CN112289533B - Regenerated neodymium iron boron magnetic material and preparation method thereof - Google Patents
Regenerated neodymium iron boron magnetic material and preparation method thereof Download PDFInfo
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- 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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- 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
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Abstract
The application relates to the field of neodymium iron boron magnetic materials, and particularly discloses a regenerated neodymium iron boron magnetic material and a preparation method thereof. A regenerated Nd-Fe-B magnetic material comprises the following components of PrNd, Cu, Al, B, Co, Ce, Zr, Ga, Tb, La, Bi and Fe. The preparation method comprises the following steps: and (3) mixing the recovered waste neodymium iron boron with a new material after hydrogen breaking and jet milling, and sintering to prepare a finished product neodymium iron boron. In the neodymium iron boron, Ce is used for replacing part of PrNd, and Bi is used for refining grains, so that the dosage of the PrNd can be reduced under the condition of ensuring that the coercive force of the neodymium iron boron magnetic material is not reduced. In addition, the preparation method of the application not only helps to reduce the development of PrNd resources by recycling the waste neodymium iron boron, but also can reduce the environmental pollution caused by waste PrNd.
Description
Technical Field
The application relates to the field of regenerated magnetic materials, in particular to a regenerated neodymium-iron-boron magnetic material and a preparation method thereof.
Background
The neodymium magnet is also called a neodymium-iron-boron magnet, and is a tetragonal crystal formed of neodymium, iron, and boron (Nd 2Fe 14B). In 1982, the neodymium magnet was discovered by a person living in the special metal of Sumitomo. The magnetic energy product (BHmax) of this magnet was greater than that of a samarium cobalt magnet, and was the largest in magnetic energy product worldwide at that time. Permanent magnets, which are second only to absolute zero holmium magnets in magnetic properties, are also the most commonly used rare earth magnets. For example, the remanence is about 11.8% s, the coercive force is 14 to 17kOe, the magnetic energy product is about 38MGOe, the working temperature is not more than 100 ℃, and the neodymium iron boron with the trade mark of 38M is widely applied to the fields of electronic products, in particular hard disks, mobile phones, earphones, tools powered by batteries and the like.
Meanwhile, since rare earth is an important nonrenewable resource, especially Pr and Nd are important constituent elements of the neodymium iron boron magnet. With the rapid development of the sintered Nd-Fe-B permanent magnet material industry in recent years, rare earth resources are greatly consumed. On the other hand, in the production and processing process of the sintered nd-fe-b product, from the initial raw material to the final finished product, each process inevitably generates scrap, and in addition, a large amount of finished products such as nd-fe-b motors and electronic products are scrapped, the number of waste sintered nd-fe-b magnets available every year is very large.
Therefore, on one hand, the formula of the original neodymium iron boron magnetic material needs to be improved, and on the other hand, the waste sintered neodymium iron boron magnetic blocks can be used for preparing the regenerated sintered neodymium iron boron magnetic material, so that the original resources of rare earth can be reduced, and the pollution of the waste magnets to the environment can be reduced due to the development of Pr and Nd resources.
Disclosure of Invention
In order to reduce development and waste of PrNd rare earth resources, the application provides a regenerated neodymium iron boron magnetic material and a preparation method thereof.
In a first aspect, the present application provides a regenerative ndfeb magnet, which adopts the following technical scheme:
the regenerated neodymium-iron-boron magnetic material comprises, by mass, 18-22% of PrNd, 0.15-0.2% of Cu, 0.2-0.7% of Al, 0.8-1.2% of B, 0.1-1% of Co, 15-20% of Ce, 0.1-0.2% of Zr, 0.6-1.2% of Ga, 0.6-1% of Tb, 0.2-0.4% of La, 0.1-0.12% of Bi, and the balance Fe and non-removable impurities.
By adopting the technical scheme, the neodymium iron boron magnetic material has the advantages that part of PrNd in the neodymium iron boron magnetic material is replaced by Ce, so that the use of the PrNd is reduced, and meanwhile, Bi can refine the whole crystal grains of the neodymium iron boron, so that the defect that the coercive force is reduced due to the fact that part of Ce is added is made up. Therefore, the using amount of PrNd can be reduced, and the problem of the reduction of the magnetic property of the neodymium iron boron is relieved.
Preferably, the mass ratio of Ce to Bi is 18: 0.11.
By adopting the technical scheme, with the increase of the bismuth content, although the crystal grains are obviously finer and more uniform than those without the bismuth, the enrichment degree of the bismuth in the crystal boundary is increased, so that part of the crystal grains grow irregularly, the boundary tissue is damaged, the neodymium-rich phase is unevenly distributed, the coercive force value of the magnet is reduced, and the magnetic performance is deteriorated.
And the mass ratio of Ce to Bi is controlled to be 18:0.11, so that Bi can effectively make up for the problem of coercive force reduction caused by Ce, and the problem of coercive force reduction of a magnet caused by nonuniform distribution of neodymium-rich phases due to excessive Bi content is avoided.
In a second aspect, the present application provides a method for preparing a regenerated ndfeb magnetic material, which adopts the following technical scheme:
a preparation method of a regenerative neodymium iron boron magnetic material comprises the following steps,
firstly, taking the recovered neodymium iron boron waste materials for oil removal, rust removal and impurity removal, then carrying out coarse crushing, and then analyzing the content of each component;
step two, performing hydrogen crushing and airflow milling treatment on the neodymium iron boron waste material coarsely crushed in the step one to obtain magnetic powder one;
step three, weighing new materials with required mass according to the content of each component in the magnetic powder I in the step two and the content of each component in the final finished product neodymium iron boron;
step four, carrying out melt refining on the new material obtained in the step three, and then pouring the new material on a water-cooled roller for melt spinning to obtain a melt spinning piece;
step five, adding the melt-spun sheet into a hydrogen breaking furnace for hydrogen breaking treatment to obtain a hydrogen broken sheet;
sixthly, performing jet milling treatment on the hydrogen fragments to obtain magnetic powder II;
step seven, uniformly mixing the magnetic powder I and the magnetic powder II to obtain mixed magnetic powder, and placing the mixed magnetic powder under the protection of nitrogen for compression molding to obtain a blank;
and step eight, placing the blank body on a carbon felt, then placing the blank body and the carbon felt together in a sintering furnace for sintering, and then performing primary tempering and secondary tempering to obtain the magnet.
Through adopting above-mentioned technical scheme, the neodymium iron boron waste material that will retrieve carries out hydrogen earlier and brokenly, later carries out the jet mill processing again to mix with new material. Therefore, not only can the development of PrNd resources be reduced, but also the pollution of waste PrNd to the environment can be avoided.
Preferably, the sintering temperature in the step eight is increased from normal temperature to 700-740 ℃ in the first stage, the temperature is kept for 0.5-1 h, and then increased to 1040-1100 ℃ in the second stage, and the temperature is kept for 2.5-3.5 h.
By adopting the technical scheme, the temperature is increased to 700-740 ℃, so that hydrogen which is not removed before the blank is completely densified can further permeate out of the blank, thereby reducing the possibility of cracking of the magnet during formal sintering and ensuring the integrity of the magnet.
Preferably, the primary tempering temperature in the step eight is 900-1000 ℃, the heat preservation lasts for 2-3 hours, the secondary tempering temperature is 640-680 ℃, and the heat preservation lasts for 2-3 hours.
By adopting the technical scheme, the secondary tempering can obviously improve the microstructure of the magnetic material, the crystal boundary becomes more regular and smooth, the Nd-rich phase is uniformly and dispersedly distributed around the crystal grains, the components of the crystal boundary phase can be further stabilized and uniform, and the thermal stability of the magnet is greatly improved.
Preferably, in the second step, neodymium hydride is doped into the coarse crushed neodymium iron boron waste material before hydrogen crushing, and the mass of neodymium in the neodymium hydride is 1-1.8% of that of neodymium in the coarse crushed neodymium iron boron waste material.
By adopting the technical scheme, the neodymium hydride is doped into the coarse crushed neodymium iron boron waste, so that the neodymium hydride can make up the loss of neodymium-rich phase of the neodymium iron boron waste caused by oxidation or volatilization, and the magnetic performance of the regenerated neodymium iron boron is ensured.
Preferably, in the seventh step, the mixed magnetic powder is compression molded in a 2.1T magnetic field.
By adopting the technical scheme, because the mixed magnetic powder does not form a compact state in the die, the orientation degree of the mixed magnetic powder can be improved by the additional 2.1T magnetic field, so that compared with the direct sintering and then the magnetic recharging, the energy consumption required for overcoming the mutual constraint among the molecules in order to improve the interior orientation degree of the magnet can be reduced, and the improvement of the magnetizing effect of the magnetic material is facilitated.
Preferably, in the seventh step, a lubricant and an antioxidant are added into the mixed magnetic powder, wherein the lubricant accounts for 0.03-0.09% of the mass of the mixed magnetic powder, and the antioxidant accounts for 1.2-1.6% of the mass of the mixed magnetic powder.
By adopting the technical scheme, firstly, the addition of the lubricant can reduce the friction force between the magnetic powder and improve the fluidity, so that the orientation degree and the compactness of the magnetic powder can be further improved in the mould pressing process, and further the improvement of the residual magnetism and the magnetic energy product of the magnet is facilitated.
Secondly, the addition of the antioxidant can inhibit the metal after hydrogenation reduction from being oxidized again in the subsequent operation process, thereby ensuring the magnetic property of the magnetic material.
In addition, the dosage of the lubricant is controlled to be 0.03-0.09%, and the dosage of the antioxidant is controlled to be 1.2-1.6%, because the lubricating effect and the antioxidant effect reach the optimal values basically, and if the dosage is increased continuously, the lubricant and the antioxidant cannot be completely removed in the sintering process, so that the serious burden is brought to a vacuum system, the content of C in the magnet is higher, and the density of the sintered magnet is reduced. So that the remanence and the energy product of the magnet are not improved but reduced.
Preferably, the lubricant is compounded by oxidized polyethylene wax and butyl oleate, and the mass ratio of the oxidized polyethylene wax to the butyl oleate is 1: 1.2.
by adopting the technical scheme, the composite lubricant of oxidized polyethylene wax and butyl oleate is selected, so that the lubricating effect can be ensured on one hand, and the volatilization is easy to occur in the neodymium iron boron sintering process on the other hand, thereby reducing the residual quantity of the lubricant and ensuring the coercive force and residual magnetism of neodymium iron boron.
Preferably, the antioxidant is compounded by tea polyphenol and vitamin E, and the mass ratio of the tea polyphenol to the vitamin E is 1.5: 1.
by adopting the technical scheme, the tea polyphenol is used for capturing oxygen free radicals and oxygen atoms, so that the reduced metal elements can be reduced and oxidized again. The vitamin E can play an auxiliary role, so that the retention time in the tea polyphenol magnetic powder is prolonged.
In summary, the present application has the following beneficial effects:
1. because Ce is used for replacing PrNd and Bi is used for refining the neodymium iron boron crystal, the application not only can reduce the using amount of PrNd resources, but also can ensure the coercive force and remanence of the neodymium iron boron magnetic material;
2. the use amounts of Ce and Bi are preferably controlled to be 18:0.11, so that on one hand, the refinement of Bi on neodymium iron boron grains can be ensured, the influence of Ce on the magnetism of neodymium iron boron can be compensated, on the other hand, the irregular growth of partial grains and the damage to boundary tissues caused by the overhigh content of Bi can be avoided, the distribution of neodymium-rich phases is uneven, and the coercive force value of a magnet is reduced;
3. according to the method, the neodymium iron boron waste materials are recycled, and are mixed with the new materials for use after being subjected to hydrogen crushing and airflow milling treatment, so that the using amount of PrNd can be reduced, and the environmental pollution caused by the waste PrNd can be avoided;
4. according to the method, neodymium hydride is added into the coarsely crushed neodymium iron boron waste, so that the loss of neodymium can be made up;
5. in the method, the lubricant is added into the magnetic powder, and the magnetic powder is subjected to die pressing in a magnetic field environment, so that the orientation degree of the magnetic material can be preliminarily improved before sintering, the compactness of the magnetic material is ensured, and the coercive force and the remanence of the magnetic material are improved after sintering;
6. according to the method, the antioxidant is added into the magnetic powder, so that the probability that the magnetic powder is oxidized in the later operation process can be reduced, and the magnetic property of the magnetic material is ensured.
Drawings
FIG. 1 is a 2000-fold magnified microstructure of the magnet of example 2;
FIG. 2 is a 1000-fold magnified microstructure of the magnet of example 6;
FIG. 3 is a 500-fold magnified microstructure of the magnet of example 7;
FIG. 4 is a 1000-fold magnified microstructure of the magnet of example 8.
Detailed Description
The present application will be described in further detail with reference to the following drawings and examples.
Example 1
A preparation method of a regenerated neodymium iron boron magnetic material comprises the following steps;
firstly, taking the recovered neodymium iron boron waste materials for oil removal, rust removal and impurity removal, then carrying out coarse crushing, and then analyzing the content of each component;
step two, adding neodymium hydride with the mass of 1% of that of neodymium in the neodymium iron boron waste into the neodymium iron boron waste which is coarsely crushed in the step one, then performing hydrogen crushing, and performing jet milling treatment after the hydrogen crushing is finished to obtain magnetic powder I;
step three, weighing new materials with required mass according to the content of each component in the magnetic powder I obtained in the step two and the content of each component in the final finished product neodymium iron boron magnet;
step four, carrying out melt refining on the new material obtained in the step three, and then pouring the new material on a water-cooled roller for melt spinning to obtain a melt spinning piece;
step five, adding the melt-spun sheet into a hydrogen breaking furnace for hydrogen breaking treatment to obtain a hydrogen broken sheet;
sixthly, performing jet milling treatment on the hydrogen fragments to obtain magnetic powder II;
step seven, uniformly mixing the magnetic powder I and the magnetic powder II to obtain mixed magnetic powder, adding a lubricant and an antioxidant into the mixed magnetic powder, and then placing the mixed magnetic powder in an environment of nitrogen and an external 2.1T pulse magnetic field for compression molding to obtain a blank;
placing the blank body on a carbon felt, then placing the blank body and the carbon felt in a vacuum sintering furnace, firstly heating the temperature from the normal temperature to 700 ℃ at a speed of 5 ℃/min at the first stage, and preserving the temperature for 0.5h, and then heating the blank body to 1040 ℃ at a speed of 4 ℃/min at the second stage, and preserving the temperature for 2.5h for sintering;
step nine: and after the sintering in the step eight is finished, reducing the temperature of the vacuum sintering furnace to normal temperature, then increasing the temperature to 900 ℃ at the speed of 5 ℃/min, preserving heat for 2 hours for primary tempering, continuing increasing the temperature to 640 ℃ at the speed of 5 ℃/min after the temperature is reduced to normal temperature, preserving heat for 2 hours for secondary tempering, and obtaining the magnet.
The magnet comprises the following components, by mass, 18% of PrNd, 0.15% of Cu, 0.2% of Al, 0.8% of B, 0.1% of Co, 15% of Ce, 0.1% of Zr, 0.6% of Ga, 0.6% of Tb, 0.2% of La, 0.1% of Bi and 64.15% of Fe.
Wherein, the lubricant accounts for 0.03 percent of the mass of the mixed magnetic powder, and the antioxidant accounts for 1.2 percent of the mass of the mixed magnetic powder. And the lubricant is compounded by oxidized polyethylene wax and butyl oleate, and the mass ratio of the oxidized polyethylene wax to the butyl oleate is 1: 1.2, the oxidized polyethylene wax of the present application is available from new materials, inc. The antioxidant is compounded by tea polyphenol and vitamin E, and the mass ratio of the tea polyphenol to the vitamin E is 1.5: 1.
the differences between examples 2 to 5 and example 1 are only the parameters shown in tables one and two,
table 1 mass percentages of each substance in the neodymium-iron-boron magnets of examples 2 to 5
Table 2 parameters of the neodymium iron boron magnet preparation methods of examples 2 to 5
The detection method comprises the following steps:
and (3) detecting the magnetic property of the neodymium iron boron magnetic material according to a GB/T3217 permanent magnet (hard magnet) material magnetic test method.
Table 3 test results of examples 1 to 5
Conclusion 1: it can be seen from the results of the above embodiments 1 to 5 that the performance of the ndfeb magnet of the present application is closer to the performance of the conventional 38M magnet, but the present application utilizes Ce to replace a large amount of PrNd, thereby reducing the production cost of the ndfeb and being beneficial to reducing the development of the PrNd resource.
Example 6
The only difference between this example and example 2 is that the Ce content is 17%, the Bi content is 0.1%, and the Fe content is 60.57%.
Example 7
The only difference between this example and example 2 is that the Ce content is 20%, the Bi content is 0.12%, and the Fe content is 57.55%.
Example 8
The only difference between this example and example 2 is that the Ce content is 16%, the Bi content is 0.1%, and the Fe content is 61.57%.
According to the detection methods of the embodiments 1 to 5, the embodiments 6 to 8 are detected, and the sections of the magnets of the embodiments 2, 6 to 8 are scanned by an electron microscope, so as to obtain the test results shown in the table 4 and the microstructure diagrams of the magnets shown in the attached figures 1 to 4:
table 4 test results of examples 6 to 8
Conclusion 2:
1. as can be seen from the comparison between FIG. 1 and FIGS. 2 and 3, when the mass ratio of Ce to Bi is 18: when 0.11, the crystal grains of the entire magnet become finer. At this time, by combining the detection results of the embodiment 2, the embodiment 6 and the embodiment 7, it can be seen that when the crystal grains are refined, the comprehensive magnetism of the neodymium iron boron magnet is also improved;
2. in addition, as can be seen from fig. 4, when the mass ratio of Ce to Bi is less than 18: at 0.11, the crystal grains of the whole magnet are finer, but the growth is irregular, and at this time, the comprehensive magnetism of the neodymium iron boron magnet is easily reduced when the crystal grains are too fine as can be seen by comparing the detection results of the embodiment 2 and the embodiment 8.
Comparative example 1
This comparative example differs from example 2 only in that a 2.1T pulsed magnetic field was not applied during the embossing.
Comparative example 2
The comparative example differs from example 2 only in that no lubricant is added to the mixed magnetic powder.
Comparative example 3
The comparative example differs from example 2 only in that the amount of lubricant added is 1.1% of the mixed magnetic powder.
Comparative example 4
This comparative example differs from example 2 only in that the lubricant is all oxidized polyethylene wax.
Comparative example 5
This comparative example differs from example 2 only in that the lubricants were all butyl oleate.
Comparative example 6
The comparative example differs from example 2 only in that no antioxidant is added to the mixed magnetic powder.
Comparative example 7
The comparative example differs from example 2 only in that the amount of antioxidant added was 1.8% of the mixed magnetic powder.
Comparative example 8
This comparative example differs from example 2 only in that the antioxidants are all tea polyphenols.
Comparative example 9
This comparative example differs from example 2 only in that the antioxidants are all vitamin E.
Comparative examples 1 to 9 were examined according to the examination methods of examples 1 to 5, and the examination results as shown in table 5 were obtained:
table 5 test results of comparative examples 1 to 9
Conclusion 3:
1. as can be seen from comparison of the detection results of example 2 and comparative example 1, the degree of orientation of the magnet is advantageously increased by applying a 2.1T pulse magnetic field, so that the magnetic properties of the magnet can be improved after sintering;
2. according to the comparison of the detection results of the embodiment 2, the comparative example 2 and the comparative example 3, when the mass of the lubricant is 0.03-0.09% of the mixed magnetic powder, the magnet can be ensured to have better orientation degree, and the magnet can not be remained in the magnet to influence the magnetic performance of the magnet.
3. According to the comparison of the detection results of the example 2 and the comparative examples 4 and 5, the comprehensive magnetism of the magnet can be effectively ensured only when the oxidized polyethylene wax and the butyl oleate are used in a compounding way;
4. according to the comparison of the detection results of the embodiment 2, the comparative example 6 and the comparative example 7, when the antioxidant accounts for 1.2-1.6% of the mass of the mixed magnetic powder, the possibility that the magnetic powder is oxidized in the subsequent blank manufacturing and sintering processes to influence the comprehensive magnetism of the magnet can be reduced, and the influence of the magnetic powder remaining in the magnet on the magnetic performance of the magnet can be avoided;
5. according to the comparison of the detection results of the example 2 and the comparative examples 8 and 9, it can be seen that the oxidation resistance of the magnet raw material can be effectively ensured only when the tea polyphenol and the vitamin E are compounded for use, so that the comprehensive magnetic performance of the magnet raw material can be ensured.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (4)
1. A regenerated neodymium-iron-boron magnetic material comprises, by mass, 18-22% of PrNd, 0.15-0.2% of Cu, 0.2-0.7% of Al, 0.8-1.2% of B, 0.1-1% of Co, 15-20% of Ce, 0.1-0.2% of Zr, 0.6-1.2% of Ga, 0.6-1% of Tb, 0.2-0.4% of La, 0.1-0.12% of Bi, and the balance of Fe and irremovable impurities, wherein the mass ratio of Ce to Bi is 18: 0.11;
the preparation method comprises the following steps of,
firstly, taking the recovered neodymium iron boron waste materials for oil removal, rust removal and impurity removal, then carrying out coarse crushing, and then analyzing the content of each component;
step two, performing hydrogen crushing and airflow milling treatment on the neodymium iron boron waste material coarsely crushed in the step one to obtain magnetic powder one;
step three, weighing new materials with required mass according to the content of each component in the magnetic powder I in the step two and the content of each component in the final finished product neodymium iron boron magnet;
step four, carrying out melt refining on the new material obtained in the step three, and then pouring the new material on a water-cooled roller for melt spinning to obtain a melt spinning piece;
step five, adding the melt-spun sheet into a hydrogen breaking furnace for hydrogen breaking treatment to obtain a hydrogen broken sheet;
sixthly, performing jet milling treatment on the hydrogen fragments to obtain magnetic powder II;
step seven, uniformly mixing the magnetic powder I and the magnetic powder II to obtain mixed magnetic powder, and placing the mixed magnetic powder under the protection of nitrogen for compression molding to obtain a blank;
placing the blank body on a carbon felt, then placing the blank body and the carbon felt together in a sintering furnace for sintering, and then performing primary tempering and secondary tempering to obtain a magnet;
in the seventh step, a lubricant and an antioxidant are added into the mixed magnetic powder, wherein the lubricant accounts for 0.03-0.09% of the mass of the mixed magnetic powder, the antioxidant accounts for 1.2-1.6% of the mass of the mixed magnetic powder, the lubricant is compounded by oxidized polyethylene wax and butyl oleate, and the mass ratio of the oxidized polyethylene wax to the butyl oleate is 1: 1.2, the antioxidant is compounded by tea polyphenol and vitamin E, and the mass ratio of the tea polyphenol to the vitamin E is 1.5: 1; and doping neodymium hydride into the coarse crushed neodymium iron boron waste before hydrogen crushing, wherein the mass of neodymium in the neodymium hydride is 1-1.8% of that of neodymium in the coarse crushed neodymium iron boron waste.
2. The recycled ndfeb magnet as set forth in claim 1, wherein: and step eight, the sintering temperature is increased from the normal temperature to 700-740 ℃ in the first stage, the temperature is kept for 0.5-1 h, and is increased to 1040-1100 ℃ in the second stage, and the temperature is kept for 2.5-3.5 h.
3. The recycled ndfeb magnet as set forth in claim 1, wherein: and in the eighth step, the primary tempering temperature is 900-1000 ℃, the heat preservation lasts for 2-3 hours, the secondary tempering temperature is 640-680 ℃, and the heat preservation lasts for 2-3 hours.
4. The recycled ndfeb magnet as set forth in claim 1, wherein: and step seven, compression molding the mixed magnetic powder in a 2.1T pulse magnetic field.
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| CN113223800A (en) * | 2021-04-28 | 2021-08-06 | 慈溪市兴发磁业科技有限公司 | Low-cost neodymium iron boron permanent magnet and preparation method thereof |
| CN113643872A (en) * | 2021-07-30 | 2021-11-12 | 宁波中杭磁材有限公司 | Cerium-containing neodymium-iron-boron magnetic steel and preparation method thereof |
| CN114999805B (en) * | 2022-06-13 | 2023-12-26 | 安徽吉华新材料有限公司 | Preparation method of high-performance regenerated permanent magnet material |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS57118605A (en) * | 1981-01-16 | 1982-07-23 | Seiko Epson Corp | Sintering type rare-earth magnet |
| US6833036B2 (en) * | 2001-06-29 | 2004-12-21 | Tdk Corporation | Rare earth permanent magnet |
| CN109192495B (en) * | 2018-11-07 | 2021-01-29 | 安徽大地熊新材料股份有限公司 | Preparation method of regenerative sintered neodymium-iron-boron permanent magnet |
| CN111180189A (en) * | 2019-12-31 | 2020-05-19 | 慈溪市恒韵照明有限公司 | Method for preparing N40M type sintered NdFeB magnetic material by adding 38M waste material |
| CN111341512B (en) * | 2020-03-09 | 2022-07-08 | 钢铁研究总院 | High-cost performance rare earth permanent magnet and preparation method thereof |
| CN111341515B (en) * | 2020-03-25 | 2022-08-23 | 余姚市宏伟磁材科技有限公司 | Cerium-containing neodymium-iron-boron magnetic steel and preparation method thereof |
| CN111613410B (en) * | 2020-06-04 | 2022-08-02 | 福建省长汀金龙稀土有限公司 | Neodymium-iron-boron magnet material, raw material composition, preparation method and application |
| CN112233868B (en) * | 2020-09-25 | 2024-04-30 | 宁波科星材料科技有限公司 | Composite gold multiphase neodymium-iron-boron magnet and preparation method thereof |
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