CN105481358A - High-coercivity permanent magnetic ferrite and preparation method thereof - Google Patents
High-coercivity permanent magnetic ferrite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-coercivity permanent magnetic ferrite and a preparation method thereof. According to the method, one or a mixture of two or more selected from the group consisting of treated raw materials, i.e., CaCO3, SrCO3 and Fe2O3 are added on the basis of the mass of strontium ferrite pre-sintered material in the procedure of batching, and CaCO3 or SrCO3 is definitely used. The method employs raw materials used in conventional processes and treats the raw materials including CaCO3, SrCO3 and Fe2O3; since one powder selected from or mixed powder of the treated CaCO3, SrCO3 and Fe2O3 is added in the procedure of batching and the powder has substantially increased surface areas and good dispersibility, a contact area is increased and great interfacial energy is produced among pre-sintered ferrite particles after the powder is mixed with the pre-sintered ferrite particles, so growth of ferrite crystal grains is inhibited, the single domain structure of a magnet is maintained, and distribution of crystal grains in the magnet is uniform; and thus, the coercive force of the magnet is improved.
Description
Technical field
The invention belongs to magneticsubstance preparing technical field, especially relate to a kind of high-coercive force permanent-magnet ferrite and preparation method thereof.
Background technology
Along with field high speed developments such as automobile industry, electric bicycle, business automation equipment, household electric appliances, power tool and toy industries, the demand of the world to permanent-magnet ferrite material increases year by year.The forwards such as current electric motor of automobile, variable-frequency motor are energy-conservation, light weight, small-sized, high efficiency future development, need permanent-magnet ferrite under low temperature or hot conditions use, there is not phenomenon of demagnetizing, ensure the reliability of product, just need the permanent-magnet ferrite material of high-coercive force.In present actual production, the preparation method of high-coercive force permanent-magnet ferrite mainly adds additive as Al in the batching stage of producing permanent-magnet ferrite
2o
3, SiO
2, Cr
2o
3, Co
2o
3deng, and these additives are improving coercitive while, remanent magnetism is also along with decline sharply.Therefore these additives are added as Al
2o
3, SiO
2, Cr
2o
3, Co
2o
3when obtaining high-coercive force, the over-all properties of magnet is effectively improved etc. being difficult to.
Chinese invention patent (publication No. is CN102408229A) discloses a kind of coercitive method of raising permanent-magnet ferrite, and its concrete steps are: 1), prepare burden: on the basis of a strontium ferrites Preburning material, add CaCO in secondary processes
3, SrCO
3, SiO
2, Al
2o
3, H
3bO
3, Cr
2o
3in any 2 ~ 6 kinds, add additive, it consists of R simultaneously
xal
yfe
zo
m, wherein x=2 ~ 7, y=1 ~ 2, z=3 ~ 9, m=5 ~ 11, R is the mixture of Pr, Bi, Gd, Nd, Cu, Cr, Co wherein two or more; Relative to Preburning material, the weight percentage of substance is: 0.2% ~ 1.4%CaCO
3, 0.1% ~ 0.6%SrCO
3, 0.2% ~ 0.8%SiO
2, 0.2% ~ 0.8%Al
2o
3, 0.1% ~ 0.5%H
3bO
3, 0.2% ~ 0.8%Cr
2o
3, 0.1% ~ 2.5%R
xal
yfe
zo
m; 2), ball milling: carry out secondary ball milling with tumbling mill, steel ball used is the bearing steel ball of diameter 5 ~ 10 millimeters, and Ball-milling Time is 15 ~ 20 hours; The mass percent of material, ball, water is 1:15:2; The granularity laser particle analyzer of secondary ball milling is tested, and its D50 controls within the scope of 0.80 ~ 0.95 μm; 3), compression moulding: suppress the slip after ball milling with hydraulic machine for magnetic material, the blank diameter after compacting is 30 ~ 40mm, is highly 15 ~ 25mm, and density is 3.1 ~ 3.3g/cm
3; Before compacting, the water content control of slip is 33 ~ 38%; 4), sinter: utilize program control type cabinet-type electric furnace to sinter blank, its working temperature is 100 ~ 1300 DEG C: concrete sintering process is as follows: (180 DEG C ± 20 DEG C)/(1.0 ~ 1.5h)+(380 DEG C ± 20 DEG C)/(1.0 ~ 1.5h)+(600 DEG C ± 20 DEG C)/(1.0 ~ 1.5h)+(850 DEG C ± 20 DEG C)/(1.0 ~ 1.5h)+(1100 DEG C ± 20 DEG C)/(1.0 ~ 1.5h)+(1200 DEG C ± 50 DEG C)/(1.5 ~ 2.0h); 5), mill processing: sintering blank top and bottom are out polished, meets product requirement.Problems existing is: the first, in secondary ball milling, add additive R
xal
yfe
zo
m, R
xal
yfe
zo
mcomplicated process of preparation, wastes time and energy; The second, the additive added contains the rare earth element such as cobalt, praseodymium, and the Costco Wholesale of rare earth element material is high, causes input cost greatly to increase.
Summary of the invention
In order to overcome the defect of prior art, the object of this invention is to provide a kind of preparation method of high-coercive force permanent-magnet ferrite, using the raw material of existing technique, when not reducing remanent magnetism, improving the coercive force of permanent-magnet ferrite.
The technical scheme that the present invention solves the employing of its technical problem is:
A preparation method for high-coercive force permanent-magnet ferrite, concrete steps are as follows:
1), batching: on the basis of Strontium ferrite powder, add the raw materials of Ca CO processed
3, SrCO
3and Fe
2o
3in one or more mixture, but must CaCO be there is
3or SrCO
3, relative to Preburning material, the weight percentage of substance is: 0.6% ~ 1.4%CaCO
3, 0.1% ~ 1.2%SrCO
3, 0.1% ~ 2.0%Fe
2o
3;
2), ball milling: add the calglucon of 0.2%, carry out secondary ball milling with tumbling mill, steel ball used is the bearing steel ball of diameter 3 ~ 8mm, and Ball-milling Time is 16 ~ 30h, the mass percent of material, ball, water is 1:20:1.5, and being milled to median size is 0.80 μm;
3), compacting green compact: by above-mentioned steps 2) in the water content control of gained slip 25% ~ 45%, then in magnetic field, carry out compacting green compact, the pressure of compacting is 500 ~ 550kg/cm
3, forming magnetic field intensity>=0.8T;
4), sinter: utilize program control type cabinet-type electric furnace to sinter blank, concrete sintering process is as follows: (180 DEG C ± 10 DEG C)/(1.0 ~ 1.5h)+(380 DEG C ± 10 DEG C)/(1.0 ~ 1.5h)+(550 DEG C ± 10 DEG C)/(1.0 ~ 1.5h)+(850 DEG C ± 10 DEG C)/(1.0 ~ 1.5h)+(550 DEG C ± 10 DEG C)/(1.0 ~ 1.5h)+(1100 DEG C ± 10 DEG C)/(1.0 ~ 1.5h)+(1200 DEG C ± 25 DEG C)/(1.5 ~ 2.0h), and the above time is soaking time;
5), mill processing: sintering blank is out polished up and down, tests with the magnetic property of auto measurement equipment for magnetic material to obtained product.
Further, step 1) described in raw materials of Ca CO
3, SrCO
3and Fe
2o
3treatment process as follows:
1) ball milling: by raw materials of Ca CO
3, SrCO
3and Fe
2o
3in two or more mixture and dispersion agent put into sand mill, must CaCO be there is
3or SrCO
3, wherein dispersion agent is: 0.1%≤calglucon≤0.8%, 0.1%≤sorbyl alcohol≤1.0%, and dispersion agent can improve the orientation degree of slip, and water is medium, material: ball: water=1:20:1.5, and rotating speed 400r/min, stirs 3 ~ 10 hours;
2) sintering: utilize program control type cabinet-type electric furnace to step 1) material that obtains carries out pre-burning, its sintering temperature is warming up to 500 DEG C from 100 DEG C, concrete sintering process is as follows: (100 DEG C ± 10 DEG C)/(0.5 ~ 2.0h)+(180 DEG C ± 10 DEG C)/(0.5 ~ 2.0h)+(380 DEG C ± 10 DEG C)/(0.5 ~ 2.0h)+(450 DEG C ± 10 DEG C)/(0.5 ~ 2.0h)+(500 DEG C ± 10 DEG C)/(1.0 ~ 3.0h), and the above time is soaking time;
3) powder process: by step 2) material of gained grinds, and obtained powder is for subsequent use.
Method of the present invention adopts the raw material of existing technique, and to wherein raw materials of Ca CO
3, SrCO
3and Fe
2o
3process, at the temperature of 500 DEG C, all can not there is rotten or reaction in several material, in the batching stage, add treated CaCO
3, SrCO
3and Fe
2o
3single powder or mixed powder; because the surface-area of these powder increases greatly; and good dispersity; after mixing with pre-burning ferrite particle, increase contact area, produce larger interfacial energy at pre-burning ferrite paricles intergranular; thus inhibit the growth of ferrite crystal grains; maintain the one-domain structure of magnet, in magnet, crystal grain is evenly distributed, thus improves the coercive force of magnet.
Embodiment
Below in conjunction with three groups of contrasts, the present invention is further described.
The Preburning material used in embodiments of the invention is the Strontium ferrite powder of different manufacturers that market is bought, and is numbered A, B and C.
First group: as shown in table 1, for Preburning material A adds additivated concrete quality composition:
Table 1 (weight: unit of gram)
Comparative example A 1
A preparation method for permanent-magnet ferrite, concrete steps are as follows:
1), batching: on the basis of 500g Strontium ferrite powder, add 0.5gAl
2o
3, 1.5gSiO
2, 1.0gCr
2o
3, 0.5gH
3bO
3, 3.0gCaCO
3;
2), ball milling: add 1g calglucon, carry out secondary ball milling with tumbling mill, steel ball used is the bearing steel ball of diameter 8mm, and Ball-milling Time is 20 hours, the mass ratio of material, ball, water is: material: ball: water=1:20:1.5, and being milled to median size is 0.8 μm;
3), compacting green compact: by above-mentioned steps 2) water content control of gained slip is 35%, then in magnetic field, carry out compacting green compact, the pressure of compacting is 550kg/cm
3, forming magnetic field intensity 1.0T;
4), sinter: utilize program control type cabinet-type electric furnace to sinter blank, concrete sintering process is as follows: 180 DEG C/1.0h+380 DEG C/1.0h+550 DEG C/1.0h+850 DEG C/1.0h+950 DEG C/1.0h+1100 DEG C/1.0h+1185 DEG C/2.5h, the above time is soaking time;
5), mill processing: polished up and down by sintering blank out, test with the magnetic property of auto measurement equipment for magnetic material to obtained product, specific performance is as shown in table 2.
Embodiment a1
The present embodiment, first processes raw material, and concrete treatment process is as follows:
1) ball milling: by raw material 500gCaCO
3, 2.5g calglucon and 3.0g sorbyl alcohol put into sand mill, water is medium, material: ball: water=1:20:1.5, and rotating speed 400r/min, stirs 8 hours;
2) sintering: utilize program control type cabinet-type electric furnace to step 1) material that obtains carries out pre-burning, its sintering temperature is warming up to 500 DEG C from 100 DEG C, concrete sintering process is as follows: 100 DEG C/1.0h+180 DEG C/1.0h+380 DEG C/1.0h+450 DEG C/1.0h+500 DEG C/2h, the above time is soaking time;
3) powder process: by step 2) material of gained grinds, and obtained powder is for subsequent use.
Adopt the raw material identical with comparative example A 1 and identical technique, difference is only, adds the CaCO that above-mentioned process obtains
3, relative to Preburning material, the weight percentage of substance is: 0.5gAl
2o
3, 1.5gSiO
2, 1.0gCr
2o
3, 0.5gH
3bO
3, 3.0g process CaCO
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 2.
Comparative example A 2
Adopt the raw material identical with comparative example A 1 and identical technique, parameter is in table 1, and specific performance parameter is as shown in table 2.
Embodiment a2
Adopt the raw material identical with comparative example A 2 and identical technique, difference is only, adds the 4.5gSrCO that above-mentioned process obtains
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 2.
Comparative example A 3
Adopt the raw material identical with comparative example A 1 and identical technique, parameter is in table 1, and specific performance parameter is as shown in table 2.
Embodiment a3
Adopt the raw material identical with comparative example A 3 and identical technique, difference is only, adds the 3.0gCaCO that above-mentioned process obtains
3and 1.5gSrCO
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 2.
Comparative example A 4
Adopt the raw material identical with comparative example A 1 and identical technique, parameter is in table 1, and specific performance parameter is as shown in table 2.
Embodiment a4
Adopt the raw material identical with comparative example A 4 and identical technique, difference is only, adds the 3.0gCaCO that above-mentioned process obtains
3and 5.0gFe
2o
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 2.
Comparative example A 5
Adopt the raw material identical with comparative example A 1 and identical technique, parameter is in table 1, and specific performance parameter is as shown in table 2.
Embodiment a5
Adopt the raw material identical with comparative example A 5 and identical technique, difference is only, adds the 4.5gSrCO that above-mentioned process obtains
3and 1.5gFe
2o
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 2.
Comparative example A 6
Adopt the raw material identical with comparative example A 1 and identical technique, parameter is in table 1, and specific performance parameter is as shown in table 2.
Embodiment a6
Adopt the raw material identical with comparative example A 6 and identical technique, difference is only, adds the 3.0gCaCO that above-mentioned process obtains
3, 1.0gSrCO
3and 1.5gFe
2o
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 2.
Table 2 Preburning material A prepares the magnetic property of product
| Sample type | Br(mT) | Hcb(kOe) | Hcj(kOe) | BH(kJ/m 3) |
| A1 | 408.4 | 2.705 | 2.985 | 31.58 |
| a1 | 407.2 | 2.935 | 3.268 | 31.49 |
| A2 | 407.9 | 3.112 | 3.469 | 30.94 |
| a2 | 408.7 | 3.246 | 3.716 | 31.25 |
| A3 | 409.2 | 3.481 | 3.768 | 31.38 |
| a3 | 410.5 | 3.657 | 3.873 | 32.19 |
| A4 | 405.8 | 2.846 | 3.076 | 33.51 |
| a4 | 404.8 | 3.087 | 3.368 | 33.19 |
| A5 | 401.5 | 2.583 | 2.863 | 28.45 |
| a5 | 400.3 | 2.816 | 3.159 | 27.96 |
| A6 | 412.5 | 3.024 | 3.467 | 32.49 |
| a6 | 413.1 | 3.168 | 3.628 | 32.28 |
Preburning material A is according to the formula of table 1, and sintering temperature is 1185 DEG C.As can be seen from Table 2, formulation Example of the present invention is compared with comparative example, and the remanent magnetism of product does not reduce, and coercive force on average improves 193Oe, and Inner reports coercive force and improves 230.7Oe.
Second group: as shown in table 3, for Preburning material B adds additivated concrete quality composition:
Table 3 (weight: unit of gram)
Comparative example B1
A preparation method for permanent-magnet ferrite, concrete steps are as follows:
1), batching: on the basis of 500g Strontium ferrite powder, add 0.5gAl
2o
3, 1.5gSiO
2, 1.0gCr
2o
3, 0.5gH
3bO
3, 5.0gCaCO
3;
2), ball milling: add 1g calglucon, carry out secondary ball milling with tumbling mill, steel ball used is the bearing steel ball of diameter 4mm, and Ball-milling Time is 20 hours, the mass ratio of material, ball, water is: material: ball: water=1:20:1.5, and being milled to median size is 0.8 μm;
3), compacting green compact: by above-mentioned steps 2) water content control of gained slip is 30%, then in magnetic field, carry out compacting green compact, the pressure of compacting is 500kg/cm
3, forming magnetic field intensity 1.0T;
4), sinter: utilize program control type cabinet-type electric furnace to sinter blank, concrete sintering process is 180 DEG C/1.0h+380 DEG C/1.0h+550 DEG C/1.0h+850 DEG C/1.0h+950 DEG C/1.0h+1100 DEG C/1.0h+1175 DEG C/2.0h, and the above time is soaking time;
5), mill processing: polished up and down by sintering blank out, test with the magnetic property of auto measurement equipment for magnetic material to obtained product, specific performance is as shown in table 4.
Embodiment b1
The present embodiment, first processes raw material, and concrete treatment process is as follows:
1) ball milling: by raw material 500gCaCO
3, 1.0g calglucon and 4g sorbyl alcohol put into sand mill, water is medium, material: ball: water=1:20:1.5, and rotating speed 400r/min, stirs 8 hours;
2) sintering: utilize program control type cabinet-type electric furnace to step 1) material that obtains carries out pre-burning, its sintering temperature is warming up to 500 DEG C from 100 DEG C, concrete sintering process is as follows: 100 DEG C/1.0h+180 DEG C/1.0h+380 DEG C/1.0h+450 DEG C/1.0h+500 DEG C/2h, the above time is soaking time;
3) powder process: by step 2) material of gained grinds, and obtained powder is for subsequent use.
Adopt the raw material identical with comparative example B1 and identical technique, difference is only, adds the CaCO that above-mentioned process obtains
3, relative to Preburning material, the weight percentage of substance is: 0.5gAl
2o
3, 1.5gSiO
2, 1.0gCr
2o
3, 0.5gH
3bO
3, 5.0g process CaCO
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 4.
Comparative example B2
Adopt the raw material identical with comparative example B1 and identical technique, parameter is in table 3, and specific performance parameter is as shown in table 4.
Embodiment b2
Adopt the raw material identical with comparative example B2 and identical technique, difference is only, adds the 2.5gSrCO that above-mentioned process obtains
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 4.
Comparative example B3
Adopt the raw material identical with comparative example B1 and identical technique, parameter is in table 3, and specific performance parameter is as shown in table 2.
Embodiment b3
Adopt the raw material identical with comparative example B3 and identical technique, difference is only, adds the 4.0gCaCO that above-mentioned process obtains
3and 1.0gSrCO
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 4.
Comparative example B4
Adopt the raw material identical with comparative example B1 and identical technique, parameter is in table 3, and specific performance parameter is as shown in table 4.
Embodiment b4
Adopt the raw material identical with comparative example B4 and identical technique, difference is only, adds the 4.0gCaCO that above-mentioned process obtains
3and 7.0gFe
2o
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 4.
Comparative example B5
Adopt the raw material identical with comparative example B1 and identical technique, parameter is in table 3, and specific performance parameter is as shown in table 4.
Embodiment b5
Adopt the raw material identical with comparative example B5 and identical technique, difference is only, adds the 3.0gSrCO that above-mentioned process obtains
3and 6.0gFe
2o
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 4.
Comparative example B6
Adopt the raw material identical with comparative example B1 and identical technique, parameter is in table 3, and specific performance parameter is as shown in table 4.
Embodiment b6
Adopt the raw material identical with comparative example B6 and identical technique, difference is only, adds the 3.0gCaCO that above-mentioned process obtains
3, 2.0gSrCO
3and 2.0gFe
2o
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 4.
Table 4 Preburning material B prepares the magnetic property of product
| Sample type | Br(mT) | Hcb(kOe) | Hcj(kOe) | BH(kJ/m 3) |
| B1 | 395.6 | 3.168 | 3.354 | 30.58 |
| b1 | 396.2 | 3.273 | 3.568 | 29.86 |
| B2 | 393.5 | 3.094 | 3.616 | 29.87 |
| b2 | 394.6 | 3.218 | 3.861 | 30.56 |
| B3 | 396.0 | 3.052 | 3.583 | 30.39 |
| b3 | 397.6 | 3.246 | 3.768 | 31.26 7 --> |
| B4 | 400.2 | 2.867 | 3.467 | 32.57 |
| b4 | 399.6 | 3.168 | 3.749 | 33.59 |
| B5 | 387.8 | 2.968 | 3.584 | 32.49 |
| b5 | 388.4 | 3.046 | 3.783 | 32.68 |
| B6 | 401.8 | 2.945 | 3.684 | 32.85 |
| b6 | 400.9 | 3.145 | 3.847 | 33.46 |
Preburning material B is according to the formula of table 3, and sintering temperature is 1175 DEG C.As can be seen from Table 4, formulation Example of the present invention is compared with comparative example, and the remanent magnetism of product does not reduce, and coercive force on average improves 167Oe, and Inner reports coercive force and improves 214.7Oe.
3rd group: as shown in table 5, for Preburning material C adds additivated concrete quality composition:
Table 5 (weight: unit of gram)
Comparative example C1
A preparation method for permanent-magnet ferrite, concrete steps are as follows:
1), batching: on the basis of 500g Strontium ferrite powder, add 0.5gAl
2o
3, 1.5gSiO
2, 1.0gCr
2o
3, 0.5gH
3bO
3, 7.0gCaCO
3;
2), ball milling: add 1g calglucon, carry out secondary ball milling with tumbling mill, steel ball used is the bearing steel ball of diameter 6mm, and Ball-milling Time is 20 hours, the mass ratio of material, ball, water is: material: ball: water=1:20:1.5, and being milled to median size is 0.8 μm;
3), compacting green compact: by above-mentioned steps 2) water content control of gained slip is 40%, then in magnetic field, carry out compacting green compact, the pressure of compacting is 550kg/cm
3, forming magnetic field intensity 0.8T;
4), sinter: utilize program control type cabinet-type electric furnace to sinter blank, concrete sintering process is 180 DEG C/1.0h+380 DEG C/1.0h+550 DEG C/1.0h+850 DEG C/1.0h+950 DEG C/1.0h+1100 DEG C/1.0h+1175 DEG C/2.0h, and the above time is soaking time;
5), mill processing: polished up and down by sintering blank out, test with the magnetic property of auto measurement equipment for magnetic material to obtained product, specific performance is as shown in table 6.
Embodiment c1
The present embodiment, first processes raw material, and concrete treatment process is as follows:
1) ball milling: by raw material 500gCaCO
3, 3.0g calglucon and 1.0g sorbyl alcohol put into sand mill, water is medium, material: ball: water=1:20:1.5, and rotating speed 400r/min, stirs 8 hours;
2) sintering: utilize program control type cabinet-type electric furnace to step 1) material that obtains carries out pre-burning, its sintering temperature is warming up to 500 DEG C from 100 DEG C, concrete sintering process is as follows: 100 DEG C/1.0h+180 DEG C/1.0h+380 DEG C/1.0h+450 DEG C/1.0h+500 DEG C/2h, the above time is soaking time;
3) powder process: by step 2) material of gained grinds, and obtained powder is for subsequent use.
Adopt the raw material identical with comparative example C1 and identical technique, difference is only, adds the CaCO that above-mentioned process obtains
3, relative to Preburning material, the weight percentage of substance is: 0.5gAl
2o
3, 1.5gSiO
2, 1.0gCr
2o
3, 0.5gH
3bO
3, 7.0g process CaCO
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 6.
Comparative example C2
Adopt the raw material identical with comparative example C1 and identical technique, parameter is in table 5, and specific performance parameter is as shown in table 6.
Embodiment c2
Adopt the raw material identical with comparative example C2 and identical technique, difference is only, adds the 5.0gSrCO that above-mentioned process obtains
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 6.
Comparative example C3
Adopt the raw material identical with comparative example C1 and identical technique, parameter is in table 5, and specific performance parameter is as shown in table 6.
Embodiment c3
Adopt the raw material identical with comparative example C3 and identical technique, difference is only, adds the 3.0gCaCO that above-mentioned process obtains
3and 2.0gSrCO
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 6.
Comparative example C4
Adopt the raw material identical with comparative example C1 and identical technique, parameter is in table 5, and specific performance parameter is as shown in table 6.
Embodiment c4
Adopt the raw material identical with comparative example C4 and identical technique, difference is only, adds the 3.0gCaCO that above-mentioned process obtains
3and 4.0gFe
2o
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 6.
Comparative example C5
Adopt the raw material identical with comparative example C1 and identical technique, parameter is in table 5, and specific performance parameter is as shown in table 6.
Embodiment c5
Adopt the raw material identical with comparative example C5 and identical technique, difference is only, adds the 2.0gSrCO that above-mentioned process obtains
3and 5.0gFe
2o
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 6.
Comparative example C6
Adopt the raw material identical with comparative example C1 and identical technique, parameter is in table 5, and specific performance parameter is as shown in table 6.
Embodiment c6
Adopt the raw material identical with comparative example C6 and identical technique, difference is only, adds the 4.0gCaCO that above-mentioned process obtains
3, 0.5gSrCO
3and 0.5gFe
2o
3, carry out magnetism testing with auto measurement equipment for magnetic material to obtained product, specific performance parameter is as shown in table 6.
Table 6 Preburning material C prepares the magnetic property of product
| Sample type | Br(mT) | Hcb(kOe) | Hcj(kOe) | BH(kJ/m 3) |
| C1 | 415.6 | 2.584 | 2.745 | 33.56 |
| c1 | 416.2 | 2.769 | 2.973 | 33.67 |
| C2 | 414.7 | 2.756 | 3.016 | 32.69 |
| c2 | 414.8 | 2.873 | 3.316 | 32.61 |
| C3 | 416.3 | 2.659 | 2.985 | 33.73 |
| c3 | 415.8 | 2.892 | 3.274 | 34.25 |
| C4 | 414.8 | 2.759 | 3.176 | 35.24 |
| c4 | 415.6 | 2.946 | 3.416 | 36.29 |
| C5 | 412.8 | 2.679 | 2.948 | 33.86 |
| c5 | 413.1 | 2.839 | 3.267 | 34.21 |
| C6 | 418.7 | 2.794 | 3.182 | 35.89 |
| c6 | 419.2 | 2.983 | 3.487 | 35.37 |
Preburning material C is according to the formula of table 5, and sintering temperature is 1195 DEG C.As can be seen from Table 6, formulation Example of the present invention is compared with comparative example, and the remanent magnetism of product does not reduce, and coercive force on average improves 178.5Oe, and Inner reports coercive force and improves 280.2Oe.
Claims (6)
1. a preparation method for high-coercive force permanent-magnet ferrite, is characterized in that, in the batching stage, based on the quality of Strontium ferrite powder, adds the raw materials of Ca CO processed
3, SrCO
3and Fe
2o
3in one or more mixture, but must CaCO be there is
3or SrCO
3.
2. the preparation method of high-coercive force permanent-magnet ferrite according to claim 1, it is characterized in that, concrete steps are as follows:
1), batching: based on the quality of Strontium ferrite powder, added the raw materials of Ca CO of process
3, SrCO
3and Fe
2o
3in two or more mixture, relative to Preburning material, the weight percentage of substance is: 0.6% ~ 1.4%CaCO
3, 0.1% ~ 1.2%SrCO
3, 0.1% ~ 2.0%Fe
2o
3;
2), ball milling: add the calglucon of 0.2%, carry out secondary ball milling with tumbling mill, steel ball used is the bearing steel ball of diameter 3 ~ 8mm, and Ball-milling Time is 16 ~ 30h; The mass percent of material, ball, water is 1:20:1.5; Being milled to median size is 0.80 μm;
3), compacting green compact: by above-mentioned steps 2) in the water content control of gained slip 25% ~ 45%, then in magnetic field, carry out compacting green compact, the pressure of compacting is 500 ~ 550kg/cm
3, forming magnetic field intensity>=0.8T;
4), sinter: utilize program control type cabinet-type electric furnace to sinter blank, concrete sintering process is as follows: (180 DEG C ± 10 DEG C)/(1.0 ~ 1.5h)+(380 DEG C ± 10 DEG C)/(1.0 ~ 1.5h)+(550 DEG C ± 10 DEG C)/(1.0 ~ 1.5h)+(850 DEG C ± 10 DEG C)/(1.0 ~ 1.5h)+(550 DEG C ± 10 DEG C)/(1.0 ~ 1.5h)+(1100 DEG C ± 10 DEG C)/(1.0 ~ 1.5h)+(1200 DEG C ± 25 DEG C)/(1.5 ~ 2.0h), and the above time is soaking time;
5), mill processing: sintering blank is out polished up and down, tests with the magnetic property of auto measurement equipment for magnetic material to obtained product.
3. the preparation method of high-coercive force permanent-magnet ferrite according to claim 2, is characterized in that, step 1) described in raw materials of Ca CO
3, SrCO
3and Fe
2o
3treatment process as follows:
1) ball milling: by raw materials of Ca CO
3, SrCO
3and Fe
2o
3in one or more mixture and a certain amount of dispersion agent put into sand mill, must CaCO be there is
3or SrCO
3, water is medium, material: ball: water=1:20:1.5, and rotating speed 400r/min, stirs 3 ~ 10 hours;
2) sintering: utilize program control type cabinet-type electric furnace to step 1) material that obtains carries out pre-burning, and its sintering temperature is warming up to 500 DEG C from 100 DEG C;
3) powder process: by step 2) material of gained grinds, and obtained powder is for subsequent use.
4. the preparation method of high-coercive force permanent-magnet ferrite according to claim 3, is characterized in that, described dispersion agent is calglucon and sorbyl alcohol, wherein: 0.1%≤calglucon≤0.8%, and 0.1%≤sorbyl alcohol≤1.0%.
5. the preparation method of high-coercive force permanent-magnet ferrite according to claim 3, it is characterized in that, described concrete sintering process is as follows: (100 DEG C ± 10 DEG C)/(0.5 ~ 2.0h)+(180 DEG C ± 10 DEG C)/(0.5 ~ 2.0h)+(380 DEG C ± 10 DEG C)/(0.5 ~ 2.0h)+(450 DEG C ± 10 DEG C)/(0.5 ~ 2.0h)+(500 DEG C ± 10 DEG C)/(1.0 ~ 3.0h), the above time is soaking time.
6. the high-coercive force permanent-magnet ferrite obtained by the preparation method described in any one of claim 1 to 5.
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| CN108585821A (en) * | 2018-05-24 | 2018-09-28 | 成都锦钛精工科技有限公司 | Solid solution structure additive and preparation method and the application in ferrite permanent-magnet materials preparation |
| CN108585822A (en) * | 2018-07-05 | 2018-09-28 | 马鞍山高科磁性材料有限公司 | A kind of preparation method of high performance La-Co systems strontium permanent-magnet ferrite material |
| CN115724654A (en) * | 2021-08-25 | 2023-03-03 | 横店集团东磁股份有限公司 | Preparation method of permanent magnetic ferrite sintered in wide temperature zone |
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