CN103232232A - Permanent magnetic ferrite preparation method - Google Patents
Permanent magnetic ferrite preparation method Download PDFInfo
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- CN103232232A CN103232232A CN2013101745498A CN201310174549A CN103232232A CN 103232232 A CN103232232 A CN 103232232A CN 2013101745498 A CN2013101745498 A CN 2013101745498A CN 201310174549 A CN201310174549 A CN 201310174549A CN 103232232 A CN103232232 A CN 103232232A
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Abstract
The invention relates to the field of chemicals, in particular relates to the field of industrial chemicals, and specifically relates to a permanent magnetic ferrite preparation method. The method is particularly suitable for a permanent magnetic ferrite material which adopts a current production mode in China, and the permanent magnetic ferrite material utilizes a presintering material as a base, is prepared by adding rare earth element into a secondary formula and has high residual magnetic flux density Br, high coercive force Hcb and high intrinsic coercive force Hcj.
Description
Technical field
The present invention relates to chemical field, particularly relate to industrial chemical field, relate to a kind of preparation method of permanent-magnet ferrite magnet specifically.
Background technology
Permanent-magnet ferrite material plays an important role in industries such as household electrical appliances, computer, automobile, communications as an important component part of magneticsubstance.Along with science and technology development, electronics is towards miniaturization, lightness, slimming development, the demands for higher performance of giving permanent-magnet ferrite material.The interpolation of rare earth element provides valid approach to developing the high-performance permanent-magnet ferrite magneticsubstance.
The interpolation of rare earth element mainly contains two kinds of addition manners, a kind of mode is once to add rare earth element in the prescription, this kind mode advantage rare earth element enters ferrite lattice easily, can prepare the very high ferrite device of magnetic property, but because a lot of enterprises of China all are the pre-imitation frosted glass of buying now, so just limited the interpolation of a rare earth element.
Another mode is to add rare earth element in the secondary prescription, and the rare earth element that adds by this kind mode improves to the magnetic property of product, but more limited.Add rare earth element at present in the secondary prescription, the performance of preparation is substantially in the FB6B of TDK company, FB6H level.
| The trade mark | Br(mT) | Hcb(kA/m) | Hcj(kA/m) | BHmax(kJ/m 3) |
| FB6B | 420±10 | 302.4±12 | 318.3±12 | 33.4±1.6 |
| |
400±10 | 302.4±12 | 358.1±12 | 30.3±1.6 |
As mentioned above, only in the secondary prescription, add rare earth element, can't obtain Br 〉=420mT as LaCo, while Hcb 〉=320kA/m, the high-performance permanent magnetic ferrite material of Hcj 〉=365kA/m.
Summary of the invention
The invention provides a kind of preparation method of permanent-magnet ferrite magnet, particularly be applicable to the present production model of China based on pre-imitation frosted glass, only by in the secondary prescription, adding rare earth element, obtain to have simultaneously high residual magnetic flux density Br, high-coercive force Hcb, the permanent-magnet ferrite material of high HCJ Hcj.
The preparation method of high-coercive force permanent-magnet ferrite magnet disclosed in this invention comprises the steps:
(1) wet-milling batch mixing: be the wet-milling dispersion medium with water, raw material and an additive are added in the ball mill simultaneously, carry out 1 ~ 20 hour wet-milling batch mixing, obtain the wet-milling slip, slurry oven dry back powder specific surface area is 1 ~ 10m
2/ g.
(2)A pre-burning: compounding process gained slip is carried out pre-burning in air, temperature is 1150 ~ 1350 ℃, and soaking time 1 ~ 5 hour obtains once pre-imitation frosted glass;
(3) coarse reduction: utilize ball mill to pulverize above-mentioned once pre-imitation frosted glass, obtain meal, carry out the grade screening simultaneously, granularity reaches 1 ~ 6 μ m;
(4) fine grinding: coarse reduction gained meal being added secondary additive adopt ball mill to carry out fine grinding, is dispersion medium with water, obtains the fine grinding slip, and fine grinding slip oven dry back powder granularity is 0.2 ~ 1.0 μ m, and specific surface area is 1 ~ 12m
2/ g.Contain the following composition of calculating by weight percentage in the described secondary additive, iron oxide red=1 ~ 20wt%, La
2O
3=1.0 ~ 5.0wt%;
(5) wet pressing pressing under magnetic field: adopt the wet method pressing under magnetic field, the fine grinding slip simmer down to that above-mentioned fine grinding is obtained is moisture to be 35 ~ 55% moulding slip, is that 6 ~ 18kOe, forming pressure are 0.1 ~ 1.0ton/cm at externally-applied magnetic field
2Condition under be pressed into green compact;
(6) double sintering: the obtained by molding green compact are carried out sintering in air, temperature is 1050 ~ 1250 ℃, and soaking time 1 ~ 6 hour obtains ripe base;
(7) mill processing: adopt self-acting grinding machine that ripe base is polished.
By preparation technology provided by the invention, can realize that with pre-imitation frosted glass be basic raw material, in the secondary prescription, add rare earth element and obtain Br 〉=420mT, while Hcb 〉=320kA/m, the high-performance permanent magnetic ferrite material of Hcj 〉=365kA/m.
Simultaneously, the present invention further preferably discloses in the described step (1), and the wet-milling batch mixing is according to Fe
2O
3With SrCO
3The preparation of major ingredient is carried out in mol ratio n=5.9 ~ 6.5, and one time additive formula is: CaCO
3=0.1 ~ 1.0wt%, SiO
2=0.1 ~ 1.0wt%, Al
2O
3=0 ~ 1.4wt%, kaolin=0 ~ 1.0wt%.
Also add one or both and above secondary additive: CaCO in the following additive when simultaneously, the invention also discloses fine grinding
3=0 ~ 1.6wt%, SiO
2=0.1 ~ 1.0wt%, H
3BO
3=0.1 ~ 1.0 wt%, Al
2O
3=0 ~ 1.4wt%, kaolin=0 ~ 1.0wt%, Co
2O
3=1.0 ~ 4.0wt%, SrCO
3=0 ~ 1.2wt%, calglucon=0 ~ 1.0wt%.
Thereby be starting point with the present production status of China, by improving production technique, realize that rare earth element as secondary additive, effectively improves the purpose of product magnetic property.
Description of drawings
Fig. 1 is sample demagnetizing curve figure among the embodiment 1.
Embodiment
Below be the specific embodiment of the present invention, technical characterictic of the present invention is described further, but the present invention is not limited to this example.
Embodiment 1
The wet-milling batch mixing: be the wet-milling dispersion medium with water, raw material and an additive are added in the ball mill simultaneously, carry out 2 hours wet-milling batch mixing, obtain the wet-milling slip, slurry oven dry back powder specific surface area is 2m
2/ g.Major ingredient iron oxide red and Strontium carbonate powder in the present embodiment are according to Fe
2O
3With SrCO
3Mol ratio n=6.18 carries out the preparation of major ingredient, and one time additive formula is: CaCO
3=0.2wt%, SiO
2=0.3wt%;
A pre-burning: compounding process gained slip is carried out pre-burning in air, temperature is 1260 ℃, and soaking time 3 hours obtains once pre-imitation frosted glass;
Coarse reduction: utilize ball mill to pulverize above-mentioned once pre-imitation frosted glass, obtain meal, carry out the grade screening simultaneously, granularity reaches 4.0 μ m;
Fine grinding: coarse reduction gained meal being added secondary additive adopt ball mill to carry out fine grinding, is dispersion medium with water, obtains the fine grinding slip, and fine grinding slip oven dry back powder granularity is about 0.7 μ m, and slurry oven dry back powder specific surface area is 2.2 m
2/ g.Add following secondary additive: iron oxide red=4.5wt%, CaCO
3=0.7wt%, SiO
2=0.4wt%, H
3BO
3=0.2wt%, La
2O
3=2.6wt%, Co
2O
3=1.31wt%, SrCO
3=0.73wt%, calglucon=0.5wt%;
The wet pressing pressing under magnetic field: adopt the wet method pressing under magnetic field, the fine grinding slip simmer down to that above-mentioned fine grinding is obtained is moisture to be 40% moulding slip, is that 15kOe, forming pressure are 0.35ton/cm at externally-applied magnetic field
2Condition under be pressed into the cylindrical green body of φ 28.5mm;
Double sintering: the obtained by molding green compact are carried out sintering in air, temperature is 1195 ℃, and soaking time 2 hours obtains ripe base;
Mill processing: adopt self-acting grinding machine that ripe base cylinder upper and lower surface is polished.
Obtain the permanent-magnet ferrite sample at last.
Above-mentioned sample detection magnetic property: Br=423.2mT, Hcb=323.4kA/m, Hcj=366.7kA/m, (BH) max=35.8kJ/m
3The sample demagnetizing curve is referring to Fig. 1.
Embodiment 2
The wet-milling batch mixing: be the wet-milling dispersion medium with water, raw material and an additive are added in the ball mill simultaneously, carry out 10 hours wet-milling batch mixing, obtain the wet-milling slip, slurry oven dry back powder specific surface area is 5m
2/ g.Major ingredient iron oxide red and Strontium carbonate powder in the present embodiment are according to Fe
2O
3With SrCO
3Mol ratio n=6.18 carries out the preparation of major ingredient, and one time additive formula is: CaCO
3=0.2wt%, SiO
2=0.1wt%, Al
2O
3=0.6wt%;
A pre-burning: compounding process gained slip is carried out pre-burning in air, temperature is 1260 ℃, and soaking time 3 hours obtains once pre-imitation frosted glass;
Coarse reduction: utilize ball mill to pulverize above-mentioned once pre-imitation frosted glass, obtain meal, carry out the grade screening simultaneously, granularity reaches 4.0 μ m;
Fine grinding: coarse reduction gained meal being added secondary additive adopt ball mill to carry out fine grinding, is dispersion medium with water, obtains the fine grinding slip, and fine grinding slip oven dry back powder granularity is about 0.7 μ m, and slurry oven dry back powder specific surface area is 2.2 m
2/ g.Add following secondary additive: iron oxide red=4.5wt%, CaCO
3=0.7wt%, SiO
2=0.2wt%, H
3BO
3=0.2wt%, La
2O
3=2.6wt%, Co
2O
3=1.31wt%, SrCO
3=0.73wt%, calglucon=0.5wt%, kaolin=0.3wt%;
The wet pressing pressing under magnetic field: adopt the wet method pressing under magnetic field, the fine grinding slip simmer down to that above-mentioned fine grinding is obtained is moisture to be 40% moulding slip, is that 15kOe, forming pressure are 0.35ton/cm at externally-applied magnetic field
2Condition under be pressed into the cylindrical green body of φ 28.5mm;
Double sintering: the obtained by molding green compact are carried out sintering in air, temperature is 1195 ℃, and soaking time 2 hours obtains ripe base;
Mill processing: adopt self-acting grinding machine that ripe base cylinder upper and lower surface is polished.
Obtain the permanent-magnet ferrite sample at last.
Above-mentioned sample detection magnetic property: Br=420.0mT, Hcb=324.9kA/m, Hcj=369.2kA/m, (BH) max=35.2kJ/m
3
Embodiment 3
The wet-milling batch mixing: be the wet-milling dispersion medium with water, raw material and an additive are added in the ball mill simultaneously, carry out 20 hours wet-milling batch mixing, obtain the wet-milling slip, slurry oven dry back powder specific surface area is 10m
2/ g.Major ingredient iron oxide red and Strontium carbonate powder in the present embodiment are according to Fe
2O
3With SrCO
3Mol ratio n=6.18 carries out the preparation of major ingredient, and one time additive formula is: CaCO
3=0.2wt%, SiO
2=0.1wt%, Al
2O
3=0.2wt%, kaolin=0.3wt%;
A pre-burning: compounding process gained slip is carried out pre-burning in air, temperature is 1260 ℃, and soaking time 3 hours obtains once pre-imitation frosted glass;
Coarse reduction: utilize ball mill to pulverize above-mentioned once pre-imitation frosted glass, obtain meal, carry out the grade screening simultaneously, granularity reaches 4.0 μ m;
Fine grinding: coarse reduction gained meal being added secondary additive adopt ball mill to carry out fine grinding, is dispersion medium with water, obtains the fine grinding slip, and fine grinding slip oven dry back powder granularity is about 0.7 μ m, and slurry oven dry back powder specific surface area is 2.2 m
2/ g.Add following secondary additive: iron oxide red=4.5wt%, CaCO
3=0.7wt%, SiO
2=0.1wt%, H
3BO
3=0.2wt%, La
2O
3=2.6wt%, Co
2O
3=1.31wt%, SrCO
3=0.73wt%, calglucon=0.5wt%, kaolin=0.2wt%, Al
2O
3=0.3wt%;
The wet pressing pressing under magnetic field: adopt the wet method pressing under magnetic field, the fine grinding slip simmer down to that above-mentioned fine grinding is obtained is moisture to be 40% moulding slip, is that 15kOe, forming pressure are 0.35ton/cm at externally-applied magnetic field
2Condition under be pressed into the cylindrical green body of φ 28.5mm;
Double sintering: the obtained by molding green compact are carried out sintering in air, temperature is 1195 ℃, and soaking time 2 hours obtains ripe base;
Mill processing: adopt self-acting grinding machine that ripe base cylinder upper and lower surface is polished.
Obtain the permanent-magnet ferrite sample at last.
Above-mentioned sample detection magnetic property: Br=420.4mT, Hcb=321.5kA/m, Hcj=368.9kA/m, (BH) max=35kJ/m
3
Embodiment 4
The wet-milling batch mixing: be the wet-milling dispersion medium with water, raw material and an additive are added in the ball mill simultaneously, carry out 2 hours wet-milling batch mixing, obtain the wet-milling slip, slurry oven dry back powder specific surface area is 2m
2/ g.Major ingredient iron oxide red and Strontium carbonate powder in the present embodiment are according to Fe
2O
3With SrCO
3Mol ratio n=6.18 carries out the preparation of major ingredient, and one time additive formula is: CaCO
3=0.2wt%, SiO
2=0.3wt%;
A pre-burning: compounding process gained slip is carried out pre-burning in air, temperature is 1260 ℃, and soaking time 3 hours obtains once pre-imitation frosted glass;
Coarse reduction: utilize ball mill to pulverize above-mentioned once pre-imitation frosted glass, obtain meal, carry out the grade screening simultaneously, granularity reaches 4.0 μ m;
Fine grinding: coarse reduction gained meal being added secondary additive adopt ball mill to carry out fine grinding, is dispersion medium with water, obtains the fine grinding slip, and fine grinding slip oven dry back powder granularity is about 0.7 μ m, and slurry oven dry back powder specific surface area is 2.2 m
2/ g.Add following secondary additive: iron oxide red=6.0wt%, CaCO
3=0.7wt%, SiO
2=0.4wt%, H
3BO
3=0.2wt%, La
2O
3=2.6wt%, Co
2O
3=1.31wt%, SrCO
3=0.73wt%, calglucon=0.5wt%;
The wet pressing pressing under magnetic field: adopt the wet method pressing under magnetic field, the fine grinding slip simmer down to that above-mentioned fine grinding is obtained is moisture to be 40% moulding slip, is that 15kOe, forming pressure are 0.35ton/cm at externally-applied magnetic field
2Condition under be pressed into the cylindrical green body of φ 28.5mm;
Double sintering: the obtained by molding green compact are carried out sintering in air, temperature is 1195 ℃, and soaking time 2 hours obtains ripe base;
Mill processing: adopt self-acting grinding machine that ripe base cylinder upper and lower surface is polished.
Obtain the permanent-magnet ferrite sample at last.
Above-mentioned sample detection magnetic property: Br=421.8mT, Hcb=323.8kA/m, Hcj=370.5kA/m, (BH) max=34.9kJ/m
3
Embodiment 5
The wet-milling batch mixing: be the wet-milling dispersion medium with water, raw material and an additive are added in the ball mill simultaneously, carry out 2 hours wet-milling batch mixing, obtain the wet-milling slip, slurry oven dry back powder specific surface area is 2m
2/ g.Major ingredient iron oxide red and Strontium carbonate powder in the present embodiment are according to Fe
2O
3With SrCO
3Mol ratio n=6.18 carries out the preparation of major ingredient, and one time additive formula is: CaCO
3=0.2wt%, SiO
2=0.3wt%;
A pre-burning: compounding process gained slip is carried out pre-burning in air, temperature is 1260 ℃, and soaking time 3 hours obtains once pre-imitation frosted glass;
Coarse reduction: utilize ball mill to pulverize above-mentioned once pre-imitation frosted glass, obtain meal, carry out the grade screening simultaneously, granularity reaches 4.0 μ m;
Fine grinding: coarse reduction gained meal being added secondary additive adopt ball mill to carry out fine grinding, is dispersion medium with water, obtains the fine grinding slip, and fine grinding slip oven dry back powder granularity is about 0.7 μ m, and slurry oven dry back powder specific surface area is 2.2 m
2/ g.Add following secondary additive: iron oxide red=7.5wt%, CaCO
3=0.7wt%, SiO
2=0.4wt%, H
3BO
3=0.2wt%, La
2O
3=2.6wt%, Co
2O
3=1.31wt%, SrCO
3=0.73wt%, calglucon=0.5wt%;
The wet pressing pressing under magnetic field: adopt the wet method pressing under magnetic field, the fine grinding slip simmer down to that above-mentioned fine grinding is obtained is moisture to be 40% moulding slip, is that 15kOe, forming pressure are 0.35ton/cm at externally-applied magnetic field
2Condition under be pressed into the cylindrical green body of φ 28.5mm;
Double sintering: the obtained by molding green compact are carried out sintering in air, temperature is 1185 ℃, and soaking time 2 hours obtains ripe base;
Mill processing: adopt self-acting grinding machine that ripe base cylinder upper and lower surface is polished.
Obtain the permanent-magnet ferrite sample at last.
Above-mentioned sample detection magnetic property: Br=423.0mT, Hcb=321.6kA/m, Hcj=365.2kA/m, (BH) max=35.1kJ/m
3
Embodiment 6
The wet-milling batch mixing: be the wet-milling dispersion medium with water, raw material and an additive are added in the ball mill simultaneously, carry out 2 hours wet-milling batch mixing, obtain the wet-milling slip, slurry oven dry back powder specific surface area is 2m
2/ g.Major ingredient iron oxide red and Strontium carbonate powder in the present embodiment are according to Fe
2O
3With SrCO
3Mol ratio n=6.18 carries out the preparation of major ingredient, and one time additive formula is: CaCO
3=0.2wt%, SiO
2=0.3wt%;
A pre-burning: compounding process gained slip is carried out pre-burning in air, temperature is 1260 ℃, and soaking time 3 hours obtains once pre-imitation frosted glass;
Coarse reduction: utilize ball mill to pulverize above-mentioned once pre-imitation frosted glass, obtain meal, carry out the grade screening simultaneously, granularity reaches 4.0 μ m;
Fine grinding: coarse reduction gained meal being added secondary additive adopt ball mill to carry out fine grinding, is dispersion medium with water, obtains the fine grinding slip, and fine grinding slip oven dry back powder granularity is about 0.7 μ m, and slurry oven dry back powder specific surface area is 2.2 m
2/ g.Add following secondary additive: iron oxide red=9.0wt%, CaCO
3=0.7wt%, SiO
2=0.4wt%, H
3BO
3=0.2wt%, La
2O
3=2.6wt%, Co
2O
3=1.31wt%, SrCO
3=0.73wt%, calglucon=0.5wt%;
The wet pressing pressing under magnetic field: adopt the wet method pressing under magnetic field, the fine grinding slip simmer down to that above-mentioned fine grinding is obtained is moisture to be 40% moulding slip, is that 15kOe, forming pressure are 0.35ton/cm at externally-applied magnetic field
2Condition under be pressed into the cylindrical green body of φ 28.5mm;
Double sintering: the obtained by molding green compact are carried out sintering in air, temperature is 1190 ℃, and soaking time 2 hours obtains ripe base;
Mill processing: adopt self-acting grinding machine that ripe base cylinder upper and lower surface is polished.
Obtain the permanent-magnet ferrite sample at last.
Above-mentioned sample detection magnetic property: Br=422.0mT, Hcb=320.6kA/m, Hcj=365.3kA/m, (BH) max=35kJ/m
3
Embodiment 7
The wet-milling batch mixing: be the wet-milling dispersion medium with water, raw material and an additive are added in the ball mill simultaneously, carry out 2 hours wet-milling batch mixing, obtain the wet-milling slip, slurry oven dry back powder specific surface area is 2m
2/ g.Major ingredient iron oxide red and Strontium carbonate powder in the present embodiment are according to Fe
2O
3With SrCO
3Mol ratio n=6.18 carries out the preparation of major ingredient, and one time additive formula is: CaCO
3=0.2wt%, SiO
2=0.3wt%;
A pre-burning: compounding process gained slip is carried out pre-burning in air, temperature is 1260 ℃, and soaking time 3 hours obtains once pre-imitation frosted glass;
Coarse reduction: utilize ball mill to pulverize above-mentioned once pre-imitation frosted glass, obtain meal, carry out the grade screening simultaneously, granularity reaches 4.0 μ m;
Fine grinding: coarse reduction gained meal being added secondary additive adopt ball mill to carry out fine grinding, is dispersion medium with water, obtains the fine grinding slip, and fine grinding slip oven dry back powder granularity is about 0.7 μ m, and slurry oven dry back powder specific surface area is 2.2 m
2/ g.Add following secondary additive: iron oxide red=11.0wt%, CaCO
3=1.0wt%, SiO
2=0.4wt%, H
3BO
3=0.2wt%, La
2O
3=2.6wt%, Co
2O
3=1.31wt%, SrCO
3=0.85wt%, calglucon=0.5wt%;
The wet pressing pressing under magnetic field: adopt the wet method pressing under magnetic field, the fine grinding slip simmer down to that above-mentioned fine grinding is obtained is moisture to be 40% moulding slip, is that 15kOe, forming pressure are 0.35ton/cm at externally-applied magnetic field
2Condition under be pressed into the cylindrical green body of φ 28.5mm;
Double sintering: the obtained by molding green compact are carried out sintering in air, temperature is 1195 ℃, and soaking time 2 hours obtains ripe base;
Mill processing: adopt self-acting grinding machine that ripe base cylinder upper and lower surface is polished.
Obtain the permanent-magnet ferrite sample at last.
Above-mentioned sample detection magnetic property: Br=422.4mT, Hcb=322.8kA/m, Hcj=366.4kA/m, (BH) max=35.8kJ/m
3
Embodiment 8
The wet-milling batch mixing: be the wet-milling dispersion medium with water, raw material and an additive are added in the ball mill simultaneously, carry out 2 hours wet-milling batch mixing, obtain the wet-milling slip, slurry oven dry back powder specific surface area is 2m
2/ g.Major ingredient iron oxide red and Strontium carbonate powder in the present embodiment are according to Fe
2O
3With SrCO
3Mol ratio n=6.18 carries out the preparation of major ingredient, and one time additive formula is: CaCO
3=0.2wt%, SiO
2=0.3wt%;
A pre-burning: compounding process gained slip is carried out pre-burning in air, temperature is 1260 ℃, and soaking time 3 hours obtains once pre-imitation frosted glass;
Coarse reduction: utilize ball mill to pulverize above-mentioned once pre-imitation frosted glass, obtain meal, carry out the grade screening simultaneously, granularity reaches 4.0 μ m;
Fine grinding: coarse reduction gained meal being added secondary additive adopt ball mill to carry out fine grinding, is dispersion medium with water, obtains the fine grinding slip, and fine grinding slip oven dry back powder granularity is about 0.7 μ m, and slurry oven dry back powder specific surface area is 2.2 m
2/ g.Add following secondary additive: iron oxide red=13.5wt%, CaCO
3=1.0wt%, SiO
2=0.4wt%, H
3BO
3=0.2wt%, La
2O
3=2.6wt%, Co
2O
3=1.31wt%, SrCO
3=0.85wt%, calglucon=0.5wt%;
The wet pressing pressing under magnetic field: adopt the wet method pressing under magnetic field, the fine grinding slip simmer down to that above-mentioned fine grinding is obtained is moisture to be 40% moulding slip, is that 15kOe, forming pressure are 0.35ton/cm at externally-applied magnetic field
2Condition under be pressed into the cylindrical green body of φ 28.5mm;
Double sintering: the obtained by molding green compact are carried out sintering in air, temperature is 1195 ℃, and soaking time 2 hours obtains ripe base;
Mill processing: adopt self-acting grinding machine that ripe base cylinder upper and lower surface is polished.
Obtain the permanent-magnet ferrite sample at last.
Above-mentioned sample detection magnetic property: Br=420.1mT, Hcb=323.6kA/m, Hcj=367.6kA/m, (BH) max=34.8kJ/m
3
Embodiment 9
The wet-milling batch mixing: be the wet-milling dispersion medium with water, raw material and an additive are added in the ball mill simultaneously, carry out 2 hours wet-milling batch mixing, obtain the wet-milling slip, slurry oven dry back powder specific surface area is 2m
2/ g.Major ingredient iron oxide red and Strontium carbonate powder in the present embodiment are according to Fe
2O
3With SrCO
3Mol ratio n=6.18 carries out the preparation of major ingredient, and one time additive formula is: CaCO
3=0.2wt%, SiO
2=0.3wt%;
A pre-burning: compounding process gained slip is carried out pre-burning in air, temperature is 1260 ℃, and soaking time 3 hours obtains once pre-imitation frosted glass;
Coarse reduction: utilize ball mill to pulverize above-mentioned once pre-imitation frosted glass, obtain meal, carry out the grade screening simultaneously, granularity reaches 4.0 μ m;
Fine grinding: coarse reduction gained meal being added secondary additive adopt ball mill to carry out fine grinding, is dispersion medium with water, obtains the fine grinding slip, and fine grinding slip oven dry back powder granularity is about 0.7 μ m, and slurry oven dry back powder specific surface area is 2.2 m
2/ g.Add following secondary additive: iron oxide red=16.0wt%, CaCO
3=1.0wt%, SiO
2=0.4wt%, H
3BO
3=0.2wt%, La
2O
3=2.6wt%, Co
2O
3=1.31wt%, SrCO
3=0.85wt%, calglucon=0.5wt%;
The wet pressing pressing under magnetic field: adopt the wet method pressing under magnetic field, the fine grinding slip simmer down to that above-mentioned fine grinding is obtained is moisture to be 40% moulding slip, is that 15kOe, forming pressure are 0.35ton/cm at externally-applied magnetic field
2Condition under be pressed into the cylindrical green body of φ 28.5mm;
Double sintering: the obtained by molding green compact are carried out sintering in air, temperature is 1195 ℃, and soaking time 2 hours obtains ripe base;
Mill processing: adopt self-acting grinding machine that ripe base cylinder upper and lower surface is polished.
Obtain the permanent-magnet ferrite sample at last.
Above-mentioned sample detection magnetic property: Br=420.3mT, Hcb=321.2kA/m, Hcj=365.2kA/m, (BH) max=34.9kJ/m
3
Reference examples 1
The wet-milling batch mixing: be the wet-milling dispersion medium with water, raw material and an additive are added in the ball mill simultaneously, carry out 2 hours wet-milling batch mixing, obtain the wet-milling slip, slurry oven dry back powder specific surface area is 2m
2/ g.Major ingredient iron oxide red and Strontium carbonate powder in the present embodiment are according to Fe
2O
3With SrCO
3Mol ratio n=6.18 carries out the preparation of major ingredient, and one time additive formula is: CaCO
3=0.2wt%, SiO
2=0.3wt%;
A pre-burning: compounding process gained slip is carried out pre-burning in air, temperature is 1260 ℃, and soaking time 3 hours obtains once pre-imitation frosted glass;
Coarse reduction: utilize ball mill to pulverize above-mentioned once pre-imitation frosted glass, obtain meal, carry out the grade screening simultaneously, granularity reaches 4.0 μ m;
Fine grinding: coarse reduction gained meal being added secondary additive adopt ball mill to carry out fine grinding, is dispersion medium with water, obtains the fine grinding slip, and fine grinding slip oven dry back powder granularity is about 0.70 μ m, and slurry oven dry back powder specific surface area is 2.2 m
2/ g.Add following secondary additive: CaCO
3=1.0wt%, SiO
2=0.3wt%, H
3BO
3=0.2wt%, La
2O
3=2.6wt%, Co
2O
3=1.31wt%, calglucon=0.5wt%;
The wet pressing pressing under magnetic field: adopt the wet method pressing under magnetic field, the fine grinding slip simmer down to that above-mentioned fine grinding is obtained is moisture to be 40% moulding slip, is that 15kOe, forming pressure are 0.35ton/cm at externally-applied magnetic field
2Condition under be pressed into the cylindrical green body of φ 28.5mm;
Double sintering: the obtained by molding green compact are carried out sintering in air, temperature is 1180 ℃, and soaking time 2 hours obtains ripe base;
Mill processing: adopt self-acting grinding machine that ripe base cylinder upper and lower surface is polished.
Obtain contrast permanent-magnet ferrite sample one at last.
Embodiment 10
The wet-milling batch mixing: be the wet-milling dispersion medium with water, raw material and an additive are added in the ball mill simultaneously, carry out 2 hours wet-milling batch mixing, obtain the wet-milling slip, slurry oven dry back powder specific surface area is 2m
2/ g.Major ingredient iron oxide red and Strontium carbonate powder in the present embodiment are according to Fe
2O
3With SrCO
3Mol ratio n=6.18 carries out the preparation of major ingredient, and one time additive formula is: CaCO
3=0.2wt%, SiO
2=0.3wt%;
A pre-burning: compounding process gained slip is carried out pre-burning in air, temperature is 1260 ℃, and soaking time 3 hours obtains once pre-imitation frosted glass;
Coarse reduction: utilize ball mill to pulverize above-mentioned once pre-imitation frosted glass, obtain meal, carry out the grade screening simultaneously, granularity reaches 4.0 μ m;
Fine grinding: coarse reduction gained meal being added secondary additive adopt ball mill to carry out fine grinding, is dispersion medium with water, obtains the fine grinding slip, and fine grinding slip oven dry back powder granularity is about 0.70 μ m, and slurry oven dry back powder specific surface area is 2.2 m
2/ g.Add following secondary additive: iron oxide red=4.5wt%, CaCO
3=1.0wt%, SiO
2=0.3wt%, H
3BO
3=0.2wt%, La
2O
3=2.6wt%, Co
2O
3=1.31wt%, calglucon=0.5wt%;
The wet pressing pressing under magnetic field: adopt the wet method pressing under magnetic field, the fine grinding slip simmer down to that above-mentioned fine grinding is obtained is moisture to be 40% moulding slip, is that 15kOe, forming pressure are 0.35ton/cm at externally-applied magnetic field
2Condition under be pressed into the cylindrical green body of φ 28.5mm;
Double sintering: the obtained by molding green compact are carried out sintering in air, temperature is 1180 ℃, and soaking time 2 hours obtains ripe base;
Mill processing: adopt self-acting grinding machine that ripe base cylinder upper and lower surface is polished.
Obtain contrast permanent-magnet ferrite sample two at last.
Embodiment 11
Obtain permanent-magnet ferrite sample one and permanent-magnet ferrite sample two respectively according to disclosed mode among Comparative Examples 1 and the embodiment 10, parallel control carries out the magnetic property detection then, and the result is as shown in the table:
| Sample number into spectrum | Br(mT) | Hcb(kA/m) | Hcj(kA/m) | BHmax(kJ/m 3) |
| One | 420.4 | 307.6 | 342.4 | 34.8 |
| Two | 421.6 | 321.8 | 367.2 | 35.2 |
Claims (3)
1. the preparation method of a permanent-magnet ferrite magnet, it is characterized in that: the magnet performance of the described high-coercive force permanent-magnet ferrite magnet for preparing reaches Br 〉=420mT, Hcb 〉=320kA/m, Hcj 〉=365kA/m, concrete preparation method comprises the following steps:
(1) wet-milling batch mixing: be the wet-milling dispersion medium with water, raw material and an additive are added in the ball mill simultaneously, carry out 1 ~ 20 hour wet-milling batch mixing, obtain the wet-milling slip, slurry oven dry back powder specific surface area is 1 ~ 10m
2/ g;
(2) pre-burnings: compounding process gained slip is carried out pre-burning in air, temperature is 1150 ~ 1350 ℃, and soaking time 1 ~ 5 hour obtains once pre-imitation frosted glass;
(3) coarse reduction: utilize ball mill to pulverize above-mentioned once pre-imitation frosted glass, obtain meal, carry out the grade screening simultaneously, granularity reaches 1 ~ 6 μ m;
(4) fine grinding: coarse reduction gained meal being added secondary additive adopt ball mill to carry out fine grinding, is dispersion medium with water, obtains the fine grinding slip, and fine grinding slip oven dry back powder granularity is 0.2 ~ 1.0 μ m, and specific surface area is 1 ~ 12m
2/ g;
Contain the following composition of calculating by weight percentage in the described secondary additive, iron oxide red=1 ~ 20wt%, La
2O
3=1.0 ~ 5.0wt%;
(5) wet pressing pressing under magnetic field: adopt the wet method pressing under magnetic field, the fine grinding slip simmer down to that above-mentioned fine grinding is obtained is moisture to be 35 ~ 55% moulding slip, is that 6 ~ 18kOe, forming pressure are 0.1 ~ 1.0ton/cm at externally-applied magnetic field
2Condition under be pressed into green compact;
(6) double sintering: the obtained by molding green compact are carried out sintering in air, temperature is 1050 ~ 1250 ℃, and soaking time 1 ~ 6 hour obtains ripe base;
(7) mill processing: adopt self-acting grinding machine that ripe base is polished.
2. according to the preparation method of the described a kind of permanent-magnet ferrite magnet of claim 1, it is characterized in that: in the described step (1), the wet-milling batch mixing is according to Fe
2O
3With SrCO
3The preparation of major ingredient is carried out in mol ratio n=5.9 ~ 6.5, and one time additive formula is: CaCO
3=0.1 ~ 1.0wt%, SiO
2=0.1 ~ 1.0wt%, Al
2O
3=0 ~ 1.4wt%, kaolin=0 ~ 1.0wt%.
3. according to the preparation method of the described a kind of permanent-magnet ferrite magnet of claim 1, it is characterized in that: also add one or both and above secondary additive: CaCO in the following additive during fine grinding
3=0 ~ 1.6wt%, SiO
2=0.1 ~ 1.0wt%, H
3BO
3=0.1 ~ 1.0 wt%, Al
2O
3=0 ~ 1.4wt%, kaolin=0 ~ 1.0wt%, Co
2O
3=1.0 ~ 4.0wt%, SrCO
3=0 ~ 1.2wt%, calglucon=0 ~ 1.0wt%.
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Cited By (5)
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| CN104591744A (en) * | 2014-12-19 | 2015-05-06 | 江西佳宝磁材有限公司 | Method for improving magnetic properties of permanent magnetic ferrite by adding combined dispersing agent |
| CN104609843A (en) * | 2014-12-11 | 2015-05-13 | 南京梅山冶金发展有限公司 | Preparation method for non-rare-earth high-remanent-magnetism permanent-magnetism ferrite |
| CN107399964A (en) * | 2017-08-21 | 2017-11-28 | 北矿磁材科技有限公司 | A kind of preparation method of bonded ferrite magnetic powder |
| CN109336579A (en) * | 2018-11-14 | 2019-02-15 | 横店集团东磁股份有限公司 | A kind of motor Ferrite Material and preparation method thereof |
| 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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