CN109346261B - Ferro-aluminum magnetic material with high cerium content and smelting method thereof - Google Patents
Ferro-aluminum magnetic material with high cerium content and smelting method thereof Download PDFInfo
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- CN109346261B CN109346261B CN201811350025.9A CN201811350025A CN109346261B CN 109346261 B CN109346261 B CN 109346261B CN 201811350025 A CN201811350025 A CN 201811350025A CN 109346261 B CN109346261 B CN 109346261B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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Abstract
The invention belongs to the technical field of magnetic material smelting, and provides a high-cerium-content bauxite magnetic material and a smelting method thereof, aiming at solving the problems that the consumption of neodymium in the existing rare earth neodymium-iron-boron permanent magnetic material accounts for 25-30%, but the utilization of rare earth resources is extremely unbalanced, so that a large amount of lanthanum and cerium are accumulated, and the magnetic performance is unstable and greatly reduced after lanthanum and cerium are added. The composite material consists of the following raw materials in percentage by mass: proportioning before hydrogen crushing: 13% -16% of praseodymium-neodymium steel ingot, 6% -40% of cerium steel ingot and 45% -80% of waste block, wherein the waste block is a scrapped product of neodymium-iron-boron magnetic material equipment, and the content of praseodymium and neodymium is more than 30%. Can achieve the stability of magnetic performance and meet the requirements of customers. The grain boundary structure in the neodymium iron boron permanent magnet material obtained by the preparation method is continuous and uniform, and the magnetic isolation effect between adjacent grains is enhanced, so that the coercive force of the neodymium iron boron permanent magnet material can be effectively improved, and the magnetic performance is excellent.
Description
Technical Field
The invention belongs to the technical field of smelting of magnetic materials, and particularly relates to a high-cerium-content ferro-aluminum magnetic material and a smelting method thereof.
Background
The rare earth permanent magnet material is a high and new technology recognized in the world and is a strategic material of top products of national defense, and the rare earth permanent magnet material is a first large application material and is widely applied to automobile communication, mobile phones, new energy automobiles, electric vehicles, wind power generation and the like.
The rare earth neodymium iron boron (sintered) permanent magnet material is manufactured, the consumption of neodymium accounts for 25-30%, but the utilization of rare earth resources is extremely unbalanced, the rare earth permanent magnet material (mainly sintered neodymium iron boron) mainly uses elements such as neodymium, praseodymium, dysprosium and terbium, the application of elements such as high-purity rare earth lanthanum and cerium with abundant reserves is less, and the rare earth ore contains various elements, so that the praseodymium and neodymium are widely applied, and a large amount of accumulation of lanthanum and cerium is caused.
The rare earth neodymium iron boron (sintered) permanent magnet material is manufactured, lanthanum is added, and cerium causes instability to magnetic performance and is greatly reduced.
Disclosure of Invention
The invention provides a high-cerium-content bauxite magnetic material and a smelting method thereof, and aims to solve the problems that the consumption of neodymium in the existing rare earth neodymium-iron-boron (sintered) permanent magnetic material accounts for 25-30%, but the utilization of rare earth resources is extremely unbalanced, so that a large amount of lanthanum and cerium are accumulated, and the magnetic performance is unstable and greatly reduced after lanthanum and cerium are added.
The invention adopts the following technical scheme: a high-cerium-content ferro-aluminum magnetic material is composed of the following raw materials in percentage by mass: proportioning before hydrogen crushing: 13% -16% of praseodymium-neodymium steel ingot, 6% -40% of cerium steel ingot and 45% -80% of waste block, wherein the waste block is a scrapped product of neodymium-iron-boron magnetic material equipment, and the content of praseodymium and neodymium is more than 30%.
The praseodymium-neodymium steel ingot is as follows: 30% of praseodymium-neodymium, 10% of gadolinium-iron, 1.05% of ferroboron, 0.8% of aluminum, 1.15% of copper, 0.6% of cobalt and 56.4% of iron.
In the praseodymium-neodymium steel ingot: 45% of praseodymium and neodymium, 5% of gadolinium and iron, 1.05% of boron, 0.8% of aluminum, 0.15% of copper and 0.6% of cobalt.
In the cerium steel ingot: 29.5 percent of cerium, 4 percent of gadolinium-iron, 1.05 percent of ferroboron, 0.8 percent of aluminum, 0.15 percent of copper and 0.6 percent of cobalt.
A method of smelting the high cerium content bauxite magnetic material of any one of claims 1 to 4, characterized by: the method comprises the following steps: batching, smelting, hydrogen crushing and jet milling powder, forming a magnetic field, and sintering and returning temperature, and the method comprises the following specific steps:
(1) preparing materials: accurately weighing praseodymium-neodymium steel ingots, cerium steel ingots and waste block raw materials in proportion, mixing the raw materials, and crushing the mixed raw materials in a coarse crusher;
(2) smelting: controlling the smelting vacuum degree in the smelting furnace to be less than or equal to 20Pa, the refining power to be 30-50KW, refining for 10min, the pouring temperature to be 1400-1440 ℃, and pouring for 3 min; after the pouring is finished, controlling the cooling crystallization time to be 40-50min, and controlling the pressure to be more than or equal to 0.1 MPa; after crystallization, the steel ingot discharged from the furnace is detected, no foreign matter exists in the steel ingot, and the fracture of the steel ingot is white; the volume fraction of the columnar crystal reaches more than 80 percent, and no serious oxide skin, wrinkles and bubbles exist;
(3) hydrogen crushing and jet milling: the dehydrogenation temperature of the hydrogen crushed powder is 500-600 ℃, the particle size of the hydrogen crushed powder is 0.01-0.5mm, the content of C is less than 150ppm, the content of O is less than 100ppm, and the content of N is less than 200 ppm; entering an air flow mill for milling: feeding when the oxygen content of the grinding gas is reduced to 0.00ppm, wherein the particle size of the ground powder of the jet mill is 3-5 mu m;
(4) magnetic field formation: isostatic pressing to manufacture a magnet: controlling the ambient temperature to<Humidity at 28 deg.C<50%，The magnetic field in the die is more than or equal to 1.4T, the pressure is more than or equal to 4Mpa, the exposure time of the prepressed blank in the air is less than or equal to 10 seconds, the isostatic pressure is more than or equal to 15Mpa, and the pressure of a high-pressure cavity is more than or equal to 150 Mpa; the density of the blank after isostatic pressing is more than or equal to 4.5g/cm3；
(5) Sintering and temperature returning, wherein the vacuum degree is controlled to be 2 × 10-3Pa, the pressure rise rate is less than or equal to 0.5Pa/Hr, the air extraction rate is less than or equal to 20min, the temperature uniformity is 1100 +/-3 ℃, and the sintering method specifically comprises the following steps: A. heating to 250 deg.C from normal temperature for 50min, maintaining the temperature at 250 deg.C for 2h, heating to 350 deg.C within 50min, maintaining the temperature for 2h, heating to 750 deg.C within 50min, maintaining the temperature at 750 deg.C for 6h, heating to 1050 deg.C within 30min, maintaining the temperature for 90min, heating to 1150 deg.C within 30min, maintaining the temperature for 4h, and air cooling to 80 deg.C; B. controlling the heating rate to be 80min, heating from 80 ℃ to 930 ℃, keeping the temperature for 4h, and then air-cooling to 80 ℃; C. controlling the heating rate to be from 80 ℃ to 550 ℃ within 80min, keeping the temperature for 4h, and then cooling from 550 ℃ to below 70 ℃ within 80min to obtain the high-cerium-content bauxite magnetic material.
The method for preparing the high-cerium-content bauxite magnetic material can be used for preparing the high-cerium-content bauxite magnetic material according to different proportions according to different magnetic performance requirements, so that the stability of the magnetic performance can be achieved, and the requirements of customers can be met. The grain boundary structure in the neodymium iron boron permanent magnet material obtained by the preparation method is continuous and uniform, and the magnetic isolation effect between adjacent grains is effectively enhanced, so that the coercive force of the neodymium iron boron permanent magnet material can be effectively improved, and the magnetic performance is excellent.
Detailed Description
Example 1: a high-cerium-content ferro-aluminum magnetic material is composed of the following raw materials in percentage by mass: proportioning before hydrogen crushing: 13% -16% of praseodymium-neodymium steel ingot, 6% -40% of cerium steel ingot and 45% -80% of waste block, wherein the waste block is a scrapped product of neodymium-iron-boron magnetic material equipment, and the content of praseodymium and neodymium is more than 30%.
The praseodymium-neodymium steel ingot is as follows: 30% of praseodymium-neodymium, 10% of gadolinium-iron, 1.05% of ferroboron, 0.8% of aluminum, 1.15% of copper, 0.6% of cobalt and 56.4% of iron. In the cerium steel ingot: 29.5 percent of cerium, 4 percent of gadolinium-iron, 1.05 percent of ferroboron, 0.8 percent of aluminum, 0.15 percent of copper and 0.6 percent of cobalt.
The method for smelting the ferro-aluminum magnetic material with high cerium content is characterized by comprising the following steps: the method comprises the following steps: batching, smelting, hydrogen crushing and jet milling powder, forming a magnetic field, and sintering and returning temperature, and the method comprises the following specific steps:
(1) preparing materials: accurately weighing praseodymium-neodymium steel ingots, cerium steel ingots and waste block raw materials in proportion, mixing the raw materials, and crushing the mixed raw materials in a coarse crusher;
(2) smelting: controlling the smelting vacuum degree in the smelting furnace to be less than or equal to 20Pa, the refining power to be 30-50KW, refining for 10min, the pouring temperature to be 1400-1440 ℃, and pouring for 3 min; after the pouring is finished, controlling the cooling crystallization time to be 40-50min, and controlling the pressure to be more than or equal to 0.1 MPa; after crystallization, the steel ingot discharged from the furnace is detected, no foreign matter exists in the steel ingot, and the fracture of the steel ingot is white; the volume fraction of the columnar crystal reaches more than 80 percent, and no serious oxide skin, wrinkles and bubbles exist;
(3) hydrogen crushing and jet milling: the dehydrogenation temperature of the hydrogen crushed powder is 500-600 ℃, the particle size of the hydrogen crushed powder is 0.01-0.5mm, the content of C is less than 150ppm, the content of O is less than 100ppm, and the content of N is less than 200 ppm; entering an air flow mill for milling: feeding when the oxygen content of the grinding gas is reduced to 0.00ppm, wherein the particle size of the ground powder of the jet mill is 3-5 mu m;
(4) magnetic field formation: isostatic pressing to manufacture a magnet: controlling the ambient temperature to<Humidity at 28 deg.C<50 percent, the magnetic field in the die is more than or equal to 1.4T, the pressure is more than or equal to 4Mpa, the exposure time of the prepressed blank in the air is less than or equal to 10 seconds, the isostatic pressure is more than or equal to 15MPa, and the pressure of a high-pressure cavity is more than or equal to 150 Mpa; the density of the blank after isostatic pressing is more than or equal to 4.5g/cm3；
(5) Sintering and temperature returning, wherein the vacuum degree is controlled to be 2 × 10-3Pa, the pressure rise rate is less than or equal to 0.5Pa/Hr, the air extraction rate is less than or equal to 20min, the temperature uniformity is 1100 +/-3 ℃, and the sintering method specifically comprises the following steps: A. heating to 250 deg.C from normal temperature for 50min, maintaining the temperature at 250 deg.C for 2h, heating to 350 deg.C within 50min, maintaining the temperature for 2h, heating to 750 deg.C within 50min, maintaining the temperature at 750 deg.C for 6h, heating to 1050 deg.C within 30min, maintaining the temperature for 90min, heating to 1150 deg.C within 30min, maintaining the temperature for 4h, and air cooling to 80 deg.C; B. controlling the heating rate to be 80min, heating from 80 ℃ to 930 ℃, keeping the temperature for 4h, and then air-cooling to 80 ℃; C. controlling the heating rate to be from 80 ℃ to 550 ℃ within 80min, keeping the temperature for 4h, and then cooling from 550 ℃ to below 70 ℃ within 80min to obtain the ferro-aluminum ore with high cerium contentA magnetic material.
Example 2: a high-cerium-content ferro-aluminum magnetic material is composed of the following raw materials in percentage by mass: proportioning before hydrogen crushing: 13% -16% of praseodymium-neodymium steel ingot, 6% -40% of cerium steel ingot and 45% -80% of waste block, wherein the waste block is a scrapped product of neodymium-iron-boron magnetic material equipment, and the content of praseodymium and neodymium is more than 30%. In the praseodymium-neodymium steel ingot: 45% of praseodymium and neodymium, 5% of gadolinium and iron, 1.05% of boron, 0.8% of aluminum, 0.15% of copper and 0.6% of cobalt. The preparation method is the same as that described in example 1.
Claims (4)
1. A method for smelting a magnetic material with high cerium content is characterized by comprising the following steps: the method comprises the following steps: the method comprises the following steps of material preparation, smelting, hydrogen crushing, jet milling, magnetic field forming, sintering and temperature return, and comprises the following specific steps:
(1) preparing materials: accurately weighing praseodymium-neodymium steel ingots, cerium steel ingots and waste block raw materials in proportion, mixing the raw materials, and crushing the mixed raw materials in a coarse crusher;
(2) smelting: controlling the smelting vacuum degree in the smelting furnace to be less than or equal to 20Pa, the refining power to be 30-50KW, refining for 10min, the pouring temperature to be 1400-1440 ℃, and pouring for 3 min; after the pouring is finished, controlling the cooling crystallization time to be 40-50min, and controlling the pressure to be more than or equal to 0.1 MPa; after crystallization, the steel ingot discharged from the furnace is detected, no foreign matter exists in the steel ingot, and the fracture of the steel ingot is white; the volume fraction of the columnar crystal reaches more than 80 percent, and no serious oxide skin, wrinkles and bubbles exist;
(3) hydrogen crushing and jet milling: the dehydrogenation temperature of the hydrogen crushed powder is 500-600 ℃, the particle size of the hydrogen crushed powder is 0.01-0.5mm, the content of C is less than 150ppm, the content of O is less than 100ppm, and the content of N is less than 200 ppm; entering an air flow mill for milling: feeding when the oxygen content of the grinding gas is reduced to 0.00ppm, wherein the particle size of the ground powder of the jet mill is 3-5 mu m;
(4) magnetic field forming: isostatic pressing to manufacture a magnet: controlling the ambient temperature to<Humidity at 28 deg.C<50 percent, the magnetic field in the die is more than or equal to 1.4T, the pressure is more than or equal to 4Mpa, the exposure time of the prepressed blank in the air is less than or equal to 10 seconds, the isostatic pressure is more than or equal to 15MPa, and the pressure of a high-pressure cavity is more than or equal to 150 Mpa; the density of the blank after isostatic pressing is more than or equal to 4.5g/cm3；
(5) Sintering and temperature returning, wherein the vacuum degree is controlled to be 2 × 10-3Pa, the pressure rise rate is less than or equal to 0.5PaHr, air extraction rate is less than or equal to 20min, temperature uniformity is 1100 +/-3 ℃, and the sintering method specifically comprises the following steps: A. heating to 250 deg.C from normal temperature for 50min, maintaining the temperature at 250 deg.C for 2h, heating to 350 deg.C within 50min, maintaining the temperature for 2h, heating to 750 deg.C within 50min, maintaining the temperature at 750 deg.C for 6h, heating to 1050 deg.C within 30min, maintaining the temperature for 90min, heating to 1150 deg.C within 30min, maintaining the temperature for 4h, and air cooling to 80 deg.C; B. controlling the heating rate to be 80min, heating from 80 ℃ to 930 ℃, keeping the temperature for 4h, and then air-cooling to 80 ℃; C. controlling the heating rate to be from 80 ℃ to 550 ℃ within 80min, keeping the temperature for 4h, and then cooling from 550 ℃ to below 70 ℃ within 80min to obtain the magnetic material with high cerium content;
the prepared magnetic material with high cerium content is prepared from the following raw materials in percentage by mass: proportioning before hydrogen crushing: 13% -16% of praseodymium-neodymium steel ingot, 6% -40% of cerium steel ingot and 45% -80% of waste block, wherein the waste block is a scrapped product of neodymium-iron-boron magnetic material equipment, and the content of praseodymium and neodymium is more than 30%.
2. The method of claim 1, wherein the step of melting the magnetic material with high cerium content comprises: the praseodymium-neodymium steel ingot is as follows: 30% of praseodymium-neodymium, 10% of gadolinium-iron, 1.05% of ferroboron, 0.8% of aluminum, 1.15% of copper, 0.6% of cobalt and 56.4% of iron.
3. The method of claim 1, wherein the step of melting the magnetic material with high cerium content comprises: in the praseodymium-neodymium steel ingot: 45% of praseodymium and neodymium, 5% of gadolinium and iron, 1.05% of boron, 0.8% of aluminum, 0.15% of copper and 0.6% of cobalt.
4. The method of claim 1, wherein the step of melting the magnetic material with high cerium content comprises: in the cerium steel ingot: 29.5 percent of cerium, 4 percent of gadolinium-iron, 1.05 percent of ferroboron, 0.8 percent of aluminum, 0.15 percent of copper and 0.6 percent of cobalt.
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| US3615914A (en) * | 1968-06-21 | 1971-10-26 | Gen Electric | Method of stabilizing permanent magnetic material powders |
| JP2002100524A (en) * | 2000-09-20 | 2002-04-05 | Daido Steel Co Ltd | METHOD OF MANUFACTURING HOT-PLASTIC WORKING ND-Fe-B MAGNET |
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