CN102924069B - Hexagonal crystal M+W mixed type sintered permanent magnetic ferrite magnet and preparation method thereof - Google Patents
Hexagonal crystal M+W mixed type sintered permanent magnetic ferrite magnet and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a hexagonal crystal M+W mixed type sintered permanent magnetic ferrite magnet and a preparation method thereof. The composition formula of the hexagonal crystal M+W mixed type sintered permanent magnetic ferrite magnet is represented by Cax1Srx2Bax3LaxFe2+aFe3+bOy, wherein x1 is 0.1-0.3, x2 is 0.2-0.5, x3 is 0.1-0.4, x is 0.1-0.3, a is 0.1-1.0, b is 12.0-14.0, 12.1<=a+b<=15.0, and y=1+1/2x+a+3/2b. Lanthanum oxide is added, the mole number of iron in the M type ferrite is enhanced, and the oxygen concentration in the sintering process is controlled to provide a appropriate non-oxidizing atmosphere so as to inhibit the generation of the alpha-Fe2O3 phase, so that the M+W mixed type magnetoplumbite structure can be generated in the original M type permanent magnetic ferrite. The invention has the following advantages: (1) compared with the single-phase M type ferrite, the invention enhances the residual flux density (Br) of the material, and maintains the high coercive force (Hcj); (2) compared with the single-phase W type ferrite, the invention has simpler production technique, and can perform industrial production only by slightly adjusting the M type permanent magnetic ferrite production technique; and (3) the magnet is free of rare and noble metal cobalt, and thus, the cost is lower.
Description
Technical field
The present invention relates to a kind of high-performance permanent-magnet ferrite magnet, relate to specifically the brilliant M+W mixed type of a kind of hexagonal sintered permanent ferrite magnet and preparation method thereof.
Technical background
M type Magnetoplumbite permanent magnetic ferrite magnet is the general name of the compound that consists of divalent cation metal oxide compound (SrO and BaO) and ferric oxide (Fe2O3), permanent-magnet ferrite magnet is widely applicable for automobile, household electrical appliance, the industries such as industrial automation.As permanent-magnet ferrite material, there is the strontium ferrites (SrFe of M type magnetoplumbite type
12o
19) and barium ferrite (BaFe
12o
19) be widely used.For M type ferrite magnet, be mainly conceived to make the particle diameter of ferrite crystal grains approach single domain particle diameter, make ferrite crystal grains arrange and carry out aspect densification, carrying out the effort of high performance always in magneticanisotropy direction.The result of this effort is that the magnetic property of M type ferrite magnet has approached its upper limit, is difficult to expect that magnetic property obtains tremendous raising.
As showing the magnetic property that is better than M type ferrite magnet, W type ferrite magnet is known.W type ferrite magnet is compared with M type ferrite magnet, and saturation magnetization (4 π Is) is high by approximately 10%, and anisotropy field is certain degree.In Chinese patent (publication number CN1082496C), a kind of W type ferrite magnet is disclosed, it is to be represented by SrO2 (FeO) n (Fe2O3), wherein n meets the composition of 7.2-7.7 and forms, the average crystal grain of its sintered compact be 2 μ m or following, (BH) max be 5 MGOe or more than.In Chinese patent (publication number CN100393664C), disclose a kind of W type ferrite magnet, it is by AFe
2+ afe
3+ bo
27represent component, at least a kind element of A for selecting, and 1.5≤a≤2.1,12.9≤b≤16.3 among Sr, Ba and Pb.By adding the optimizing of minor component, improve magnetic property, having obtained high magnetic characteristics is residual flux density (Br) 4600Gs, coercive force (Hcj) 3200Oe.
Summary of the invention
The object of this invention is to provide the brilliant M+W mixed type of a kind of hexagonal sintered permanent ferrite magnet and preparation method thereof, by adding the mole number of iron in lanthanum trioxide and raising M type ferrite, and the concentration of controlling oxygen in sintering process is to provide suitable nonoxidizing atmosphere to suppress the generation of α-Fe2O3 phase, can in former M type permanent-magnet ferrite, generate M+W mixed type magnetoplumbite type, thereby improved the residual flux density (Br) of ferrite sintered body, and kept higher coercive force (Hcj).
For realizing above object, the technical solution used in the present invention is as follows:
A brilliant M+W mixed type sintered permanent ferrite magnet, is characterized in that its composition formula Ca
x1sr
x2ba
x3la
xfe
2+ afe
3+ boy represents, wherein, x1 is 0.1-0.3, and x2 is 0.2-0.5, and x3 is 0.1-0.4, and x is 0.1-0.3, and a is 0.1-1.0, and b is 12.0-14.0,12.1≤a+b≤15.0, y=1+1/2x+a+3/2b.
The preparation method of the brilliant M+W mixed type of hexagonal sintered permanent ferrite magnet, is characterized in that, comprise the operations such as batching mixing, pre-burning, coarse reduction, ball milling, moulding and sintering, concrete steps are as follows:
(1) batching is mixed
Press Ca
x1sr
x2ba
x3la
xfe
2+ afe
3+ boy calculates and weighs calcium carbonate powders, strontium carbonate powder, barium carbonate powder, lanthanum oxide powder and the croci that contains required element.
Wherein: x1 is 0.1-0.3,
X2 is 0.2-0.5,
X3 is 0.1-0.4,
X is 0.1-0.3,
A is 0.1-1.0,
B is 12.0-14.0,
12.1≤a+b≤15.0,
y=1+1/2x+a+3/2b。
Above-mentioned load weighted powder is mixed by wet process, and mixing time is controlled at 3-5 hour, and mixed mixture mean particle size is not more than 1.0 μ m.If Slurry Granularity is excessive after mixing, in pre-burning process, easily cause that pre-burning is insufficient, make to generate the ferritic content of hexagonal crystalline phase too low;
(2) pre-burning
Said mixture material is carried out in air to pre-burning, calcined temperature is 1200-1350 ℃, and soaking time is 1-3 hour, obtains Preburning material particle;
(3) coarse reduction
Above-mentioned Preburning material particle is carried out to dry type ball mill pulverizing to mean particle size 3-5 μ m, obtain Preburning material powder;
(4) ball milling:
To above-mentioned Preburning material powder, in weight proportion mode, add secondary additive, gained mixture is adopted to wet ball-milling mode continuously grinding, until the mean particle size that reaches particle is at 0.7-0.8 μ m;
(5) moulding
The slip of above-mentioned steps gained is carried out to processed, and dewatering type can adopt centrifugation or press filtration mode to carry out, and is adjusted to pulp density at 60-65wt%, then carries out pressing under magnetic field, and forming magnetic field intensity is not less than 500 kA/m;
(6) sintering
Molding is carried out in nonoxidizing atmosphere to sintering, sintering temperature is 1150-1250 ℃, and insulation 1.0-3.0 hour, controls oxygen partial pressure by pass into nitrogen in sintering oven, and passing into of nitrogen, carries out in the temperature range between top temperature at 500 ℃.
In described proportion mixed process, also include additive silicon-dioxide and boric acid, its adding proportion is: silicon-dioxide 0.05-0.5wt%, boric acid 0.05-0.2wt%.
Described secondary additive comprises CaCO
3powder, SiO
2powder, Al
2o
3powder, Cr
2o
3powder, H
3bO
3powder, ZnO powder, Mn
3o
4one or more in powder, wherein the mean particle size of each compound powder is not more than 2.0 μ m, and the adding proportion of each additive is: CaCO
3: 0.3~1.5wt%, SiO
2: 0.1~1.0wt%, Al
2o
3: 0.1~1.5wt%, Cr
2o
3: 0.1~1.5wt%, H
3bO
3: 0.05~0.2wt%, ZnO:0.05~1.2wt%, Mn
3o
4: 0.05~1.5wt%.
Described secondary additive is also included in the carbon black of sintering circuit performance reductive action.
In described ball milling operation, need to add a certain amount of dispersion agent, described dispersion agent is one or more of calglucon, Sorbitol Powder, xitix etc., and addition is the 0.2-1.5wt% of total composition weight.
The brilliant M+W mixed type of hexagonal of the present invention sintered permanent ferrite magnet, has Br more than 4500Gs, Hcj more than 3500 Oe, 0.90 above rectangular degree (Hk/Hcj).
In sum, the present invention has the following advantages:
(1) compare the residual flux density (Br) that has improved material with single-phase M type ferrite, and kept higher coercive force (Hcj);
(2) simpler than single-phase W type ferrite production technique, on M type permanent-magnet ferrite production technique basis, slightly adjust, can carry out suitability for industrialized production;
(3) in magnet, do not contain rare precious metals cobalt, cost is lower.
Accompanying drawing explanation
Fig. 1 is process flow sheet.
Embodiment
Below by embodiment, technical scheme of the present invention is further described in detail: but the present invention is not limited to these embodiment.
Embodiment 1
The research of La addition:
Weigh the ferric oxide (Fe of specified amount
2o
30.7~1.0 μ m), calcium carbonate (CaCO) powder (the original mean particle size of purity>=99.0wt%, particle:
32.0~5.0 μ m), Strontium carbonate powder (SrCO) powder, (the original mean particle size of purity>=98.5wt%, particle:
31.0~2.0 μ m), barium carbonate (BaCO) powder (the original mean particle size of purity>=98.5wt%, particle:
31.0~2.0 μ m), lanthanum trioxide (La) powder (the original mean particle size of purity>=98.5wt%, particle:
2o
3) powder (the original mean particle size of purity>=99.0wt%, particle: 2.0~5.0 μ m), add the SiO of 0.3wt% in said mixture
21.0 μ m), the H of 0.1wt% powder (the original mean particle size of purity>=98.0wt%, particle:
3bO
3powder (purity>=99.0wt%) also carries out wet mixing, and after mixing, the mean particle size of mixture is 0.9 μ m.After mixture is dry, with 1280 ℃ of pre-burnings 2 hours in atmosphere.
The Preburning material particle of gained is carried out to dry type coarse reduction in vibrating mill, obtain the meal of mean particle size 3.0~5.0 μ m.
Then, take 500 grams, above-mentioned meal material, add the SiO of 0.25wt%
2, 0.60wt% CaCO
3, 0.80wt% Cr
2o
3, 0.10wt% H
3bO
3, 0.25wt% Al
2o
3, the ZnO of 0.20wt% is, the Mn of 0.25wt%
3o
4, the calglucon of 0.60wt% and the carbon black of 0.30wt%, then add the water of 700 milliliters, carry out case of wet attrition, obtain the ferrite slurry of mean particle size 0.75 μ m.
By after the slurry dewatering after Crushing of Ultrafine, in the parallel magnetic field of additional magneticstrength 700 kA/m, with forming pressure 0.4ton/cm
3carry out compressed moulding.The diameter of gained molding is the right cylinder of 40mm, height 15mm.
Temperature at 100-500 ℃ is heat-treated molding, removes moisture and organic dispersing agent, then to passing into nitrogen in sintering oven, controls oxygen concn, in nonoxidizing atmosphere, carry out sintering, heat-up rate is 120 ℃/h, 1200 ℃ of insulations 1.5 hours, obtains sintered permanent magnet.
Prepared ferrimagnet sample composition is analyzed, measured formula Ca
x1sr
x2ba
x3la
xfe
2+ afe
3+ bx1 in Oy, x2, x3, x, a, b, oxygen level y value (y=1+1/2x+a+3/2b) is to calculate and obtain according to valency balance principle.A (Fe
2+) mensuration adopt volumetry, the mensuration of x1, x2, x3, x, b adopts x-ray fluorescence analysis, principal phase state is measured with X-ray diffraction method.Measurement result is as shown in table 1.
Residual magnetic flux density (Br), HCJ (Hcj) and the rectangular degree (Hk/Hcj) of with magnetism testing instrument, measuring magnet sample, gained measured value is as shown in table 2.
Table 1
Table 2
Result from table 1 and table 2 shows, in ferrimagnet of the present invention, adds La
3+with generation Fe
2+between positive correlation.And can find out, x was at 0.1~0.3 o'clock, through strict technology controlling and process, rationally once and secondary adds and the control of sintering atmosphere, in the situation that magnet does not contain rare precious metals cobalt, can obtain Br more than 4500Gs completely, Hcj more than 3500 Oe, the brilliant M+W mixed type of the hexagonal sintered permanent ferrite magnet of 0.90 above rectangular degree (Hk/Hcj).Know that by analysis x was lower than 0.1 o'clock, La is insufficient to the displacement of hexagonal crystalline substance, Fe
2+growing amount not enough, also there is α-Fe2O3 phase, magnetic property is lower; And when x surpasses 0.3, the replacement of La is incomplete, also have α-Fe2O3 to generate mutually, magnetic property is also lower.
Embodiment 2
The mole number research of iron:
Use the ferric oxide (Fe identical with embodiment 1
2o
3) powder, calcium carbonate (CaCO
3) powder, Strontium carbonate powder (SrCO
3) powder, barium carbonate (BaCO
3) powder and lanthanum trioxide (La
2o
3) powder, be deployed into Ca
x1sr
x2ba
x3la
xfe
2+ afe
3+ boy(is x1=0.15 wherein, x2=0.35, x3=0.3, x=0.2, a+b=11.5,12.5,13.5,14.5 and 15.5) composition.In said mixture, add the SiO of 0.3wt%
2the H of powder, 0.1wt%
3bO
3powder also carries out wet mixing, mixture mean particle size 0.9 μ m.After mixture is dry, with 1280 ℃ of pre-burnings 2 hours in atmosphere.
The Preburning material particle of gained is carried out to dry type coarse reduction in vibrating mill, obtain the meal of mean particle size 3.0~5.0 μ m.
Then, take 500 grams, above-mentioned meal material, add the SiO of 0.25wt%
2, 0.60wt% CaCO
3, 0.80wt% Cr
2o
3, 0.10wt% H
3bO
3, 0.25wt% Al
2o
3, the ZnO of 0.20wt% is, the Mn of 0.25wt%
3o
4, the calglucon of 0.60wt% and the carbon black of 0.30wt%, then add the water of 700 milliliters, carry out case of wet attrition, obtain the ferrite slurry of mean particle size 0.75 μ m.
By after the slurry dewatering after Crushing of Ultrafine, in the parallel magnetic field of additional magneticstrength 700 kA/m, with forming pressure 0.4ton/cm
3carry out compressed moulding.The diameter of gained molding is the right cylinder of 40mm, height 15mm.
Temperature at 100-500 ℃ is heat-treated molding, removes moisture and organic dispersing agent, then by passing into nitrogen in sintering oven, controls oxygen concn, in nonoxidizing atmosphere, carry out sintering, heat-up rate is 120 ℃/h, 1200 ℃ of insulations 1.5 hours, obtains sintered permanent magnet.
Prepared ferrimagnet sample is carried out to compositional analysis and principal phase analysis.Measurement result is as shown in table 3.
Residual magnetic flux density (Br), HCJ (Hcj) and the rectangular degree (Hk/Hcj) of with magnetism testing instrument, measuring magnet sample, gained measured value is as shown in table 4.
Table 3
Table 4
Result from table 3 can find out, a+b is less than at 12.0 o'clock, generates single M phase ferrite; A+b, at 12.5~14.5 o'clock, generates M+W phase ferrite, and a+b is greater than at 15.0 o'clock, has α-Fe2O3 to generate mutually.
Result from table 4 can find out, a+b, at 12.5~14.5 o'clock, has obtained excellent magnetic property.
Embodiment 3
The research of sintering atmosphere and carbon black addition:
Use the ferric oxide (Fe identical with embodiment 1
2o
3) powder, calcium carbonate (CaCO
3) powder, Strontium carbonate powder (SrCO
3) powder, barium carbonate (BaCO
3) powder and lanthanum trioxide (La
2o
3) powder, be deployed into Ca
x1sr
x2ba
x3la
xfe
2+ afe
3+ boy(x1=0.15, x2=0.35, x3=0.3, x=0.2, a+b=13.5) composition.In said mixture, add the SiO of 0.3wt%
21.0 μ m), the H of 0.1wt% powder (the original mean particle size of purity>=98.0wt%, particle:
3bO
3powder (purity>=99.0wt%) also carries out wet mixing, mixture mean particle size 0.9 μ m.After mixture is dry, with 1280 ℃ of pre-burnings 2 hours in atmosphere.
The Preburning material particle of gained is carried out to dry type coarse reduction in vibrating mill, obtain the meal of mean particle size 3.0~5.0 μ m.
Then, take each 500 grams, 5 parts of above-mentioned meal material, add the SiO of 0.25wt%
2, 0.60wt% CaCO
3, 0.80wt% Cr
2o
3, 0.10wt% H
3bO
3, 0.25wt% Al
2o
3,, the ZnO of 0.20wt% is, the Mn of 0.25wt%
3o
4, 0.60wt% calglucon, add respectively 0, the carbon black of 0.1wt%, 0.2wt%, 0.3wt% and 0.4wt% simultaneously, then add the water of 700 milliliters, carry out case of wet attrition, obtain the ferrite slurry of mean particle size 0.75 μ m.
By after the slurry dewatering after Crushing of Ultrafine, in the parallel magnetic field of additional magneticstrength 700 kA/m, with forming pressure 0.4ton/cm
3carry out compressed moulding.The diameter of gained molding is the right cylinder of 40mm, height 15mm.
Molding is divided into 2 parts again, a copy of it is sintering in air, and portion carries out sintering in nonoxidizing atmosphere, obtains respectively sintered permanent magnet.
Prepared ferrimagnet sample is carried out to compositional analysis and principal phase analysis.Measurement result is as shown in table 5.
Residual magnetic flux density (Br), HCJ (Hcj) and the rectangular degree (Hk/Hcj) of with magnetism testing instrument, measuring magnet sample, gained measured value is as shown in table 6.
Table 5
Table 6
From table 5 and table 6, obtaining result can find out, in oxidizing atmosphere, sintering can not obtain the Hxagonal ferrite structure of M+W type.And add and nonoxidizing atmosphere sintering by appropriate carbon, can obtain hexagonal ferrite polycrystal structure and the excellent magnetic property of M+W type.
The invention provides the preparation method of ferrimagnet and ferrimagnet, accordingly can be by adding lanthanum, increase mole number, the appropriate interpolation reductibility carbon of iron and control the generation that sintering atmosphere suppresses α-Fe2O3 phase, obtained excellent magnetic property, do not need to add rare precious metals cobalt, save scarce resource, reduce manufacturing cost.
Claims (4)
1. the brilliant M+W mixed type of a hexagonal sintered permanent ferrite magnet, is characterized in that its composition formula Ca
x1sr
x2ba
x3la
xfe
2+ afe
3+ bo
yrepresent, wherein, x1 is 0.1-0.3, and x2 is 0.2-0.5, and x3 is 0.1-0.4, and x is 0.1-0.3, and a is 0.1-1.0, and b is 12.0-14.0,12.1≤a+b≤15.0, y=1+1/2x+a+3/2b; Its preparation method comprises the operation of batching mixing, pre-burning, coarse reduction, ball milling, moulding and sintering, and concrete steps are as follows:
(1) batching is mixed:
Press Ca
x1sr
x2ba
x3la
xfe
2+ afe
3+ bo
ycalculate and weigh calcium carbonate powders, strontium carbonate powder, barium carbonate powder, lanthanum oxide powder and the croci that contains required element; Wherein: x1 is 0.1-0.3, x2 is 0.2-0.5, and x3 is 0.1-0.4, and x is 0.1-0.3, and a is 0.1-1.0, and b is 12.0-14.0,12.1≤a+b≤15.0, y=1+1/2x+a+3/2b; Load weighted powder is mixed by wet process, and mixing time is controlled at 3-5 hour, and mixed mixture mean particle size is not more than 1.0 μ m; If Slurry Granularity is excessive after mixing, in pre-burning process, easily cause that pre-burning is insufficient, make to generate the ferritic content of hexagonal crystalline phase too low;
(2) pre-burning:
Said mixture material is carried out in air to pre-burning, calcined temperature is 1200-1350 ℃, and soaking time is 1-3 hour, obtains Preburning material particle;
(3) coarse reduction:
Above-mentioned Preburning material particle is carried out to dry type ball mill pulverizing to mean particle size 3-5 μ m, obtain Preburning material powder;
(4) ball milling:
To above-mentioned Preburning material powder, in weight proportion mode, add secondary additive, gained mixture is adopted to wet ball-milling mode continuously grinding, until the mean particle size that reaches particle is at 0.7-0.8 μ m; Described secondary additive comprises CaCO
3powder, SiO
2powder, Al
2o
3powder, Cr
2o
3powder, H
3bO
3powder, ZnO powder, Mn
3o
4one or more in powder, wherein the mean particle size of each compound powder is not more than 2.0 μ m, and the adding proportion of each additive is: CaCO
3: 0.3~1.5wt%, SiO
2: 0.1~1.0wt%, Al
2o
3: 0.1~1.5wt%, Cr
2o
3: 0.1~1.5wt%, H
3bO
3: 0.05~0.2wt%, ZnO:0.05~1.2wt%, Mn
3o
4: 0.05~1.5wt%;
(5) moulding:
The slip of above-mentioned steps gained is carried out to processed, and dewatering type can adopt centrifugation or press filtration mode to carry out, and is adjusted to pulp density at 60-65wt%, then carries out pressing under magnetic field, and forming magnetic field intensity is not less than 500 kA/m;
(6) sintering:
Molding is carried out in nonoxidizing atmosphere to sintering, sintering temperature is 1150-1250 ℃, and insulation 1.0-3.0 hour, controls oxygen partial pressure by pass into nitrogen in sintering oven, and passing into of nitrogen, carries out in the temperature range between top temperature at 500 ℃.
2. the preparation method of the brilliant M+W mixed type of hexagonal according to claim 1 sintered permanent ferrite magnet, it is characterized in that, in described proportion mixed process, also include additive silicon-dioxide and boric acid, its adding proportion is: silicon-dioxide 0.05-0.5wt%, boric acid 0.05-0.2wt%.
3. the preparation method of the brilliant M+W mixed type of hexagonal according to claim 1 sintered permanent ferrite magnet, is characterized in that, described secondary additive is also included in the carbon black of sintering circuit performance reductive action.
4. the preparation method of the brilliant M+W mixed type of hexagonal according to claim 1 sintered permanent ferrite magnet, it is characterized in that, in described ball milling operation, need to add a certain amount of dispersion agent, described dispersion agent is one or more in calglucon, Sorbitol Powder, xitix, and addition is the 0.2-1.5wt% of total composition weight.
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CN102329128A (en) * | 2011-06-11 | 2012-01-25 | 宜宾职业技术学院 | Hard calcium ferrite and manufacturing method thereof |
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US3638207A (en) * | 1969-11-17 | 1972-01-25 | Bell Telephone Labor Inc | Magnetic devices |
EP0297392A2 (en) * | 1987-07-01 | 1989-01-04 | Bayer Ag | Process for preparing finely divided barium hescaferrite pigments from halide molten masses and use thereof |
CN101599333A (en) * | 2009-04-28 | 2009-12-09 | 横店集团东磁股份有限公司 | The manufacture method of anisotropic multi-pole magnetic ring through dry-press forming |
CN102329128A (en) * | 2011-06-11 | 2012-01-25 | 宜宾职业技术学院 | Hard calcium ferrite and manufacturing method thereof |
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