CN111644580A - Neodymium-iron-boron material, preparation method and application thereof - Google Patents

Neodymium-iron-boron material, preparation method and application thereof Download PDF

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Publication number
CN111644580A
CN111644580A CN202010611642.0A CN202010611642A CN111644580A CN 111644580 A CN111644580 A CN 111644580A CN 202010611642 A CN202010611642 A CN 202010611642A CN 111644580 A CN111644580 A CN 111644580A
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cooling
liquid
neodymium
iron
cooling roller
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黄杰华
李智翔
孔维峰
兰文辉
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Fujian Changting Jinlong Rare Earth Co Ltd
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Xiamen Tungsten Co Ltd
Fujian Changting Jinlong Rare Earth Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
    • B22D11/0611—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
    • B22D11/0637—Accessories therefor
    • B22D11/0665—Accessories therefor for treating the casting surfaces, e.g. calibrating, cleaning, dressing, preheating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
    • B22D11/0637—Accessories therefor
    • B22D11/068—Accessories therefor for cooling the cast product during its passage through the mould surfaces
    • B22D11/0682—Accessories therefor for cooling the cast product during its passage through the mould surfaces by cooling the casting wheel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/16—Controlling or regulating processes or operations
    • B22D11/18—Controlling or regulating processes or operations for pouring
    • 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
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • 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
    • 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
    • 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
    • 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
    • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets

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  • Crystallography & Structural Chemistry (AREA)
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  • Manufacturing & Machinery (AREA)
  • Hard Magnetic Materials (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Continuous Casting (AREA)

Abstract

The invention discloses a neodymium iron boron material, a preparation method and application thereof. The preparation method of the neodymium iron boron alloy sheet comprises the steps of pouring liquid alloy liquid on a ground cooling roller, and cooling the liquid alloy liquid to form the neodymium iron boron alloy sheet, wherein the rotating speed of the cooling roller is 27-32 r/min, and the temperature of cooling liquid in the cooling roller is-2-15 ℃; and an air pipe is arranged above the cooling roller, and the air pipe is used for performing air injection cooling on the cooling roller. The casting method of the neodymium iron boron alloy sheet provided by the invention can effectively improve the coercivity, and the prepared neodymium iron boron alloy sheet has excellent physical and chemical properties.

Description

Neodymium-iron-boron material, preparation method and application thereof
Technical Field
The invention relates to a neodymium iron boron material, a preparation method and application thereof.
Background
When the total RE content of the neodymium iron boron alloy sheet is less than 31.5%, the decrease of the coercive force can be reduced to a certain extent by the existing means, but in high-grade products, particularly products with RE less than or equal to 30.5%, the coercive force is easy to be lower by the existing process.
Chinese patent CN201610650925.X discloses a preparation method of a neodymium iron boron alloy sheet, wherein the alloy sheet with low oxygen content and good crystal form is obtained by controlling the water inlet temperature of a quenching roller to be 17-19 ℃ and then casting an alloy liquid and polishing the quenching roller in the casting stage. However, the method still causes low coercive force when preparing the neodymium iron boron alloy sheet with the total RE of less than 30.5%.
Chinese patent CN201710305563.5 also discloses a method for preparing neodymium iron ore alloy sheet, which shortens the processing period of neodymium iron ore alloy sheet and reduces the manufacturing cost by controlling the conditions of the water inlet temperature of the copper roller, the rotating speed of the cooling roller, etc. in the casting stage, but the decrease of coercive force cannot be completely avoided only by the above method in the neodymium iron ore alloy sheet with the total amount of rare earth RE less than 30.5%.
Therefore, it is an urgent problem to develop a casting process that can effectively improve the magnetic performance, especially when the total amount of rare earth RE is less than 30.5%.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defect of low magnetic property of the neodymium iron boron material in the prior art, and provides the neodymium iron boron material and the preparation method thereof.
The invention solves the technical problems by the following technical means:
the invention provides a preparation method of a neodymium iron boron alloy sheet, which comprises the following steps:
pouring liquid alloy liquid on a ground cooling roller, cooling the liquid alloy liquid to form the neodymium iron boron alloy sheet, wherein,
the rotating speed of the cooling roller is 27-32 r/min, and the temperature of the cooling liquid in the cooling roller is-2-15 ℃;
and an air pipe is arranged above the cooling roller, and the air pipe is used for performing air injection cooling on the cooling roller.
Further, the rotating speed of the cooling roller is (29 +/-0.2) r/min.
Further, the temperature of the cooling liquid is-2-12 ℃, for example, 5 ℃.
Further, the cooling liquid uses an antifreeze; ensure that the water is in a liquid state when the temperature of the water is lower than 0 ℃.
Further, the material of the cooling roller may be conventional in the art, and preferably, the material of the cooling roller is copper, such as red copper.
Further, the thickness of the cooling roll may be conventional in the art, and preferably, the thickness of the cooling roll is 50mm to 60 mm.
Further, the thickness of neodymium iron boron alloy piece can be for this field conventionality, and preferably, the thickness of neodymium iron boron alloy piece is 0.2 ~ 0.4 mm.
Further, the material of the grinding cooling roller is SiO2Particles, e.g. abrasive being SiO2Granulated sandpaper, such as brown corundum sandpaper; by using SiO2The stress is even when the granule is polished and is made the chill roll surface polish to make chill roll surface even polish, evenly cool off when the cooling, the cooling direction uniformity obtains improving.
Further, the air pipe is located 10mm above the copper roller.
Further, the number of the air pipes can be conventional in the art, and preferably, the number of the air pipes is 5-30.
Furthermore, 10-200 air holes aligned with the cooling roller are distributed on the air pipe; the cooling area is increased by using the air curtain generated by the gas flow in the air pipe.
Further, the angle between the opening position of the air pipe and the tangent line of the cooling roller is 70-100 degrees.
And further, during casting, the liquid alloy liquid is rolled on the cooling roller and the tundish through the tundish.
Further, the pressure of the gas jet can be conventional in the art, and preferably, the pressure of the gas jet is 0.5MPa to 0.6 MPa.
Further, the temperature of the gas jet can be conventional in the art, and preferably, the temperature of the gas jet is 0 ℃ to 25 ℃.
Further, the gas jet is an inert gas, such as one or more of helium, neon, argon, krypton, xenon, and radon, preferably argon.
Further, the casting temperature may be conventional in the art, preferably 1350 ℃ to 1480 ℃.
Further, the liquid alloy liquid may be prepared by methods conventional in the art, and generally includes the steps of: charging, vacuumizing, filling argon, melting, refining, standing and cooling.
Wherein the charging may be conventional in the art, for example, charging the feedstock into a crucible, holding the crucible in a furnace, and closing the furnace door.
Wherein the raw materials can be conventional in the field, such as 29.5% PrNd, 0.5% Al, 0.2% Cu, 1.5% Co, 0.2% Zr, 0.25% Ga, 0.95% B, and the balance of pure iron; or 29.8% PrNd, 0.5% Al, 0.2% Cu, 1% Co, 0.2% Zr, 0.25% Ga, 0.1% Ti, 0.98% B, and the balance pure iron.
The vacuumizing can be conventional in the field, for example, the furnace is vacuumized, after the vacuum degree reaches 15-18 Pa, the raw materials are heated and continuously vacuumized to 8-9 Pa on the premise that the raw materials are not heated to be red.
Wherein, the argon filling can be conventional in the field, for example, high-purity argon with the purity of more than or equal to 99.99 percent is filled into the furnace, and the argon filling is stopped after the gas pressure in the furnace reaches 50 kPa.
Wherein the melting may be conventional in the art, such as by induction heating to melt all of the solid raw materials into a liquid state.
Wherein the refining can be conventional in the field, for example, the liquid metals are fully mixed and reacted by continuously heating and electromagnetically stirring, and the temperature of the alloy liquid is raised to 1450-1500 ℃.
Wherein the waiting time can be conventional in the field, for example, the alloy liquid is kept at 1450-1500 ℃ for 3-5 minutes by adjusting the heating power to be proper.
Wherein the temperature reduction can be that the alloy liquid is naturally cooled to 1430-1460 ℃.
The invention also provides a neodymium iron boron alloy sheet which is prepared by the preparation method.
The invention also provides a preparation method of the neodymium iron boron material, which comprises the following steps:
the neodymium iron boron alloy sheet obtained by the casting method is prepared by milling, molding, sintering and aging.
The operation and conditions of the powder preparation can be conventional powder preparation process in the field, and generally comprise hydrogen powder preparation and/or airflow powder preparation.
Wherein, the hydrogen crushing powder generally comprises hydrogen absorption, dehydrogenation and cooling treatment. The temperature of the hydrogen absorption is generally 20-200 ℃. The dehydrogenation temperature is generally 400-650 ℃. The pressure of the hydrogen absorption is generally 50 to 600 kPa.
Wherein the jet milling powder is generally carried out under the condition of 0.1-2 MPa, preferably 0.5-0.7 MPa (such as 0.65 MPa). The gas flow in the gas flow milled powder can be, for example, nitrogen and/or argon. The efficiency of the airflow milling powder can be different according to different equipment, and for example, the efficiency can be 30-400 kg/h, and preferably 200 kg/h.
The molding operation and conditions may be those conventional in the art. Such as magnetic field molding. The magnetic field intensity of the magnetic field forming method is generally 1.5T or more.
Wherein the operation of sinteringThe sintering start phase may be at a vacuum level of less than 5 × 10 when an inert atmosphere sintering process is used-1Pa, and the like. The inert atmosphere may be an atmosphere containing an inert gas as is conventional in the art, such as helium, argon.
Wherein, the sintering temperature can be 1000-1200 ℃, preferably 1030-1090 ℃.
Wherein, the sintering time can be 0.5-10 h, preferably 2-8 h.
The operation and conditions of the aging treatment can be the conventional aging treatment process in the field, and after sintering is finished, a fan is started to reduce the temperature of the alloy sheet to 30-40 ℃.
The invention also provides the neodymium iron boron material prepared by the preparation method.
The invention also provides an application of the neodymium iron boron material as an electronic component.
The pressure referred to in the present invention is generally an absolute pressure.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
Compared with the prior art, the invention has the following implementation effects:
adopt control cooling liquid temperature, reduce the chill roll rotational speed, set up the trachea in the chill roll top and carry out the primary cooling ability that jet-propelled cooling can improve the alloy piece, the fine granularity of fine piece crystalline neodymium iron boron alloy tissue simultaneous control is obtained to control and the super-cooled rate of casting, prevents crystalline granularity undersize, can increase the cooling area effectively, promotes the cooling effect, control thin slice thickness distribution and thickness concentration. Furthermore, the cooling roller can be polished to keep the surface of the cooling roller smooth, so that the heat conductivity is improved, and the grain growth directions of the alloy sheets are consistent to ensure that the cooling directions are consistent. The alloy sheet prepared by the invention has high coercive force, greatly improved squareness and excellent physical and chemical properties.
The preparation method provided by the invention can be used for repeatedly preparing the thin strip alloy sheet, has strong process stability and can be used for large-scale production.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
In the following examples,% represents the weight percentage of each element in the raw material of the ndfeb alloy sheet.
In the following examples, the equipment used for the oxynitrilic hydrogen analysis was: saimer Feishale (China) science and technology, model EMGA-830; the equipment used for carbon content analysis is as follows: shanghai Baoying science and technology, model CS-206.
In the following examples, the apparatus used for magnetic performance was a PFM pulsed magnetic field magnetometer.
Example 1
(1) Charging raw materials (29.8% of praseodymium and neodymium in percentage) comprising 29.8% of PrNd, 0.5% of Al, 0.2% of Cu, 1% of Co, 0.2% of Zr, 0.25% of Ga, 0.1% of Ti, 0.98% of B and the balance of pure iron are put into a crucible.
(2) And (3) vacuumizing, namely vacuumizing the furnace to ensure that the vacuum degree reaches 15-18 Pa, heating and continuously vacuumizing to 8-9 Pa on the premise of not heating the raw materials to be reddened.
(3) And (4) oxygenation, namely, high-purity oxygen with the purity of less than or equal to 99.99 percent is filled into the furnace, and the oxygenation is stopped after the gas pressure in the furnace reaches 50 kPa.
(4) And (3) melting, namely melting all the solid raw materials into liquid by induction heating.
(5) Refining, namely, continuously heating and fully mixing liquid metals by electromagnetic stirring to react, and heating the alloy liquid to 1500 ℃.
(6) And (5) standing, namely adjusting to a proper heating power, and keeping the temperature of the alloy liquid at 1500 ℃ for 3-5 minutes.
(7) And (5) cooling, namely closing the heating power for 0-2 minutes, and naturally cooling the alloy liquid to 1450 ℃.
(8) Casting: in the casting process, chilled water is introduced into a copper roller, the temperature of inlet water is controlled to be 5 ℃, meanwhile, argon gas with the temperature of 9 ℃ is introduced into a high-temperature-resistant air pipe arranged above the copper roller, the gas pressure is controlled to be 0.5Mpa, the copper roller is polished by using abrasive paper before casting, the cooling capacity of the copper roller is improved, alloy liquid is poured out from an inclined crucible, the alloy liquid passes through a prefabricated tundish and is poured onto the surface of a rotating quenching roller, the rotating speed of the quenching roller is 29r/min, the alloy liquid is thrown out under the action of centrifugal force, the thickness of a formed neodymium iron boron alloy sheet is 0.28mm, and the alloy liquid falls on a material receiving disc.
(9) And collecting the cast neodymium iron boron alloy sheet in a recovery container, cooling to 30-40 ℃, and discharging.
(10) The alloy sheet produced by the method is vacuumized at room temperature in a hydrogen breaking furnace in which a quenching alloy is placed, hydrogen with the purity of 99.9% is introduced into the hydrogen breaking furnace, the pressure of the hydrogen is maintained at 160kPa, after the hydrogen is fully absorbed, the temperature is raised while the vacuum is pumped, the hydrogen is fully dehydrogenated, then the hydrogen is cooled, and the powder after the hydrogen breaking and crushing is taken out. Wherein the temperature for hydrogen absorption is room temperature, and the temperature for dehydrogenation is 550 ℃.
(11) And (3) carrying out jet milling on the powder subjected to hydrogen crushing and crushing in the atmosphere of nitrogen under the condition that the pressure of a crushing chamber is 0.65Mpa to obtain fine powder with the granularity of 3.9-4.0 microns.
(12) And (3) sintering: and conveying each formed body to a sintering furnace for sintering, and sintering at 1030-1090 ℃ for 2-8 h under vacuum of less than 0.5Pa to obtain a sintered body.
(13) Aging treatment: and after sintering, starting the fan to reduce the temperature of the neodymium iron boron material to 30 ℃ to obtain the neodymium iron boron permanent magnet material.
The magnetic performance and the composition of the neodymium iron boron material are tested, and Br is 14.0KGs, Hcj is 17.64KOe, and Hk/Hcj is 98.8%; the carbon content is 460ug/g and the nitrogen content is 218 ug/g.
Comparative example 1
The comparative example is different from example 1 only in that no chilled water is introduced during the casting process, the water inlet temperature is 25 ℃, no gas is introduced above the copper roller to reduce the temperature, the rotation speed of the copper roller is 31rpm, and the rest of the operations are the same as example 1, wherein the measured Br of the neodymium iron boron material obtained in step (13) is 14.0KGs, and the Hcj is 16.43 Koe. Compared with the performance of the neodymium iron boron material produced in the comparative example 1, Br of the neodymium iron boron material produced in the example 1 is unchanged, and Hcj of the neodymium iron boron material produced in the example 1 is improved by 1.03%.
Example 2
(1) Charging raw materials (29.5% of praseodymium and neodymium) comprising 29.5% of PrNd, 0.5% of Al, 0.2% of Cu, 1.5% of Co, 0.2% of Zr, 0.25% of Ga, 0.95% of B and the balance of pure iron were charged into a crucible.
(2) And (3) vacuumizing, namely vacuumizing the furnace to ensure that the vacuum degree reaches 15-18 Pa, heating and continuously vacuumizing to 8-9 Pa on the premise of not heating the raw materials to be reddened.
(3) And (4) oxygenation, namely, high-purity oxygen with the purity of less than or equal to 99.99 percent is filled into the furnace, and the oxygenation is stopped after the gas pressure in the furnace reaches 50 kPa.
(4) And (3) melting, namely melting all the solid raw materials into liquid by induction heating.
(5) Refining, namely, continuously heating and fully mixing liquid metals by electromagnetic stirring to react, and heating the alloy liquid to 1500 ℃.
(6) And (5) standing, namely adjusting to a proper heating power, and keeping the temperature of the alloy liquid at 1500 ℃ for 3-5 minutes.
(7) And (5) cooling, namely closing the heating power for 0-2 minutes, and naturally cooling the alloy liquid to 1450 ℃.
(8) Casting: in the casting process, chilled water is introduced into a copper roller, the water inlet temperature is controlled to be minus 2 ℃, meanwhile, argon gas with the temperature of 0 ℃ is introduced into a high-temperature-resistant air pipe arranged above the copper roller, the gas pressure is controlled to be 0.6Mpa, the copper roller is polished by using abrasive paper before casting, the cooling capacity of the copper roller is improved, alloy liquid is poured out from an inclined crucible, the alloy liquid passes through a prefabricated tundish and is poured onto the surface of a rotating quenching roller, the rotating speed of the quenching roller is 29r/min, the alloy liquid is thrown out under the action of centrifugal force, the thickness of a formed neodymium iron boron alloy sheet is 0.28mm, and the formed neodymium iron boron alloy sheet falls on a material.
(9) And collecting the cast neodymium iron boron alloy sheet in a recovery container, cooling to 30-40 ℃, and discharging.
(10) The alloy sheet produced by the method is vacuumized at room temperature in a hydrogen breaking furnace in which a quenching alloy is placed, hydrogen with the purity of 99.9% is introduced into the hydrogen breaking furnace, the pressure of the hydrogen is maintained at 160kPa, after the hydrogen is fully absorbed, the temperature is raised while the vacuum is pumped, the hydrogen is fully dehydrogenated, then the hydrogen is cooled, and the powder after the hydrogen breaking and crushing is taken out. Wherein the temperature for hydrogen absorption is room temperature, and the temperature for dehydrogenation is 550 ℃.
(11) And (3) carrying out jet milling on the powder subjected to hydrogen crushing and crushing in the atmosphere of nitrogen under the condition that the pressure of a crushing chamber is 0.65Mpa to obtain fine powder with the granularity of 3.9-4.0 microns.
(12) And (3) sintering: and conveying each formed body to a sintering furnace for sintering, and sintering at 1030-1090 ℃ for 2-8 h under vacuum of less than 0.5Pa to obtain a sintered body.
(13) Aging treatment: and after sintering, starting the fan to reduce the temperature of the neodymium iron boron material to 30 ℃ to obtain the neodymium iron boron permanent magnet material.
The magnetic performance and the composition of the neodymium iron boron material are tested, and the Br is 14.38KGs, the Hcj is 17.47KOe, and the Hk/Hcj is 98%; the carbon content is 593ug/g, and the nitrogen content is 333 ug/g.
Comparative example 2
The comparative example is different from example 2 only in that no chilled water is introduced during the casting process, the water inlet temperature is 25 ℃, no gas is introduced above the copper roller to reduce the temperature, the rotation speed of the copper roller is 31rpm, and the rest of the operations are the same as example 2, wherein the measured Br of the neodymium iron boron material obtained in step (13) is 14.39KGs, and the Hcj is 17.25 Koe. Compared with the performance of the neodymium iron boron alloy material produced in the comparative example 2, Br is almost unchanged, and Hcj of the neodymium iron boron material produced in the example 2 is improved by 1.27%.
Example 3
(1) Charging raw materials (29.5% of praseodymium and neodymium) comprising 29.5% of PrNd, 0.5% of Al, 0.2% of Cu, 1.5% of Co, 0.2% of Zr, 0.25% of Ga, 0.95% of B and the balance of pure iron were charged into a crucible.
(2) And (3) vacuumizing, namely vacuumizing the furnace to ensure that the vacuum degree reaches 15-18 Pa, heating and continuously vacuumizing to 8-9 Pa on the premise of not heating the raw materials to be reddened.
(3) And (4) oxygenation, namely, high-purity oxygen with the purity of less than or equal to 99.99 percent is filled into the furnace, and the oxygenation is stopped after the gas pressure in the furnace reaches 50 kPa.
(4) And (3) melting, namely melting all the solid raw materials into liquid by induction heating.
(5) Refining, namely, continuously heating and fully mixing liquid metals by electromagnetic stirring to react, and heating the alloy liquid to 1500 ℃.
(6) And (5) standing, namely adjusting to a proper heating power, and keeping the temperature of the alloy liquid at 1500 ℃ for 3-5 minutes.
(7) And (5) cooling, namely closing the heating power for 0-2 minutes, and naturally cooling the alloy liquid to 1450 ℃.
(8) Casting: the method comprises the steps of introducing chilled water into a copper roller in the casting process, controlling the water inlet temperature to be 15 ℃, introducing argon gas at the temperature of 25 ℃ into a high-temperature-resistant air pipe arranged above the copper roller, controlling the gas pressure to be 0.6Mpa, polishing the copper roller by using abrasive paper before casting, increasing the cooling capacity of the copper roller, inclining a crucible, pouring alloy liquid out, enabling the alloy liquid to pass through a prefabricated tundish, pouring the alloy liquid onto the surface of a rotating quenching roller, enabling the rotating speed of the quenching roller to be 29r/min, throwing the alloy liquid out under the action of centrifugal force to form neodymium iron boron alloy sheets with the thickness of 0.2-0.4 mm, and enabling the alloy sheets to fall on a material receiving.
(9) And collecting the cast neodymium iron boron alloy sheet in a recovery container, cooling to 30-40 ℃, and discharging.
(10) The alloy sheet produced by the method is vacuumized at room temperature in a hydrogen breaking furnace in which a quenching alloy is placed, hydrogen with the purity of 99.9% is introduced into the hydrogen breaking furnace, the pressure of the hydrogen is maintained at 160kPa, after the hydrogen is fully absorbed, the temperature is raised while the vacuum is pumped, the hydrogen is fully dehydrogenated, then the hydrogen is cooled, and the powder after the hydrogen breaking and crushing is taken out. Wherein the temperature for hydrogen absorption is room temperature, and the temperature for dehydrogenation is 550 ℃.
(11) And (3) carrying out jet milling on the powder subjected to hydrogen crushing and crushing in the atmosphere of nitrogen under the condition that the pressure of a crushing chamber is 0.65Mpa to obtain fine powder with the granularity of 3.9-4.0 microns.
(12) And (3) sintering: and conveying each formed body to a sintering furnace for sintering, and sintering at 1030-1090 ℃ for 2-8 h under vacuum of less than 0.5Pa to obtain a sintered body.
(13) Aging treatment: and after sintering, starting the fan to reduce the temperature of the neodymium iron boron material to 30 ℃ to obtain the neodymium iron boron permanent magnet material.
The magnetic performance and the composition of the neodymium iron boron material are tested, and Br is 14.38KGs, Hcj is 17.396KOe, and Hk/Hcj is 98%; the carbon content is 593ug/g, and the nitrogen content is 333 ug/g.
Comparative example 3
(1) Charging raw materials (29.5% of praseodymium and neodymium) comprising 29.5% of PrNd, 0.5% of Al, 0.2% of Cu, 1.5% of Co, 0.2% of Zr, 0.25% of Ga, 0.95% of B and the balance of pure iron were charged into a crucible.
(2) And (3) vacuumizing, namely vacuumizing the furnace to ensure that the vacuum degree reaches 15-18 Pa, heating and continuously vacuumizing to 8-9 Pa on the premise of not heating the raw materials to be reddened.
(3) And (4) oxygenation, namely, high-purity oxygen with the purity of less than or equal to 99.99 percent is filled into the furnace, and the oxygenation is stopped after the gas pressure in the furnace reaches 50 kPa.
(4) And (3) melting, namely melting all the solid raw materials into liquid by induction heating.
(5) Refining, namely, continuously heating and fully mixing liquid metals by electromagnetic stirring to react, and heating the alloy liquid to 1500 ℃.
(6) And (5) standing, namely adjusting to a proper heating power, and keeping the temperature of the alloy liquid at 1500 ℃ for 3-5 minutes.
(7) And (5) cooling, namely closing the heating power for 0-2 minutes, and naturally cooling the alloy liquid to 1450 ℃.
(8) Casting: in the casting process, chilled water is introduced into a copper roller, the temperature of inlet water is controlled to be 25 ℃, meanwhile, argon gas with the temperature of 25 ℃ is introduced into a high-temperature-resistant air pipe arranged above the copper roller, the gas pressure is controlled to be 0.6Mpa, the copper roller is polished by using abrasive paper before casting, the cooling capacity of the copper roller is improved, alloy liquid is poured out from an inclined crucible, the alloy liquid passes through a prefabricated tundish and is poured onto the surface of a rotating quenching roller, the rotating speed of the quenching roller is 29r/min, the alloy liquid is thrown out under the action of centrifugal force, the thickness of a formed neodymium iron boron alloy sheet is 0.2-0.4 mm, and the formed neodymium iron boron alloy sheet falls on.
(9) And collecting the cast neodymium iron boron alloy sheet in a recovery container, cooling to 30-40 ℃, and discharging.
(10) The alloy sheet produced by the method is vacuumized at room temperature in a hydrogen breaking furnace in which a quenching alloy is placed, hydrogen with the purity of 99.9% is introduced into the hydrogen breaking furnace, the pressure of the hydrogen is maintained at 160kPa, after the hydrogen is fully absorbed, the temperature is raised while the vacuum is pumped, the hydrogen is fully dehydrogenated, then the hydrogen is cooled, and the powder after the hydrogen breaking and crushing is taken out. Wherein the temperature for hydrogen absorption is room temperature, and the temperature for dehydrogenation is 550 ℃.
(11) And (3) carrying out jet milling on the powder subjected to hydrogen crushing and crushing in the atmosphere of nitrogen under the condition that the pressure of a crushing chamber is 0.65Mpa to obtain fine powder with the granularity of 3.9-4.0 microns.
(12) And (3) sintering: and conveying each formed body to a sintering furnace for sintering, and sintering at 1030-1090 ℃ for 2-8 h under vacuum of less than 0.5Pa to obtain a sintered body.
(13) Aging treatment: and after sintering, starting the fan to reduce the temperature of the neodymium iron boron material to 30 ℃ to obtain the neodymium iron boron permanent magnet material.
The magnetic performance and the composition of the neodymium iron boron material are tested, and Br is 14.376KGs, Hcj is 17.25KOe, and Hk/Hcj is 98%; the carbon content is 654ug/g, and the nitrogen content is 246 ug/g. Comparative example 3 is a comparative term to example 3. The performance of the alloy sheet produced by the embodiment 3 is almost unchanged compared with that of the alloy sheet produced by the comparative example 3, and the Hcj of the neodymium-iron-boron material produced by the embodiment 3 is improved by 0.84%.
Comparative example 4
(1) Charging raw materials (29.5% of praseodymium and neodymium) comprising 29.5% of PrNd, 0.5% of Al, 0.2% of Cu, 1.5% of Co, 0.2% of Zr, 0.25% of Ga, 0.95% of B and the balance of pure iron were charged into a crucible.
(2) And (3) vacuumizing, namely vacuumizing the furnace to ensure that the vacuum degree reaches 15-18 Pa, heating and continuously vacuumizing to 8-9 Pa on the premise of not heating the raw materials to be reddened.
(3) And (4) oxygenation, namely, high-purity oxygen with the purity of less than or equal to 99.99 percent is filled into the furnace, and the oxygenation is stopped after the gas pressure in the furnace reaches 50 kPa.
(4) And (3) melting, namely melting all the solid raw materials into liquid by induction heating.
(5) Refining, namely, continuously heating and fully mixing liquid metals by electromagnetic stirring to react, and heating the alloy liquid to 1500 ℃.
(6) And (5) standing, namely adjusting to a proper heating power, and keeping the temperature of the alloy liquid at 1500 ℃ for 3-5 minutes.
(7) And (5) cooling, namely closing the heating power for 0-2 minutes, and naturally cooling the alloy liquid to 1450 ℃.
(8) Casting: and (3) introducing chilled water into the copper roller in the casting process, controlling the water inlet temperature to be 25 ℃, polishing the copper roller by using abrasive paper before casting, increasing the cooling capacity of the copper roller, inclining the crucible to pour out the alloy liquid, enabling the alloy liquid to pass through a prefabricated tundish and be poured onto the surface of a rotating quenching roller, wherein the rotating speed of the quenching roller is 29r/min, throwing out the alloy liquid under the action of centrifugal force to form neodymium iron boron alloy sheets with the thickness of 0.2-0.4 mm, and dropping the neodymium iron boron alloy sheets on a material receiving disc.
(9) And collecting the cast neodymium iron boron alloy sheet in a recovery container, cooling to 30-40 ℃, and discharging.
(10) The alloy sheet produced by the method is vacuumized at room temperature in a hydrogen breaking furnace in which a quenching alloy is placed, hydrogen with the purity of 99.9% is introduced into the hydrogen breaking furnace, the pressure of the hydrogen is maintained at 160kPa, after the hydrogen is fully absorbed, the temperature is raised while the vacuum is pumped, the hydrogen is fully dehydrogenated, then the hydrogen is cooled, and the powder after the hydrogen breaking and crushing is taken out. Wherein the temperature for hydrogen absorption is room temperature, and the temperature for dehydrogenation is 550 ℃.
(11) And (3) carrying out jet milling on the powder subjected to hydrogen crushing and crushing in the atmosphere of nitrogen under the condition that the pressure of a crushing chamber is 0.65Mpa to obtain fine powder with the granularity of 3.9-4.0 microns.
(12) And (3) sintering: and conveying each formed body to a sintering furnace for sintering, and sintering at 1030-1090 ℃ for 2-8 h under vacuum of less than 0.5Pa to obtain a sintered body.
(13) Aging treatment: and after sintering, starting the fan to reduce the temperature of the neodymium iron boron material to 30 ℃ to obtain the neodymium iron boron permanent magnet material.
The magnetic performance and the composition of the neodymium iron boron material are tested, and Br is 14.363KGs, Hcj is 17.21KOe, and Hk/Hcj is 96%; the carbon content was 603ug/g and the nitrogen content was 252 ug/g.

Claims (10)

1. The preparation method of the neodymium iron boron alloy sheet is characterized by comprising the following steps:
pouring liquid alloy liquid on a ground cooling roller, cooling the liquid alloy liquid to form the neodymium iron boron alloy sheet, wherein,
the rotating speed of the cooling roller is 27-32 r/min, and the temperature of the cooling liquid in the cooling roller is-2-15 ℃;
and an air pipe is arranged above the cooling roller, and the air pipe is used for performing air injection cooling on the cooling roller.
2. The method for preparing the neodymium-iron-boron alloy sheet according to claim 1, wherein the rotating speed of the cooling roller is (29 ± 0.2) r/min.
3. The method for preparing the neodymium-iron-boron alloy sheet according to claim 1, wherein the temperature of the cooling liquid is-2 to 12 ℃, for example, 5 ℃.
4. The method for preparing the neodymium-iron-boron alloy sheet according to claim 1, wherein the grinding and cooling roller is made of SiO2And (3) granules.
5. The method for preparing the neodymium-iron-boron alloy sheet according to any one of claims 1 to 4, wherein the cooling liquid is an anti-freezing liquid;
and/or the material of the cooling roller is copper;
and/or the thickness of the cooling roller is 50 mm-60 mm;
and/or the air pipe is positioned 10mm above the copper roller;
and/or the number of the air pipes is 5-30;
and/or 10-200 air holes aligned with the cooling roller are distributed on the air pipe;
and/or the angle between the opening position of the air pipe and the tangent line of the cooling roller is 70-100 degrees;
and/or the liquid alloy liquid is rolled on the cooling roller and the tundish through the tundish;
and/or the gas pressure of the gas injection is 0.5MPa to 0.6 MPa;
and/or the gas injection gas is an inert gas; for example, one or more of helium, neon, argon, krypton, xenon, and radon, again for example argon;
and/or the temperature of the gas for gas injection is 0-25 ℃;
and/or the temperature of the liquid alloy is 1350-1480 ℃;
and/or, the preparation method also comprises the following steps: charging, vacuumizing, filling argon, melting, refining, standing and cooling to obtain the liquid alloy liquid.
6. The method for preparing the neodymium-iron-boron alloy sheet according to claim 5, wherein the method further comprises the following steps: loading, vacuumizing, filling argon, melting, refining, standing and cooling, wherein the raw materials of the loading are 29.5% of PrNd, 0.5% of Al, 0.2% of Cu, 1.5% of Co, 0.2% of Zr, 0.25% of Ga, 0.95% of B and the balance of pure iron; or 29.8% PrNd, 0.5% Al, 0.2% Cu, 1% Co, 0.2% Zr, 0.25% Ga, 0.1% Ti, 0.98% B, and the balance pure iron;
and/or the material of the cooling roller is red copper;
and/or the grinding material for grinding the cooling roller is brown corundum abrasive paper;
and/or the vacuum degree of the vacuumizing is 8-9 Pa;
and/or the refining temperature is 1450-1500 ℃;
and/or the waiting time is 3-5 minutes.
7. A neodymium iron boron alloy sheet, which is prepared according to the preparation method of the neodymium iron boron alloy sheet as claimed in any one of claims 1 to 6.
8. The preparation method of the neodymium iron boron permanent magnet material is characterized by comprising the following steps:
the neodymium-iron-boron permanent magnet material is prepared by carrying out powder making, molding, sintering treatment and aging treatment on the neodymium-iron-boron alloy sheet according to claim 7.
9. A neodymium iron boron permanent magnet material prepared according to the preparation method of the neodymium iron boron permanent magnet material as claimed in claim 8.
10. Use of a neodymium-iron-boron permanent magnetic material according to claim 9 as an electronic component.
CN202010611642.0A 2020-06-29 2020-06-29 Neodymium-iron-boron material, preparation method and application thereof Pending CN111644580A (en)

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