CN111056832A - Ferrite permanent magnetic material and preparation method thereof - Google Patents
Ferrite permanent magnetic material and preparation method thereof Download PDFInfo
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Abstract
A ferrite permanent magnetic material and a preparation method thereof, wherein the chemical formula of the ferrite permanent magnetic material is (Sr)1‑wBaw）1‑x‑ yLaxCayFe2n‑zCozO, wherein x is more than or equal to 0.5 and less than or equal to 0.68, y is more than or equal to 0.3 and less than or equal to 0.5, z is more than or equal to 0.48 and less than or equal to 0.68, n is more than or equal to 4.9 and less than or equal to 5.4, and w is more than or equal to 0.001 and less than or equal to 1. The ferrite permanent magnetic material contains rare earth La element and Co, and La/Co is more than or equal to 1.65; and contains Si, B and Mn, SiO in terms of oxide weight20.2% -0.4% of B2O31 to 2 percent of the total amount of the manganese oxide and 0.1 to 0.3 percent of MnO. The preparation method obtains fine and uniform crystal grains through lower-temperature sintering, and can improve the performance of Br, Hcj and the like of products.
Description
Technical Field
The invention relates to a permanent magnet material and a preparation method thereof, in particular to a ferrite permanent magnet material and a preparation method thereof.
Background
Ferrite permanent magnet materials are used as important permanent magnet materials and widely applied to the fields of automobile motors, electric tools, energy-saving household appliances and the like. With the improvement of the performance of the ferrite permanent magnet material, the sizes of devices such as magnetic shoes and the like are thinner and thinner, and finally, the motor is miniaturized more and more. Because the magnetic shoe in the motor provides a magnetic field in an open circuit state, a certain demagnetizing field exists in the magnetic shoe, and along with the thinning of the magnetic shoe, the thinner the magnetic shoe is, the larger the demagnetizing factor is, the larger the internal demagnetizing field is, and the requirement on the demagnetization resistance of the material is correspondingly improved, so that the material is required to have high remanence and high coercivity at the same time.
CN 101351853A discloses a ferrite material, which adopts Ca1-x-yLaxSryFe2n-zCoz, relative to CN101013622A, x is more than or equal to 0.4 and less than or equal to 0.6, y is more than or equal to 0.01 and less than or equal to 0.3, z is more than or equal to 0.2 and less than or equal to 0.45, and n is more than or equal to 5.2 and less than or equal to 5.8, the ferrite material obtains a ferrite material with more excellent performance than the prior SrLaCo ferrite and CaLaCo ferrite materials by setting the La/Co ratio (x/z) to be more than or equal to 1, preferably the x/z to be more than or equal to 1.3, more preferably the x/z to be more than or equal to 1, and the intrinsic coercive force Hcj is more than 4500 Oe. The technology has low lanthanum-cobalt ratio (x/z) and needs high cobalt content.
CN 103724004 a discloses a high coercivity permanent magnetic ferrite material and a preparation method thereof, wherein the high coercivity permanent magnetic ferrite material consists of a main component and an auxiliary component, and the contents of the main component and the auxiliary component are calculated as oxides: fe2O383-91mol％，CaCO31.0-4.5mol％，La2O32.1-6.0mol％，Co2O31.5-3.5 mol%, the balance being SrCO3Or the balance being SrCO3With BaCO3A mixture of (a); based on the total weight of the main componentsThe content of each component of the accessory ingredient is SiO20.1-0.8wt％、Al2O30-0.6wt％、H3BO30-0.4wt％，Cr2O30-0.6 wt%, and the Hcj of the ferrite material is more than or equal to 5800 Oe. This technique adds Al2O3And Cr2O3When Hcj is increased, the remanence Br is decreased.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art and provides a high-performance ferrite permanent magnetic material and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows: a ferrite permanent magnetic material has a chemical formula of (Sr)1-wBaw)1-x-yLaxCayFe2n-zCozO, wherein x is more than or equal to 0.5 and less than or equal to 0.68, y is more than or equal to 0.3 and less than or equal to 0.5, z is more than or equal to 0.48 and less than or equal to 0.68, n is more than or equal to 4.9 and less than or equal to 5.4, and w is more than or equal to 0.001 and less than or equal to 1; and contains the other elements Si, B and Mn, based on the weight of the oxides, SiO20.2% -0.4% of B2O30.1-0.3 percent of MnO and 0.1-0.3 percent of MnO.
Further, the ferrite permanent magnetic material has a chemical formula (Sr)1-wBaw)1-x-yLaxCayFe2n-zCozIn O, La/Co is more than or equal to 1.65.
Further, the ferrite permanent magnetic material has a chemical formula (Sr)1-wBaw)1-x-yLaxCayFe2n-zCozIn O, n is more than or equal to 4.9 and less than or equal to 5.1, and w is more than or equal to 0.7 and less than or equal to 1.
Further, the ferrite permanent magnetic material has a chemical formula (Sr)1-wBaw)1-x-yLaxCayFe2n-zCozIn O, n is more than or equal to 4.9 and less than or equal to 5.0, and w is more than or equal to 0.1 and less than or equal to 0.3.
The preparation method of the ferrite permanent magnetic material comprises the following steps:
(1) pre-sintering material mixing: adding raw materials such as iron oxide red, strontium carbonate, barium carbonate, calcium carbonate, lanthanum oxide, cobalt oxide and the like into a sand mill according to a ratio, adding water for slurrying and mixing to obtain a pre-sintered material;
(2) pre-burning main materials: dehydrating the pre-sintered material obtained in the step (1), placing the dehydrated pre-sintered material in a pre-sintered material kiln for sintering to obtain pre-sintered material balls, and then crushing to obtain pre-sintered material powder;
(3) ball milling: putting the pre-sintering material powder obtained in the step (2) into a ball mill, adding silicon oxide, boric acid, calcium gluconate and ammonium bicarbonate, and then adding water for ball milling to obtain slurry;
(4) and (3) dehydrating: precipitating or dehydrating the slurry obtained in the step (3) to obtain slurry with low water content;
(5) molding and sintering: placing the slurry with low water content obtained in the step (4) in a forming press, and carrying out orientation forming in a magnetic field to obtain a green body;
(6) and (3) sintering: and (5) placing the green body obtained in the step (5) on a sintering plate, and sintering in a sintering kiln to obtain the ferrite permanent magnet material blank.
Further, in the step (2), the sintering temperature is 1185-1200 ℃, and the particle size of the pre-sintering material powder is less than or equal to 6 microns.
Further, in the step (3), the adding amount of the silicon oxide is 0.2-0.4% of the weight of the pre-sintering powder, the adding amount of the boric acid is 0.1-0.2% of the weight of the pre-sintering powder, the adding amount of the calcium gluconate is 0.1-0.3% of the weight of the pre-sintering powder, and the adding amount of the ammonium bicarbonate is 0.1-0.3% of the weight of the pre-sintering powder.
Further, in the step (3), the ratio of the ball material and the water added with water for ball milling is 5-15: 1-2, the ball milling method is rolling ball milling, and the ball milling time is 12-20 h.
Further, in the step (3), the particle size of the solid material in the slurry is 0.65-0.78 μm; the pH value of the slurry is less than or equal to 9.
Further, in the step (4), the water content of the slurry with low water content is 30-35%.
Further, in the step (5), the magnetic field intensity of the magnetic field forming is more than or equal to 0.7T, and the green body density is more than or equal to 3.0g/cm3。
Further, in the step (6), the sintering temperature is 1120-1160 ℃, and the sintering time is 2h-4h, the heating rate is 0.1 ℃/min-3 ℃/min, and the blank density of the obtained ferrite permanent magnet material is more than or equal to 5.05g/cm3。
The invention has the beneficial effects that: on one hand, the La/Co ratio is increased to 1.7-2.2, La with high abundance reserves is fully utilized, and the anisotropy field is essentially improved from the material, so that the Hcj of the material is improved; on the other hand, Ba and Ca are added into the pre-sintering material to replace Sr, and the ratio of (Sr + Ba)/Ca is less than or equal to 0.4, which is equivalent to that Ca/(Sr + Ba) is more than or equal to 2.5. The Br of the ferrite permanent magnet material is improved by utilizing the high saturation magnetization characteristic of Ba and the high density characteristics of Ba and Ca; the coercive force of the ferrite material is improved by fully utilizing the light rare earth element La, the using amount of strategic element cobalt Co is reduced, Ba and Ca with high saturation magnetization and high density are added, the aims of improving remanence and coercive force are fulfilled by optimizing a preparation process and a grain boundary phase, and the ferrite permanent magnet material with high comprehensive performance is prepared, so that Br of the ferrite permanent magnet material can reach more than 4500Gs, and the coercive force can reach more than 5000 Oe.
Detailed Description
The present invention will be further described with reference to the following examples.
The chemical reagents used in the examples of the present invention, unless otherwise specified, are commercially available in a conventional manner.
Example 1
The ferrite permanent magnetic material of the embodiment has a chemical formula of (Sr)1-wBaw)1-x-yLaxCayFe2n-zCozO, wherein x is more than or equal to 0.5 and less than or equal to 0.65, y is more than or equal to 0.3 and less than or equal to 0.5, z is more than or equal to 0.28 and less than or equal to 0.38, n is more than or equal to 4.9 and less than or equal to 5.4, and w is more than or equal to 0.001 and less than or equal to 1.
According to the chemical formula (Sr) of ferrite permanent magnet material1-wBaw)1-x-yLaxCayFe2n-zCozWeighing raw materials of O, wherein x is 0.5, y is 0.3, z is 0.28(La/Co is 1.79), n is 5.2, and w is 0.001, wherein Sr is SrCO3Ba with BaCoO3Ca and CaCO3La and La2O3Co with Co2O3Fe and Fe2O3Adding the mixture in a form.
The preparation method of the ferrite permanent magnetic material of the embodiments 1-3 comprises the following steps:
(1) pre-sintering material mixing: adding raw materials such as iron red, strontium carbonate, barium carbonate, calcium carbonate, lanthanum oxide, cobalt oxide and the like into a sand mill according to a ratio, adding water for slurrying and mixing to obtain slurry;
(2) pre-burning main materials: dewatering the slurry obtained in the step (1), then putting the slurry into a continuous pre-sintering material kiln, sintering at 1185 ℃ to obtain pre-sintering material balls, and then crushing to obtain pre-sintering material powder with the average particle size of 5 microns;
(3) ball milling: putting the pre-sintering powder obtained in the step (2) into a rolling ball mill, referring to table 1, respectively adding 0.6%, 0.8%, 1.1% of calcium carbonate, 0.1%, 0.2%, 0.3% of silicon oxide, 0.1%, 0.2% of boric acid, 0.3% of calcium gluconate and 0.2% of ammonium bicarbonate into examples 1-3, and then adding water for rolling ball milling to obtain slurry with the average particle size of the solid material of 0.72-0.75 μm;
(4) and (3) dehydrating: precipitating or dehydrating the slurry obtained in the step (3) to obtain slurry with the water content of 30%;
(5) molding: the slurry obtained in the step (4) is conveyed into a forming press, and orientation forming is carried out under a 1T magnetic field to obtain the density of 5.0g/cm3Green bodies;
(6) and (3) sintering: placing the green body obtained in the step (5) on a sintering plate, placing the green body into a sintering kiln at 1150 ℃ for sintering, wherein the sintering time is 3h, and the heating rate is 1.3 ℃/min, so that the density is 6.05g/cm3Ferrite permanent magnet material blank.
The ferrite permanent magnet material blanks obtained in examples 1 to 3 were ground and then tested for magnetic properties, and the results are shown in Table 1 below.
TABLE 1 magnetic Properties of the ferrite permanent magnet materials of examples 1-3
Example 2
The ferrite permanent magnetic material of the embodiment has the chemical formula of (Sr)1-wBaw)1-x-yLaxCayFe2n-zCozO, wherein x is more than or equal to 0.5 and less than or equal to 0.65, and y is more than or equal to 0.3 and less than or equal to 0.5，0.28≤z≤0.38，4.9≤n≤5.4，0.001≤w≤1。
According to the chemical formula (Sr) of ferrite permanent magnet material1-wBaw)1-x-yLaxCayFe2n-zCozThe raw materials are weighed according to the following formula that x is 0.6, y is 0.3, z is 0.35(La/Co is 1.71), n is 5.0, and w is 1.
The preparation method of the ferrite permanent magnetic material of the embodiments 4-6 comprises the following steps:
(1) pre-sintering material mixing: adding raw materials such as iron red, strontium carbonate, barium carbonate, calcium carbonate, lanthanum oxide, cobalt oxide and the like into a sand mill according to a ratio, adding water for slurrying and mixing to obtain slurry;
(2) pre-burning main materials: dewatering the slurry obtained in the step (1), then putting the slurry into a continuous pre-sintering material kiln at 1185 ℃ for sintering to obtain pre-sintering material balls, and then crushing to obtain pre-sintering material powder with the average particle size of 5 microns;
(3) ball milling: putting the pre-sintering powder obtained in the step (2) into a rolling ball mill, referring to table 2, respectively adding 0.8%, 1.0% of calcium carbonate, 0.3%, 0.2%, 0.1% of silicon oxide, 0.1%, 0.2% of boric acid, 0.3% of calcium gluconate and 0.2% of ammonium bicarbonate into examples 4-6, and then adding water for rolling ball milling to obtain slurry with the average particle size of the solid material of 0.72-0.75 μm;
(4) and (3) dehydrating: precipitating or dehydrating the slurry obtained in the step (3) to obtain slurry with the water content of 30%;
(5) molding: the slurry obtained in the step (4) is conveyed to a forming press, and orientation forming is carried out under a 1T magnetic field to obtain the slurry with the density of 4.0g/cm3Green bodies;
(6) and (3) sintering: placing the green body obtained in the step (5) on a burning bearing plate, placing the green body into a 1160 ℃ sintering kiln for sintering, wherein the sintering time is 3h, and the heating rate is 1.3 ℃/min, so that the density is 5.2g/cm3Ferrite permanent magnet material blank.
The ferrite permanent magnet material blanks obtained in examples 4 to 6 were ground and tested for their properties, and the results are shown in Table 2 below.
TABLE 2 PERMANENT-MAGNET FERRITE MATERIAL PERFORMANCES OF EXAMPLES 4-6
Claims (10)
1. A ferrite permanent magnetic material is characterized in that: the ferrite permanent magnetic material has a chemical formula of (Sr)1-wBaw）1-x- yLaxCayFe2n-zCozO, wherein x is more than or equal to 0.5 and less than or equal to 0.68, y is more than or equal to 0.3 and less than or equal to 0.5, z is more than or equal to 0.48 and less than or equal to 0.68, n is more than or equal to 4.9 and less than or equal to 5.4, and w is more than or equal to 0.001 and less than or equal to 1; and contains the other elements Si, B and Mn, based on the weight of the oxides, SiO20.2% -0.4% of B2O30.1-0.3 percent of MnO and 0.1-0.3 percent of MnO.
2. The ferrite permanent magnetic material of claim 1, wherein: the chemical formula (Sr)1-wBaw）1-x- yLaxCayFe2n-zCozIn O, La/Co is more than or equal to 1.65.
3. The ferrite permanent magnetic material of claim 1 or 2, characterized in that: the chemical formula (Sr)1-wBaw）1-x- yLaxCayFe2n-zCozIn O, n is more than or equal to 4.9 and less than or equal to 5.1, and w is more than or equal to 0.7 and less than or equal to 1.
4. The ferrite permanent magnetic material of claim 1 or 2, characterized in that: the chemical formula (Sr)1-wBaw）1-x- yLaxCayFe2n-zCozIn O, n is more than or equal to 4.9 and less than or equal to 5.0, and w is more than or equal to 0.1 and less than or equal to 0.3.
5. A method for preparing the ferrite permanent magnetic material as claimed in claims 1 to 4, characterized by comprising the following steps:
(1) pre-sintering material mixing: adding iron red, strontium carbonate, barium carbonate, calcium carbonate, lanthanum oxide and cobalt oxide into a sand mill according to a ratio, adding water for slurrying and mixing to obtain a pre-sintered material;
(2) pre-burning main materials: dehydrating the pre-sintered material obtained in the step (1), placing the dehydrated pre-sintered material in a pre-sintered material kiln for sintering to obtain pre-sintered material balls, and crushing to obtain pre-sintered material powder;
(3) ball milling: putting the pre-sintering material powder obtained in the step (2) into a ball mill, adding silicon oxide, boric acid, calcium gluconate and ammonium bicarbonate, and then adding water for ball milling to obtain slurry;
(4) and (3) dehydrating: precipitating or dehydrating the slurry obtained in the step (3) to obtain slurry with low water content;
(5) molding: placing the dehydrated slurry obtained in the step (4) in a forming press, and carrying out orientation forming in a magnetic field to obtain a green body;
(6) and (3) sintering: and (5) placing the green body obtained in the step (5) on a sintering plate, and sintering in a sintering kiln to obtain a ferrite permanent magnet material blank.
6. The method for preparing a ferrite permanent magnetic material according to claim 5, wherein in the step (2), the sintering temperature is 1185-1200 ℃, and the average particle size of the pre-sintered material powder is less than or equal to 6 microns.
7. The method for preparing a ferrite permanent magnet material according to any one of claims 5 to 6, wherein in the step (3), the addition amount of the silicon oxide is 0.2 to 0.4 percent of the weight of the pre-sintering powder, the addition amount of the boric acid is 0.1 to 0.2 percent of the weight of the pre-sintering powder, the addition amount of the calcium gluconate is 0.1 to 0.3 percent of the weight of the pre-sintering powder, and the addition amount of the ammonium bicarbonate is 0.1 to 0.3 percent of the weight of the pre-sintering powder;
the ball material water ratio of the water to be added for ball milling is 5-15: 1-2, the ball milling method is rolling ball milling, and the ball milling time is 12-20 hours;
in the slurry, the granularity of the solid material is 0.65-0.78 μm; the pH value of the slurry is less than or equal to 9.
8. The method for preparing a ferrite permanent magnetic material according to any one of claims 5 to 7, wherein in the step (4), the water content of the slurry with low water content is 30% to 35%.
9. The method for preparing a ferrite permanent magnet material according to any of claims 5 to 8, wherein in the step (5), the magnetic field forming magnetic field strength is not less than 0.7T, and the green density is not less than 3.0g/cm3。
10. The method for preparing a ferrite permanent magnet material according to any one of claims 5 to 9, wherein in the step (6), the sintering temperature is 1120 ℃ to 1160 ℃, the sintering time is 2h to 4h, the sintering temperature rise rate is 0.1 ℃/min to 3 ℃/min, and the sintered blank density is more than or equal to 5.05g/cm3。
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