CN115588570A - Method for utilizing waste neodymium iron boron materials of dismantling machine - Google Patents

Method for utilizing waste neodymium iron boron materials of dismantling machine Download PDF

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Publication number
CN115588570A
CN115588570A CN202211166165.7A CN202211166165A CN115588570A CN 115588570 A CN115588570 A CN 115588570A CN 202211166165 A CN202211166165 A CN 202211166165A CN 115588570 A CN115588570 A CN 115588570A
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magnet
iron boron
neodymium iron
waste
utilizing
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Inventor
黄伟超
甘家毅
陈东雯
谢觉
黄粟
利天军
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China Rare Earth Guangxi Jinyuan Rare Earth New Material Co Ltd
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China Rare Earth Guangxi Jinyuan Rare Earth New Material Co Ltd
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    • 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
    • H01F41/0266—Moulding; Pressing
    • 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
    • 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
    • H01F1/0573—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 obtained by reduction or by hydrogen decrepitation or embrittlement
    • 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
    • H01F1/0576—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 pressed, e.g. hot working
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies

Abstract

The invention belongs to the technical field of reutilization of neodymium iron boron waste materials, and particularly relates to a utilization method of dismantling neodymium iron boron waste materials, which comprises the steps of sequentially carrying out thermal demagnetization treatment and surface treatment on dismantling neodymium iron boron waste materials, adopting reducing metal or hydride thereof to repair the surface of a magnet, then mechanically processing the magnet into a required size, and sequentially carrying out grain boundary diffusion and thermal treatment to recover the service performance; the method is simple and efficient, does not need to be subjected to separation, purification or crushing and remanufacturing processes, obviously shortens the flow, avoids the pollution of the regeneration process to the environment and the processing loss, and has the characteristics of environmental protection, energy conservation, high efficiency, low cost and the like; the method adopts various reducing metals or compounds thereof to repair the surface of the waste magnet, improves the coercive force and the heat resistance of the magnet, basically does not damage the remanence of the magnet, meets the application requirement that the coercive force of the magnet needs to be synchronously improved due to the thinning of the magnet during processing and the reduction of a working load line in the recycling process of the magnet, and has better practical effect.

Description

Method for utilizing waste neodymium iron boron materials of dismantling machine
Technical Field
The invention belongs to the technical field of neodymium iron boron waste recycling, and particularly relates to a method for utilizing machine dismantling neodymium iron boron waste.
Background
Sintered Nd-Fe-B is the third generation rare earth permanent magnetic material, is the magnetic material with the widest application and the highest comprehensive magnetic performance at present, and is widely applied to IT electronics, industrial motors and new energy industries.
The sintered NdFeB can be used for a long time under the working condition, however, due to the requirement of updating and upgrading of the equipment, the sintered NdFeB magnets applied to the equipment are scrapped, and therefore a large amount of NdFeB waste materials are generated. The sintered neodymium iron boron contains active rare earth elements, and surface damage, oxidation and corrosion are easy to occur due to long-term use. Therefore, the waste neodymium iron boron materials detached from the scrapping equipment can not be directly used.
The rare earth elements in the sintered neodymium iron boron have great recovery value, and the early recovery of the neodymium iron boron mainly adopts a hydrochloric acid preferential dissolution recovery process. The process comprises the steps of completely dissolving a neodymium iron boron matrix by using strong acid, removing iron element impurities by controlling a valence state and a pH value, and then obtaining the high-purity rare earth oxide by sequentially carrying out extraction separation, precipitation and ignition. Furthermore, single rare earth metal can be prepared by an electrolytic reduction method and recycled as a raw material of the neodymium iron boron. The rare earth element obtained by the process has high purity, and the performance of the material cannot be reduced. However, the disadvantages are obvious, and mainly include complex process flow, large acid and alkali consumption, high treatment cost, large pollution, low yield and the like.
The HD method for preparing the regenerated magnet is a newly developed technology for efficiently recycling the neodymium iron boron waste. For example, patent No. CN201710160868.1 discloses a method for manufacturing high-performance neodymium iron boron by using sintered neodymium iron boron waste materials, which specifically comprises the following steps: pretreating sintered neodymium iron boron waste to prepare a magnet block; step (2) performing the hydrogen explosion treatment on the magnet block to prepare coarse powder; mechanically crushing the coarse powder, adding a solid additive, grinding the coarse powder into fine powder with the average particle size of 2.8-3.2 mu m by using an air flow mill, adding a liquid lubricant into the fine powder, and adding DyH3 into the fine powder according to the weight proportion of the DyH3; step (4) after the fine powder added with DyH3 is passivated, pressing the fine powder into a pressed blank, and carrying out isostatic pressing treatment; and (5) sintering and tempering. The disadvantages of this process are also evident, since the rare earths in the scrap are oxidized, and therefore the regeneration process requires the replenishment of large amounts of rare earths, increasing the cost of the process and significantly reducing the magnet performance. In the remanufacturing process of the magnet, the yield is only 60-70%, which further increases the material consumption and cost.
Disclosure of Invention
The invention provides a utilization method of a machine disassembling neodymium iron boron waste material aiming at the defects of the prior art.
The method is realized by the following technical scheme:
a method for utilizing the waste material of neodymium iron boron includes such steps as thermal demagnetizing, surface treating, repairing the surface of magnet by reductive substance, machining to needed size, and grain boundary diffusion and heat treatment.
Specifically, the utilization method of the waste neodymium iron boron materials comprises the following steps:
(1) Placing the disassembled neodymium iron boron waste magnet at the temperature of 350-600 ℃, and carrying out demagnetization treatment for 1-5 hours under the protection of any gas of air, argon or nitrogen to obtain a nonmagnetic matrix;
(2) Removing a plating layer, corrosion and surface inclusions on the surface of the substrate by any one of acid washing, mechanical grinding and grinding, and then blowing by airflow and drying in a drying box to obtain the neodymium iron boron substrate with a clean surface;
(3) Covering the surface of the magnet with reducing metal or hydride powder thereof, and then treating for 3-5 h at 675-850 ℃ in a vacuum sintering furnace under the vacuum condition or under the protection of protective gas;
(4) The magnet is machined to the desired dimensions and subsequently heat treated in a vacuum sintering furnace to restore its properties.
The machine-disassembling neodymium iron boron waste material refers to a massive neodymium iron boron magnet which is disassembled and stored on a motor, a magnetic separator or other neodymium iron boron devices.
The reducing metal is any one of Ca, mg, zn, al and lanthanide series.
The protective gas is any one of nitrogen or argon.
The heat treatment comprises a secondary tempering process, and the sintering is carried out for 6 to 12 hours at the temperature of 850 to 1020 ℃ and then for 1 to 5 hours at the temperature of 470 to 530 ℃.
The grain boundary diffusion refers to that a layer of mixture of heavy rare earth elements, BFe and normal hexane is attached to the surface of the magnet through any one of physical adhesion, spraying and coating; the heavy rare earth element is Dy, tb or a compound thereof; the ratio of n-hexane to rare earth metal to BFe in the mixture is 50.
The utilization method of the machine dismantling neodymium iron boron waste material can further comprise the steps of further surface treatment and magnetization of the regenerated magnet.
Has the advantages that:
the invention mainly adopts a surface repairing method, which comprises simple surface treatment, surface layer reduction and grain boundary diffusion, realizes the recovery of the performance of the magnet and meets the requirement of the continuous service of the magnet. The process is simple and efficient, does not need a separation, purification or crushing and remanufacturing process, obviously shortens the flow, avoids the pollution and processing loss of the regeneration process to the environment, and has the characteristics of environmental protection, energy conservation, high efficiency, low cost and the like.
The invention adopts a plurality of reducing metals or compounds thereof to repair the surface of the waste magnet, particularly takes the mixture of BFe and heavy rare earth elements as a penetrating agent, obviously improves the coercive force and the heat resistance of the magnet, basically does not damage the residual magnetism of the magnet, meets the application requirement that the coercive force of the magnet needs to be synchronously improved because the magnet is processed to be thinned and the working load line is reduced in the recycling process of the magnet, and has better practical effect.
Detailed Description
The following is a detailed description of the embodiments of the present invention, but the present invention is not limited to these embodiments, and any modifications or substitutions in the basic spirit of the embodiments are included in the scope of the present invention as claimed in the claims.
Example 1
A utilization method of machine-dismantling neodymium iron boron waste materials comprises the following steps:
(1) Placing the disassembled neodymium iron boron waste magnet at the temperature of 350 ℃, and carrying out demagnetization treatment for 5 hours in the air atmosphere to obtain a nonmagnetic matrix;
(2) The method comprises the following steps of (1) adopting a mechanical grinding method, enabling a plating layer, corrosion and impurities on the surface of a substrate to fall off through material self-grinding, removing impurities adhered to the surface through air flow blowing, and then drying in a drying oven at 100 ℃ to obtain the neodymium iron boron substrate with a clean surface;
(3) Adding CaH 2 Covering the powder on the surface of the magnet, and treating for 3h at 675 ℃ in a vacuum sintering furnace under the vacuum condition to obtain the surface-repaired magnet.
(4) Machining the magnet to a required size, coating a mixture of dysprosium fluoride, ferroboron and n-hexane on the surface of the magnet by a spraying method, wherein the ratio of the n-hexane: dysprosium fluoride: the ferroboron ratio was 50.
Example 2
A utilization method of machine-dismantling neodymium iron boron waste materials comprises the following steps:
(1) Placing the disassembled neodymium iron boron waste magnet at the temperature of 600 ℃, and carrying out demagnetization treatment for 1h under the protection of argon atmosphere to obtain a nonmagnetic matrix;
(2) Adopting a nitric acid-assisted ultrasonic cleaning method to dissolve a plating layer, rust and impurities on the surface of the substrate, washing the surface with flowing clear water, and drying at 100 ℃ in a drying oven to obtain a neodymium iron boron substrate with a clean surface;
(3) And covering the surface of the magnet with NdHx powder, and treating for 5h at 850 ℃ in a vacuum sintering furnace under a vacuum condition to obtain the surface-repaired magnet.
(4) The magnet is machined to a required size, and a blend of terbium hydride, ferroboron and n-hexane is coated on the surface of the magnet by a coating method, wherein the ratio of the n-hexane: terbium hydride: the ferroboron ratio was 50.
Example 3
A utilization method of machine-dismantling neodymium iron boron waste materials comprises the following steps:
(1) Placing the disassembled neodymium iron boron waste magnet at the temperature of 550 ℃, and carrying out demagnetization treatment for 2 hours under the protection of nitrogen atmosphere to obtain a nonmagnetic matrix;
(2) Removing a plating layer, corrosion and impurity dissolution on the surface of the matrix by adopting a mechanical grinding method, washing the surface by using flowing clear water, and drying at 100 ℃ in a drying box to obtain a neodymium iron boron matrix with a clean surface;
(3) And covering the PrHx powder on the surface of the magnet, and treating for 4 hours at 800 ℃ in a vacuum sintering furnace under a vacuum condition to obtain the surface-repaired magnet.
(4) The magnet is machined to the required size, and a blend of dysprosium hydride, terbium hydride, ferroboron and n-hexane is coated on the surface of the magnet by a coating method, wherein the weight ratio of the n-hexane: dysprosium hydride, terbium hydride: the ferroboron ratio is 50.
The initial properties of the examples 1-3 and the disassembled ndfeb scrap are shown in table 1, as detected:
TABLE 1
Figure BDA0003861445410000061

Claims (8)

1. A method for utilizing the waste Nd-Fe-B material includes such steps as thermal demagnetizing, surface treating, repairing the surface of magnet by reductive metal or its hydride, machining to needed size, and grain boundary diffusion and heat treatment.
2. The method for utilizing the waste neodymium iron boron materials of the dismantling machine as claimed in claim 1, characterized by comprising the following steps:
(1) Placing the disassembled neodymium iron boron waste magnet at the temperature of 350-600 ℃, and carrying out demagnetization treatment for 1-5 h under the protection of air or any gas of argon or nitrogen to obtain a nonmagnetic matrix;
(2) Removing a plating layer, corrosion and surface inclusions on the surface of the substrate by any one of acid washing, mechanical grinding and grinding, and then blowing by airflow and drying in a drying box to obtain the neodymium iron boron substrate with a clean surface;
(3) Covering the surface of the magnet with reducing metal or hydride powder thereof, and then treating for 3-5 h at 675-850 ℃ in a vacuum sintering furnace under the vacuum condition or under the protection of protective gas;
(4) The magnet is machined to the desired dimensions and subsequently heat treated in a vacuum sintering furnace to restore its properties.
3. The method for utilizing the scrapper neodymium iron boron scrap according to claim 1 or 2, wherein the reducing metal is any one of Ca, mg, zn, al and lanthanide series.
4. The method for utilizing the scrapper neodymium iron boron waste material of claim 2, wherein the protective gas is any one of nitrogen or argon.
5. The utilization method of the disassembled neodymium iron boron waste material as claimed in claim 1 or 2, wherein the heat treatment comprises a secondary tempering process, sintering is carried out for 6-12 h under the condition of 850-1020 ℃, and then sintering is carried out for 1-5 h under the condition of 470-530 ℃.
6. The utilization method of the scrapper neodymium iron boron scrap according to claim 1 or 2, wherein the grain boundary diffusion means that a layer of mixture of heavy rare earth elements, BFe and n-hexane is attached to the surface of the magnet by any one of physical adhesion, spraying and coating.
7. The method for utilizing the waste neodymium iron boron material is characterized in that the heavy rare earth element is Dy, tb or a compound thereof.
8. The utilization method of the disassembled neodymium iron boron waste material is characterized in that the ratio of n-hexane to rare earth metal to BFe in the mixture is (50).
CN202211166165.7A 2022-09-23 2022-09-23 Method for utilizing waste neodymium iron boron materials of dismantling machine Pending CN115588570A (en)

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