent is one or both in calglucon, Sorbitol Powder, and wherein, the addition of secondary addition material controls at CaCO 3: 0.1 ~ 1.0wt%; SiO 2: 0.1 ~ 0.6wt%; Al 2o 3: 0 ~ 0.2wt%; H 3bO 3: 0 ~ 0.4wt%; Cr 2o 3: 0.1 ~ 0.4wt%.Secondary adds a small amount of Al, Cr can improve Hcj, but due to Al be nonmagnetic, enter lattice too much, molecular magnetic moment can be made significantly to decline, and then Ms is declined, cause Br to reduce.H 3bO 3b is generated under high temperature 2o 3, with SiO 2and SrO generates liquid phase eutectic at a certain temperature, thus impel crystal grain homoepitaxial at a lower temperature, calcining temperature and sintered density can be reduced, be conducive to increasing sintered density, improve Br.SiO 2at high temperature with CaCO 3melt altogether, generate the Calucium Silicate powder of low melting point, can sintering temperature be reduced.Meanwhile, SiO 2can crystal boundary be formed, prevent grain growth, crystal grain thinning.But due to SiO 2be nonmagnetic, too much interpolation can cause Br to be deteriorated.
As preferably, in secondary addition material, the interpolation ratio of Ca/Si is 1.0 ~ 1.7.For addition material, the present inventor found through experiments, and control Si, Ca rationally add than being very important, very remarkable on product performance impact, so Ca/Si should be advisable with 1.0 ~ 1.7 in the present invention.
As preferably, in step (3), during secondary ball milling, first adopt and mix steel ball ball milling 15 ~ 20h, then use complete thin steel ball ball milling 5 ~ 8h, the mean particle size of ball milling disposed slurry particle is less than 0.7um, and size distribution is even.Control suitable water, powder, steel ball ratio during ball milling, in conjunction with grading ball milling during secondary ball milling, to obtain uniform single domain particle, thus be easy to orientation, improve material orientation degree; According to test, this method also can make Hcj improve 200Oe.
As preferably, in step (4), above-mentioned slip vacuum pump is dewatered, by moisture control 30% ~ 45%, and at 10000 ~ 14000GS magnetic field compacted under.If water ratio is too high, then molding time is long; Water ratio is too low, then slip mobility is very poor, causes product homogeneity to be deteriorated, and is unfavorable for magnetic field orientating.Forming magnetic field should at 10000 ~ 14000GS, thus improving product orientation degree as far as possible.
As preferably, in step (5), sintering temperature is 1150 ~ 1300 DEG C, insulation 1 ~ 3h.
The invention has the beneficial effects as follows: 1, ionic replacement, be mainly substituted by master with Ca, Bi, a Zn, do not need to add expensive La, Co, effectively reduce cost; 2, secondary ball milling is in conjunction with grading ball milling, to obtain uniform single domain particle, thus improves the orientation degree of material, effectively increases Br; 3, with the addition of CaCO in secondary addition material 3, SiO 2, H 3bO 3deng small powder, in conjunction with suitable sintering curre temperature, crystal grain thinning, and improve sintered density.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
All embodiments of the present invention are respectively with each material purity used in comparative example: Fe 2o 399%, SrCO 397%, CaCO 398.5%, ZnO99%, SiO 299.8%, Bi 2o 399.8%, Cr 2o 399.5%, Al 2o 399.3%, H 3bO 399%.
According to following table (table one) proportioning, the various starting compound of accurate weighing, wet ball grinding 5 hours.
Table one: primary material compound proportioning table (unit: g)
Numbering Fe 2O 3 SrCO 3 CaCO 3 ZnO Bi 2O 3 Main formula chemical formula
Embodiment 1 485.3 74.04 1.56 2.10 2.40 Sr 0.95Ca 0.03Bi 0.02Fe 11.75Zn 0.05O 19
Embodiment 2 485.3 2.60 0 2.10 6.00 Sr 0.95Bi 0.05Fe 11.75Zn 0.05O 19
Embodiment 3 485.3 71.90 4.22 0.43 1.21 Sr 0.91Ca 0.08Bi 0.01Fe 11.59Zn 0.01O 19
Embodiment 4 485.3 73.11 1.54 4.16 2.36 Sr 0.95Ca 0.03Bi 0.02Fe 11.9Zn 0.1O 19
Comparative example 1 485.3 74.04 1.56 2.10 2.40 Sr 0.95Ca 0.03Bi 0.02Fe 11.75Zn 0.05O 19
Comparative example 2 485.3 2.60 0 2.10 6.00 Sr 0.95Bi 0.05Fe 11.75Zn 0.05O 19
Comparative example 3 485.3 71.70 0 2.10 9.6 Sr 0.92Bi 0.08Fe 11.75Zn 0.05O 19
Comparative example 4 485.3 76.32 1.61 0 2.46 Sr 0.95Ca 0.03Bi 0.02F e11.4O 19
Comparative example 5 485.3 72.02 1.52 4.91 2.33 Sr 0.95Ca 0.03Bi 0.02Fe 12.08Zn 0.12O 19
Comparative example 6 485.3 70.15 5.20 2.10 0 Sr 0.9Ca 0.1Fe 11.75Zn 0.05O 19
Comparative example 7 485.3 77.61 0 0 0 SrFe 11.8O 19
By gained slip, put into oven drying 10 hours, design temperature is 120 DEG C.Again material is pressed into round pie under 10MP, puts into pit furnace pre-burning.Calcined temperature is set as being warming up to 120 DEG C of insulation 1h by initial temperature, then is warming up to 300 DEG C of insulation 1h, and then is warming up to 1230 DEG C of insulation 2h.By the gained Preburning material broken 5min of centrifugal crusher.
Take above-mentioned Preburning material 450g, and add secondary addition material and dispersion agent by following form (table two), secondary ball milling.Wherein comparative example 1 and comparative example 2 adopt mixing steel ball ball milling 24h, and all the other all adopt mixing steel ball ball milling 18h, then use complete thin steel ball ball milling 6h.
Table two: secondary addition material and dispersion agent proportioning table (unit wt%)
Numbering SiO 2 CaCO 3 Al 2O 3 Cr 2O 3 H 3BO 3 Calglucon
Embodiment 1 0.35 0.55 0.1 0.2 0.2 0.6
Embodiment 2 0.35 0.55 0.2 0.1 0 0.6
Embodiment 3 0.6 1.0 0 0.1 0.4 0.6
Embodiment 4 0.3 0.5 0.1 0.4 0.2 0.6
Comparative example 1 0.35 0.55 0.1 0.2 0.2 0.6
Comparative example 2 0.35 0.55 0.2 0.1 0 0.6
Comparative example 3 0.35 0.55 0 0.2 0 0.6
Comparative example 4 0.7 1.2 0.1 0.2 0.2 0.6
Comparative example 5 0.4 0.3 0 0.5 0.2 0.6
Comparative example 6 0.3 0.5 0.3 0 0.5 0.6
Comparative example 7 0.35 0.55 0.1 0.2 0.2 0.6
After ball milling after slip pumping for water pump to water ratio 30% ~ 45%, oriented moulding under 12000GS magnetic field, often group test compacting round pie Mao Pi two, compiles respectively as 1#, 2#, puts into box-type furnace and sinter.Heating up, it is identical with pre-burning to arrange, and 1# sintering temperature is set to 1220 DEG C, and 2# sintering temperature is set to 1225 DEG C, and insulation is all set to 1h.
After above-mentioned gained sample mill plane surface, test magnetic property, the data obtained is as shown in following table (table three):
Table three: properties of sample data logger
From table three data analysis, prepared sintered permanent ferrite Br can reach 4400 ~ 4500Gs, Br (Gs)+1/3Hcj (Oe) is greater than 5600 simultaneously, as can be seen here, after adopting Ca, Bi, Zn ionic replacement, significantly can improve Br, simultaneously reasonably secondary addition material and optimize ball-milling technology, also can obtain excellent Hcj, thus obtain premium quality product.

Claims (10)

1. a sintered permanent magnet materials, is characterized in that, its chemical formula is A 1-x-yca xbi y(Fe 12-zzn z) no 19, wherein, A represents one or more elements in Sr, Ba, and x, y, z, n represent mol ratio, and x is 0 ~ 0.08, y be 0.01 ~ 0.05, z be 0.01 ~ 0.1, n is 0.97 ~ 1.0.
2. a kind of sintered permanent magnet materials according to claim 1, is characterized in that, described A represents Sr, and its starting compound comprises Fe 2o 3, SrCO 3, CaCO 3, ZnO and Bi 2o 3.
3. a preparation method for sintered permanent magnet materials, is characterized in that, concrete operation step is as follows:
(1) prepare burden: by chemical formula A 1-x-ybi xca y(Fe 12-zzn z) no 19starting compound mixes by composition, adds primary material compound by weight percentage, is pulverized and mixed after mixing by wet ball-milling mode;
(2) pre-burning: after being dried by above-mentioned raw materials, be pressed into closely knit bulk, carry out pre-burning in air atmosphere, a heating and heat preservation, secondary temperature elevation is incubated, and lowers the temperature after three heating and heat preservation, broken with centrifugal crusher after the cooling of pre-burning body, obtain Preburning material;
(3) ball milling: take above-mentioned Preburning material, and add secondary addition material and dispersion agent in quality proportioning mode, adopt wet method mode to carry out secondary ball milling after mixing;
(4) shaping: above-mentioned slip vacuum pump is dewatered, shaping in magnetic field;
(5) sinter: gained magnet in step (4) is sintered in oxygen-enriched environment.
4. the preparation method of a kind of sintered permanent magnet materials according to claim 3, is characterized in that, in step (1), undertaken being pulverized and mixed 3 ~ 8h by wet ball-milling mode after mixing, the mean particle size of ball milling disposed slurry particle is less than 0.8um.
5. the preparation method of a kind of sintered permanent magnet materials according to claim 3, it is characterized in that, in step (2), depress to closely knit bulk at 5 ~ 10MP, in air atmosphere, carry out pre-burning, be warming up to 120 DEG C of insulation 1h, be warming up to 300 DEG C of insulation 1h again, and then be warming up to 1150 DEG C ~ 1250 DEG C, be incubated after 1 ~ 3 hour and lower the temperature, with the broken 5min of centrifugal crusher after the cooling of pre-burning body, obtain Preburning material.
6. the preparation method of a kind of sintered permanent magnet materials according to claim 3, is characterized in that, in step (3), secondary addition material comprises CaCO 3, SiO 2, Al 2o 3, H 3bO 3, Cr 2o 3, dispersion agent is one or both in calglucon, Sorbitol Powder, and wherein, the addition of secondary addition material controls at CaCO 3: 0.1 ~ 1.0wt%; SiO 2: 0.1 ~ 0.6wt%; Al 2o 3: 0 ~ 0.2wt%; H 3bO 3: 0 ~ 0.4wt%:Cr 2o 3: 0.1 ~ 0.4wt%.
7. the preparation method of a kind of sintered permanent magnet materials according to claim 6, is characterized in that, in secondary addition material, the interpolation ratio of Ca/Si is 1.0 ~ 1.7.
8. the preparation method of a kind of sintered permanent magnet materials according to claim 3 or 6 or 7, it is characterized in that, in step (3), during secondary ball milling, first adopt mixing steel ball ball milling 15 ~ 20h, use complete thin steel ball ball milling 5 ~ 8h again, the mean particle size of ball milling disposed slurry particle is less than 0.7um, and size distribution is even.
9. the preparation method of a kind of sintered permanent magnet materials according to claim 3, it is characterized in that, in step (4), above-mentioned slip vacuum pump is dewatered, by moisture control 30% ~ 45%, and at 10000 ~ 14000GS magnetic field compacted under.
10. the preparation method of a kind of sintered permanent magnet materials according to claim 3, is characterized in that, in step (5), sintering temperature is 1150 ~ 1300 DEG C, insulation 1 ~ 3h.
CN201510280427.6A 2015-05-28 2015-05-28 Sintered permanent magnetic ferrite material and preparation method thereof Pending CN104973858A (en)

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Cited By (8)

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Publication number Priority date Publication date Assignee Title
CN105384433A (en) * 2015-10-27 2016-03-09 横店集团东磁股份有限公司 Manufacturing method of permanent magnetic ferrite
CN110642615A (en) * 2019-10-25 2020-01-03 中磁电科有限公司 Preparation method of permanent magnetic ferrite magnetic material
CN111755193A (en) * 2019-03-27 2020-10-09 Tdk株式会社 Ferrite sintered magnet and rotating electrical machine provided with same
CN112919895A (en) * 2020-12-28 2021-06-08 横店集团东磁股份有限公司 Preparation method of magnet applying anisotropic dry-pressed ferrite fine powder
CN115043651A (en) * 2021-03-08 2022-09-13 Tdk株式会社 Ferrite sintered magnet and method for producing ferrite sintered magnet
US11521769B2 (en) 2019-03-27 2022-12-06 Tdk Corporation Ferrite sintered magnet and rotary electrical machine comprising the same
US11532413B2 (en) 2019-03-27 2022-12-20 Tdk Corporation Ferrite sintered magnet and rotary electrical machine comprising the same
US11626222B2 (en) 2019-10-18 2023-04-11 Tdk Corporation Ferrite sintered magnet and rotary electrical machine comprising the same

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CN101154491A (en) * 2006-09-26 2008-04-02 横店集团东磁股份有限公司 Permanent ferrite material added with nano constituent and sintered magnet and magnetic powder
CN102167576A (en) * 2011-01-15 2011-08-31 五邑大学 High performance permanent magnetic ferrite magnetic powder and method for preparing same
EP2452928A1 (en) * 2009-07-08 2012-05-16 TDK Corporation Ferrite magnetic material
CN102964120A (en) * 2012-08-31 2013-03-13 横店集团东磁股份有限公司 Sintered permanent magnetic ferrite and its preparation method

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Publication number Priority date Publication date Assignee Title
CN105384433A (en) * 2015-10-27 2016-03-09 横店集团东磁股份有限公司 Manufacturing method of permanent magnetic ferrite
CN111755193A (en) * 2019-03-27 2020-10-09 Tdk株式会社 Ferrite sintered magnet and rotating electrical machine provided with same
US11521769B2 (en) 2019-03-27 2022-12-06 Tdk Corporation Ferrite sintered magnet and rotary electrical machine comprising the same
US11532413B2 (en) 2019-03-27 2022-12-20 Tdk Corporation Ferrite sintered magnet and rotary electrical machine comprising the same
CN111755193B (en) * 2019-03-27 2023-02-10 Tdk株式会社 Ferrite sintered magnet and rotating electrical machine provided with same
US11610705B2 (en) 2019-03-27 2023-03-21 Tdk Corporation Ferrite sintered magnet and rotating electric machine comprising the same
US11626222B2 (en) 2019-10-18 2023-04-11 Tdk Corporation Ferrite sintered magnet and rotary electrical machine comprising the same
CN110642615A (en) * 2019-10-25 2020-01-03 中磁电科有限公司 Preparation method of permanent magnetic ferrite magnetic material
CN112919895A (en) * 2020-12-28 2021-06-08 横店集团东磁股份有限公司 Preparation method of magnet applying anisotropic dry-pressed ferrite fine powder
CN112919895B (en) * 2020-12-28 2022-02-18 横店集团东磁股份有限公司 Preparation method of magnet applying anisotropic dry-pressed ferrite fine powder
CN115043651A (en) * 2021-03-08 2022-09-13 Tdk株式会社 Ferrite sintered magnet and method for producing ferrite sintered magnet
CN115043651B (en) * 2021-03-08 2023-10-13 Tdk株式会社 Ferrite sintered magnet and method for producing ferrite sintered magnet

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Application publication date: 20151014