CN109473247B - Preparation method of neodymium iron boron grain boundary infiltration alloy cast sheet - Google Patents
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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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- 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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- 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
- H01F41/0293—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 diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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Abstract
A preparation method of a neodymium iron boron grain boundary infiltration alloy cast sheet comprises the following steps: (1) vacuum smelting: adding the neodymium iron boron alloy distribution raw materials into a crucible of a vacuum smelting furnace in sequence for smelting; (2) casting: pouring the alloy solution in the crucible above a casting roller, and forming an alloy casting sheet after passing through the casting roller; (3) vacuum sputtering: carrying out vacuum sputtering coating on the alloy casting sheet; (4) cooling and discharging: after vacuum sputtering coating, the alloy cast sheet enters a water cooling device for cooling, and is discharged from the furnace after cooling; (5) vacuum heat treatment: and carrying out heat treatment twice on the alloy cast sheet after the alloy cast sheet is taken out of the furnace. The invention carries out vacuum sputtering coating on the uncooled alloy casting sheet, forms a heavy rare earth sputtering film on the side surface, carries out heat treatment after cooling, and leads the heavy rare earth to permeate into the alloy casting sheet, the permeation effect of the heavy rare earth is good, the use amount of the heavy rare earth can be reduced by 20-30%, the utilization rate of heavy rare earth elements is improved, and the production cost is greatly reduced.
Description
Technical Field
The invention relates to a preparation method of a neodymium iron boron grain boundary infiltration alloy casting sheet.
Background
Neodymium iron boron as rare earth permanent magnetic material has the advantages of high cost performance, small volume, light weight, good mechanical property and strong magnetism, has extremely high magnetic energy and coercive force, is known as Magen in the magnetic field, is widely applied to the fields of electronics, electric machinery, medical appliances, toys, packaging, hardware machinery, aerospace and the like, and is more commonly used as a permanent magnet motor, a loudspeaker, a magnetic separator, a computer disk driver, a magnetic resonance imaging device instrument and the like.
The coercive force characteristic of the sintered neodymium iron boron is mainly realized by heavy rare earth elements dysprosium and terbium in the distribution, and researches find that the heavy rare earth elements are distributed in a neodymium-rich phase, the generated coercive force improving effect is very obvious, and the heavy rare earth elements are remained in a main phase and have little effect of improving the coercive force. If the heavy rare earth elements are directly added in the smelting stage, a large part of the heavy rare earth elements enter the main phase, and the distribution cost is increased. At present, dysprosium and terbium elements enter a neodymium-rich phase by using a heavy rare earth permeation technology in the industry, so that the use amount of the heavy rare earth elements is reduced, but the coercive force is improved.
At present, the main coating methods of penetrant are: 1. coating by adopting a powder penetrating agent which is composed of dysprosium oxide, dysprosium fluoride, terbium oxide, terbium fluoride and related mixed powder and an organic solvent, wherein the mode has the defects of large waste and nonuniform coating; 2. the mode of vacuum coating is adopted, and penetrant (in a metal state) is sputtered onto the neodymium iron boron black sheet to be permeated in a vacuum mode, so that the mode has high requirement on equipment, the use cost is high, the thickness of the black sheet is required to be within 2-10 mm, and the permeation purpose of an over-thick product cannot be achieved.
The rare earth is a general name of seventeen metal elements including lanthanide elements, scandium and yttrium in a chemical periodic table, and is divided into light rare earth and heavy rare earth, the light rare earth is cheap relative to the heavy rare earth, and terbium and dysprosium are used in vacuum coating of the neodymium iron boron magnet, and the two heavy rare earths are higher in price, so that the more the heavy rare earth is used, the higher the coating cost of the neodymium iron boron magnet is, the existing coating mode of grain boundary permeation can reduce the use amount of the heavy rare earth by 2% -8% compared with the common coating mode, but the cost is higher. Therefore, the method for reducing the use amount of heavy rare earth and improving the performance when sintering neodymium iron boron is a subject which needs to be overcome urgently in the magnetic material industry at present.
Disclosure of Invention
The invention overcomes the defects and provides the preparation method of the neodymium iron boron grain boundary infiltration alloy cast sheet, which greatly improves the utilization rate of heavy rare earth elements, reduces the use amount of heavy rare earth, and has good infiltration effect and high production efficiency.
The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the neodymium iron boron grain boundary infiltration alloy cast sheet comprises the following steps:
(1) vacuum smelting: adding the neodymium iron boron alloy distribution raw materials into a crucible of a vacuum smelting furnace in sequence for smelting;
(2) casting: pouring the alloy melt in the crucible above a casting roller after the temperature of the melted alloy reaches 1450-1500 ℃, and forming an alloy casting sheet after the alloy melt passes through the casting roller;
(3) vacuum sputtering: the alloy cast sheet falling from the casting roll passes through a vacuum sputtering device, and the vacuum sputtering device carries out vacuum sputtering coating operation on the alloy cast sheet;
(4) cooling and discharging: after the vacuum sputtering coating operation, cooling the alloy cast sheet in a water cooling device, and discharging the alloy cast sheet after cooling to 20-60 ℃;
(5) vacuum heat treatment: placing the alloy cast sheet discharged from the furnace into a heat treatment furnace for carrying out heat treatment twice; the first heat treatment process comprises the following steps: vacuum degree of 10-5～10-3Pa, the treatment temperature is 750-920 ℃, the heat preservation time is 5-7 h, and the temperature is cooled to be below 100 ℃; the second heat treatment process comprises the following steps: vacuum degree of 10-2～10-1Pa, the treatment temperature is 480-520 ℃, the heat preservation time is 4-5 h, and the temperature is cooled to the room temperature.
Wherein, the vacuum sputtering device is arranged below the casting roller and above the water cooling device.
Wherein, in the step (3), the time of vacuum sputtering is 9-12 minutes.
Wherein, in the step (3), the thickness of the vacuum sputtering coating is 0.02-0.2 mm.
Compared with the prior art, the invention carries out vacuum sputtering coating operation after casting the alloy casting piece and before cooling, so that a layer of heavy rare earth sputtering film is formed on the side surface of the uncooled alloy casting piece, and then the heavy rare earth is subjected to heat treatment after cooling, so that the heavy rare earth is infiltrated into the alloy casting piece, the infiltration effect of the heavy rare earth is good, the use amount of the heavy rare earth can be reduced by 20-30%, the utilization rate of heavy rare earth elements is improved, the production cost is greatly reduced, and the invention can be popularized and applied in a large scale.
Drawings
FIG. 1 is a process flow diagram of the preparation method of the NdFeB grain boundary infiltration alloy casting sheet of the invention.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Example 1
Referring to fig. 1, a method for preparing an ndfeb grain boundary infiltration alloy cast sheet includes the following steps:
(1) charging in a vacuum smelting furnace: adding the conventional commercial neodymium iron boron alloy distribution raw materials of N45 in the industry into a crucible of a vacuum smelting furnace in sequence;
(2) vacuum smelting: smelting the alloy, and preparing for casting after smelting;
(3) preparing vacuum sputtering: starting a vacuum sputtering device, setting parameters, and performing coating preparation according to the coating thickness of 0.05 mm;
(4) starting a casting system: after the temperature of the alloy melt subjected to vacuum melting reaches 1450 ℃, starting a casting roller, pressing down an automatic pouring device of the crucible, pouring the alloy melt in the crucible above the casting roller, and forming an alloy casting sheet after passing through the casting roller;
(5) starting vacuum sputtering: when the alloy cast sheet begins to fall from the casting roll, starting a vacuum sputtering device, and carrying out vacuum sputtering coating operation on the fallen alloy cast sheet, wherein the whole process is about 9 minutes;
(6) cooling and discharging: stopping the vacuum sputtering device after the end, cooling the alloy cast sheet in a water cooling device for about 1 hour, and discharging the alloy cast sheet after the alloy cast sheet is cooled to 60 ℃;
(7) vacuum heat treatment: placing the neodymium iron boron alloy coated with the heavy rare earth coating in a vacuum heat treatment furnace for twice heat treatment; the first heat treatment process comprises the following steps: degree of vacuum 10-5Pa, the treatment temperature is 750 ℃, the heat preservation time is 5 hours, and the temperature is cooled to be below 100 ℃; the second heat treatment process comprises the following steps: degree of vacuum 10-2Pa, the treatment temperature is 480 ℃, the heat preservation time is 5 hours, and the temperature is cooled to the room temperature;
(8) and (3) processing and forming: after the heat treatment is finished, the black sheet with the specification of 30mm multiplied by 20mm multiplied by 7mm is processed, and the obtained black sheet is subjected to performance test, so that the coercive force can be improved by 5.9kOe under the original process condition, and the residual magnetism and the magnetic energy product are basically unchanged.
Example 2
Referring to fig. 1, a method for preparing an ndfeb grain boundary infiltration alloy cast sheet includes the following steps:
(1) charging in a vacuum smelting furnace: adding the conventional commercial neodymium iron boron alloy distribution raw materials of N45 in the industry into a crucible of a smelting furnace in sequence;
(2) vacuum smelting: smelting the alloy, and preparing for casting after smelting;
(3) preparing vacuum sputtering: starting a vacuum sputtering device, setting parameters, and performing coating preparation according to the coating thickness of 0.1 mm;
(4) starting a casting system: after the temperature of the alloy melt subjected to vacuum melting reaches 1450 ℃, starting a casting roller, pressing down an automatic pouring device of the crucible, pouring the alloy melt in the crucible above the casting roller, and forming an alloy casting sheet after passing through the casting roller;
(5) starting vacuum sputtering: when the alloy cast sheet begins to separate from the casting roll and fall downwards, starting a vacuum sputtering device, and carrying out vacuum sputtering coating operation on the fallen alloy cast sheet, wherein the whole process is about 10 minutes;
(6) cooling and discharging: stopping the vacuum sputtering device after the end, cooling the alloy cast sheet in a water cooling device for about 1 hour, and discharging the alloy cast sheet after the alloy cast sheet is cooled to 60 ℃;
(7) vacuum heat treatment: placing the neodymium iron boron alloy coated with the heavy rare earth coating in a vacuum heat treatment furnace for twice heat treatment; the first heat treatment process comprises the following steps: degree of vacuum 10-5Pa, the treatment temperature is 750 ℃, the heat preservation time is 5 hours, and the temperature is cooled to be below 100 ℃; the second heat treatment process comprises the following steps: degree of vacuum 10-2Pa, the treatment temperature is 480 ℃, the heat preservation time is 5 hours, and the temperature is cooled to the room temperature;
(8) and (3) processing and forming: after the heat treatment is finished, the black sheet with the specification of 30mm multiplied by 20mm multiplied by 7mm is processed, and the obtained black sheet is subjected to performance test, so that the coercive force can be improved by 8.5kOe under the original process condition, and the residual magnetism and the magnetic energy product are basically unchanged.
Example 3
Referring to fig. 1, a method for preparing an ndfeb grain boundary infiltration alloy cast sheet includes the following steps:
(1) charging in a vacuum smelting furnace: adding the conventional commercial neodymium iron boron alloy distribution raw materials of N45 in the industry into a crucible of a smelting furnace in sequence;
(2) vacuum smelting: smelting the alloy, and preparing for casting after smelting;
(3) preparing vacuum sputtering: starting a vacuum sputtering device, setting parameters, and performing coating preparation according to the coating thickness of 0.15 mm;
(4) starting a casting system: after the temperature of the alloy melt subjected to vacuum melting reaches 1500 ℃, starting a casting roller, pressing down an automatic pouring device of the crucible, pouring the alloy melt in the crucible above the casting roller, and forming an alloy casting sheet after passing through the casting roller;
(5) starting vacuum sputtering: when the alloy cast sheet begins to separate from the casting roll and fall downwards, starting a vacuum sputtering device, and carrying out vacuum sputtering coating operation on the fallen alloy cast sheet, wherein the whole process is about 12 minutes;
(6) cooling and discharging: and after the end, stopping the vacuum sputtering device, cooling the alloy casting sheet in a water cooling device for about 2 hours, and discharging the alloy casting sheet after the alloy casting sheet is cooled to 20 ℃.
(7) Vacuum heat treatment: placing the neodymium iron boron alloy coated with the heavy rare earth coating in a vacuum heat treatment furnace for twice heat treatment; the first heat treatment process comprises the following steps: degree of vacuum 10-3Pa, the treatment temperature is 920 ℃, the heat preservation time is 7 hours, and the temperature is cooled to be below 100 ℃; the second heat treatment process comprises the following steps: degree of vacuum 10-1Pa, the treatment temperature is 520 ℃, the heat preservation time is 4 hours, and the temperature is cooled to the room temperature.
(8) And (3) processing and forming: after the heat treatment is finished, the black sheet with the specification of 30mm multiplied by 20mm multiplied by 7mm is processed, and the obtained black sheet is subjected to performance test, so that the coercive force can be improved by 9.4kOe under the original process condition, and the residual magnetism and the magnetic energy product are basically unchanged.
In the above embodiments 1 to 3, a crucible, a casting roll, a vacuum sputtering apparatus, and a water cooling apparatus may be sequentially disposed in a vacuum melting furnace, the crucible being disposed above the casting roll, the vacuum sputtering apparatus being disposed below the casting roll, and above the water cooling apparatus; the existing vacuum rapid hardening furnace can be modified, a support frame is added above a water cooling device, a vacuum magnetron sputtering device is installed on the support frame, the center position of a nozzle is aligned to an effective area of an alloy casting sheet, and the height of the nozzle is 10-20 cm; the vacuum sputtering device adopts heavy rare earth elements dysprosium, terbium and alloys of dysprosium, terbium, aluminum and copper in a certain proportion as target materials for vacuum sputtering.
The thickness of the coating film of the sample after the coating treatment in examples 1 to 3 can be 0.02 to 0.2 mm.
The magnetic properties of the coated samples of examples 1-3 were compared with those of untreated commercial N45 dispensed black flakes in Table 1.
TABLE 1 comparison of magnetic Properties of the samples of the examples with those of the untreated samples
| Sample (I) | Br/kGs | Hcb/kOe | Hcj/kOe | (BH)max/MGOe | △Hcj/kOe |
| Commercial N45 partition | 13.52 | 12.80 | 13.21 | 43.26 | / |
| Example 1 sample | 13.48 | 12.96 | 19.11 | 43.68 | 5.9 |
| Example 2 sample | 13.47 | 12.98 | 21.71 | 43.72 | 8.5 |
| Example 3 sample | 13.46 | 13.01 | 22.61 | 43.85 | 9.4 |
In the process of casting in the vacuum rapid hardening furnace, the infiltration material is sputtered onto the uncooled alloy casting sheet in vacuum, a layer of heavy rare earth sputtering film is formed on the side surface of the alloy casting sheet, and the alloy casting sheet is placed into the vacuum heat treatment furnace for heat treatment, so that the heavy rare earth element is infiltrated into the alloy casting sheet, the effect of infiltration process is achieved, the infiltration effect of the heavy rare earth is good, the use amount of the heavy rare earth can be reduced by 20-30%, the utilization rate of the heavy rare earth element is improved, the production cost is greatly reduced, and the method can be popularized and applied in a large scale.
Finally, it should be noted that: the above examples are merely illustrative of the technical solutions of the present invention, and not limitative thereof; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (4)
1. A preparation method of a neodymium iron boron grain boundary infiltration alloy cast sheet is characterized by comprising the following steps: the method comprises the following steps:
(1) vacuum smelting: adding the neodymium iron boron alloy distribution raw materials into a crucible of a vacuum smelting furnace in sequence for smelting;
(2) casting: pouring the alloy melt in the crucible above a casting roller after the temperature of the melted alloy reaches 1450-1500 ℃, and forming an alloy casting sheet after the alloy melt passes through the casting roller;
(3) vacuum sputtering: after the alloy cast sheet is cast, carrying out vacuum sputtering coating operation before cooling to form a layer of heavy rare earth sputtering film on the side surface of the uncooled alloy cast sheet;
(4) cooling and discharging: after the vacuum sputtering coating operation, cooling the alloy cast sheet in a water cooling device, and discharging the alloy cast sheet after cooling to 20-60 ℃;
(5) vacuum heat treatment: placing the alloy cast sheet discharged from the furnace into a heat treatment furnace for carrying out heat treatment twice; the first heat treatment process comprises the following steps: vacuum degree of 10-5～10-3Pa, the treatment temperature is 750-920 ℃, the heat preservation time is 5-7 h, and the temperature is cooled to be below 100 ℃; the second heat treatment process comprises the following steps: vacuum degree of 10-2～10-1Pa, the treatment temperature is 480-520 ℃, the heat preservation time is 4-5 h, and the temperature is cooled to the room temperature.
2. The method for preparing the NdFeB grain boundary infiltration alloy casting sheet according to claim 1, wherein the vacuum sputtering device is arranged below the casting roller and above the water cooling device.
3. The method for preparing the NdFeB grain boundary infiltration alloy casting sheet according to claim 1, wherein in the step (3), the vacuum sputtering time is 9-12 minutes.
4. The method for preparing the NdFeB grain boundary infiltration alloy casting sheet according to claim 1, wherein in the step (3), the thickness of the vacuum sputtering coating is 0.02-0.2 mm.
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| CN104240883A (en) * | 2014-09-12 | 2014-12-24 | 沈阳中北通磁科技股份有限公司 | Rare-earth permanent magnet alloy plate, double-alloy neodymium-iron-boron permanent magnet and manufacturing methods thereof |
| CN104733148A (en) * | 2015-03-31 | 2015-06-24 | 安徽省瀚海新材料有限公司 | High-performance Re-TM-B permanent magnetic material manufacturing method |
| CN107424825A (en) * | 2017-07-21 | 2017-12-01 | 烟台首钢磁性材料股份有限公司 | A kind of neodymium iron boron magnetic body coercivity improves method |
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| CN104240883A (en) * | 2014-09-12 | 2014-12-24 | 沈阳中北通磁科技股份有限公司 | Rare-earth permanent magnet alloy plate, double-alloy neodymium-iron-boron permanent magnet and manufacturing methods thereof |
| CN104733148A (en) * | 2015-03-31 | 2015-06-24 | 安徽省瀚海新材料有限公司 | High-performance Re-TM-B permanent magnetic material manufacturing method |
| CN107424825A (en) * | 2017-07-21 | 2017-12-01 | 烟台首钢磁性材料股份有限公司 | A kind of neodymium iron boron magnetic body coercivity improves method |
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