CN105195735A - Method for preparing rare earth permanent magnetic material by adding liquid-phase cerium in waste magnetic steel - Google Patents
Method for preparing rare earth permanent magnetic material by adding liquid-phase cerium in waste magnetic steel Download PDFInfo
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Abstract
The invention provides a method for preparing rare earth permanent magnetic material by adding liquid-phase cerium in waste magnetic steel. The method comprises the steps of pre-sorting the collected waste magnetic steel according to the same type and same model of waste magnetic steel containing the same rare earth elements, thus obtaining pre-processed magnetic materials; directly carrying out hydrogen crushing on the pre-processed magnetic materials to prepare powder, thus obtaining rare earth-hydrogen magnetic powder; sampling and analyzing the rare earth-hydrogen magnetic powder, and adding liquid-phase cerium into the rare earth-hydrogen crushing powder to obtain mixed powder; and finally carrying out static pressure, sintering and annealing to prepare the rare earth permanent magnetic material. Therefore, the problem of segregation of alloy ingot obtained by melting due to different melting points of components and manual operation can be effectively solved; through the pre-sorting, not only can the time for recovering the waste magnetic steel be saved, but also the process steps of extracting rare earth elements can be reduced; liquid-phase cerium is added into the pre-processed magnetic materials, so that the reduction of the melting point of alloy liquid can be facilitated, fine crystal grain magnets can be obtained and thus, the coercivity of the magnet can be improved.
Description
Technical field
The present invention relates to rare-earth permanent-magnet material technical field, particularly relate to a kind of method of adding liquid phase cerium and preparing rare earth permanent-magnetic material in waste and old magnet steel.
Background technology
In recent years, along with the continuous expansion of rare earth permanent-magnetic material application, increasing to raw-material demand, but because the cost of rare earth mining is higher and along with the increasing of national regulation and control dynamics, its material cost also strengthens gradually.And when present price amount of increase is excessive, the price endurance of down-stream enterprise is more limited, the materials such as the ferrite that therefore portion downstream enterprise choice for use is more cheap or aluminium nickel cobalt, SmCo replace the rare earth in neodymium iron boron magnetic body raw material, and this brings larger unstability to neodymium iron boron magnetic body market.Simultaneously because Nd-Fe-B magnetic material fragility is high, specification is mixed, the problem such as very easily occur unfilled corner and size is bad in electroplating process; And then the learies causing electroplating rear neodymium iron boron magnetic body is very large, be only the scrappage of finished appearance and size just between 2 ~ 5%, and also often cause that generation is bad scraps phenomenon due to other aspect particular/special requirements of client.
Process at present for the recycle and reuse of waste and old magnet steel is: lumped together by all waste and old magnet steel collected, presort, and unification is back to returnable, in returnable, various rare earth elements contained in waste and old magnet steel are extracted one by one, then again process according to the rare earth permanent-magnetic material of required preparation.Although this process recycles waste and old magnet steel, but its abstraction process is complicated, and need for the various technological parameters of different rare earth element fusing point adjustment returnable, with the extraction process requirement of satisfied different rare earth element, this has put forward higher requirement to the equipment of returnable.Again carry out adding man-hour simultaneously, recovery is obtained single rare-earth oxide, after proportioning smelts Deng Ge road technique, the permanent-magnet material requiring preparation is obtained in rear road, and the permanent magnet adopting this technique to obtain has many defects, production process is difficult to control, human factor is more, and then the quality of impact batch production.In addition, the actual coercivity of permanent-magnet material that existing production technology is produced is low, service temperature stability is lower, and corrosion resistance is weak, becomes the principal element limiting its development and application.
In addition, usually the metal adding a small amount of low melting point is adopted in prior art, as gallium, copper, aluminium, germanium, zinc, tin etc., forming new low melting point eutectic phase acceleration of sintering by adding one or more alloying elements and the rare earth element such as neodymium, praseodymium, improving the microstructure of rich neodymium phase, thus realize coercitive regulation and control.But because above-mentioned metal is non-magnetic phase, can only add by trace, therefore it can only realize regulation and control to the distribution of neodymium phase rich in sintering temperature and drawing process and heterogeneous microstructure in more among a small circle.On the other hand, the rare-earth elements of lanthanum, cerium etc. of interpolation can reduce sintering temperature, but the saturation magnetization of lanthanum iron boron and ferrocerium boron phase is lower than neodymium iron boron phase, and reduce the remanent magnetism of magnet, particularly its anisotropy field is only 1/3rd of neodymium iron boron phase.And the raising of oxygen content, easily cause the changes in microstructure of Nd-rich phase, cause the coercivity of magnet to reduce further, be difficult to arrive the requirement of business magnet to the comprehensive magnetic such as coercivity and magnetic energy product energy.
And by rare earth permanent-magnetic material prepared by rare earth element, there is the characteristics such as high catalytic activity, high magnetic, superconductivity, photoelectric conversion, optomagnetic memory, high weight of hydrogen, corrosion-proof wear; Therefore, under the prerequisite not changing rare earth permanent-magnetic material characteristic, how to improve the bending strength of rare earth permanent-magnetic material, hardness and toughness, avoid alloy pig material during follow-up melting to produce segregation, and reduction has become those skilled in the art's major issue urgently to be resolved hurrily to the technical requirement of production equipment simultaneously.
Summary of the invention
Technical problem solved by the invention is to provide a kind of method of adding liquid phase cerium and preparing rare earth permanent-magnetic material in waste and old magnet steel, to solve the shortcoming in above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
In waste and old magnet steel, add the method that liquid phase cerium prepares rare earth permanent-magnetic material, its concrete steps are as follows:
1) presorted according to rare earth element contained in magnet steel by the waste and old magnet steel collected, the standard of presorting is classified as a class for the waste and old magnet steel identical with rare earth element contained by batch same model, obtains pretreatment magnet material;
2) according to preparation rare earth permanent-magnetic material, to step 1) in obtain pretreatment magnet material directly carry out the broken powder process of hydrogen, obtain the broken magnetic of rare earth hydrogen;
3) to step 2) in obtain the broken magnetic of rare earth hydrogen carry out sample analysis, obtain rare-earth magnetic component parameter;
4) according to step 3) in analyze the rare-earth magnetic component parameter that obtains, in the broken magnetic of rare earth hydrogen obtained, add liquid phase cerium obtain mixed powder, the percent mass proportioning of mixed powder: the broken magnetic of 98 ~ 99.5% rare earth hydrogen, 0.5 ~ 2% liquid phase cerium;
5) by step 4) in mixed powder, the airflow milling broken by hydrogen that obtain be broken into fine powder, and put into quantitative air when carrying out airflow milling and carry out passivation, and mix and blend is carried out to the powder that front and back grind;
6) by step 5) in the fine powder that obtains add isostatic pressing method by mold pressing and be pressed into pressed compact;
7) by step 6) in the pressed compact that obtains be placed in vacuum sintering furnace and sinter and be incubated;
8) by step 7) in sintering after pressed compact in vacuum sintering furnace, be cooled to 300 DEG C ~ 350 DEG C, be warming up to first paragraph heat treatment again and be incubated, then continue to be cooled to 300 DEG C ~ 350 DEG C, finally be warming up to second segment heat treatment and be incubated, and respectively tempering is carried out to two sections of heat treatments, to obtain rare earth permanent-magnetic material base substrate;
9) by step 8) the middle rare earth permanent-magnetic material base substrate obtained, carry out machining cutting according to the actual requirements and refine, reserved size of carrying out electroplating, obtains rare earth permanent-magnetic material simultaneously.
In the present invention, described step 5) in, fine powder particle mean size is 2.4 ~ 3.2 μm.
In the present invention, described step 6) in, the pressure of isostatic pressed is 230 ~ 280MPa.
In the present invention, described step 7) in, sintering temperature is 1070 DEG C ~ 1095 DEG C.
In the present invention, described step 7) in, temperature retention time is 200 minutes.
In the present invention, described step 8) in, first paragraph heat treatment temperature is 900 DEG C ~ 920 DEG C, and temperature retention time is 90 minutes; Second segment heat treatment temperature is 530 DEG C ~ 620 DEG C, and temperature retention time is 200 minutes.
In the present invention, by the waste and old magnet steel collected is presorted according to rare earth element contained in magnet steel, the content of various rare earth element in the waste and old magnet steel being about to process can be obtained, and then effectively adjust for different rare earth element fusing point, not only save the time of reclaiming waste and old magnet steel, and reduce the processing step extracting different rare earth element in waste and old magnet steel and the requirement reduced returnable equipment, also provide convenient for producing with the rare earth permanent-magnetic material later process of the equal model of waste and old magnet steel simultaneously; Be conducive to the adding of cerium the fusing point reducing aluminium alloy, because the fusing point of liquid phase is low, can low-temperature sintering be realized, obtain fine grain magnet, thus improve the coercivity of magnet; Simultaneously because liquid phase has lower fusing point, the good fluidity therefore in sintering process, can be evenly distributed between neodymium iron boron main phase grain, make the Grain-Boundary Phase of sintered magnet smooth straight, effectively improve the ability that it removes exchange-coupling interaction.
A kind of rare earth permanent-magnetic material, comprises neodymium, praseodymium, cerium, boron, copper, aluminium, yttrium and iron; Each constituent mass percentage is: 10 ~ 20% neodymiums, 8 ~ 15% praseodymiums, 0.5 ~ 2% cerium, 0.5 ~ 1.2% boron, 0 ~ 0.25% bronze medal, 0 ~ 0.8% aluminium, 0.2 ~ 3% yttrium, 57 ~ 81% iron, and iron is iron and inevitable impurity.
Beneficial effect: the present invention is by by presorting the waste and old magnet steel collected according to rare earth element contained in magnet steel, the content of various rare earth element in the waste and old magnet steel being about to process can be obtained, and then effectively adjust for different rare earth element fusing point, not only save the time of reclaiming waste and old magnet steel, and reduce the processing step extracting different rare earth element in waste and old magnet steel and the requirement reduced returnable equipment, also provide convenient for producing with the alloy permanent-magnet material later process of the equal model of waste and old magnet steel simultaneously; And by analyzing the rare-earth magnetic component parameter obtained, in the broken magnetic of rare earth hydrogen obtained, add liquid phase cerium obtain mixed powder, the production cost of effective reduction enterprise, and the fusing point solving each component in traditional fusion process is different and manual operation factor and the problem of alloy pig generation segregation to cause after melting, be conducive to the adding of cerium the fusing point reducing aluminium alloy, because the fusing point of liquid phase is low, be convenient to realize low-temperature sintering, obtain fine grain magnet, thus improve the coercivity of magnet; Be conducive to the adding of yttrium the actual coercivity improving alloy pig, reduce neodymium, praseodymium consumption simultaneously.
Detailed description of the invention
Describe the present invention below by following specific embodiment.
Embodiment 1
A kind of rare earth permanent-magnetic material, prepare burden by such as following table 1-1:
Table 1-1 embodiment 1 formula table
| Component | Neodymium | Praseodymium | Cerium | Yttrium | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 4.2 | 3.2 | 0.1 | 0.04 | 0.17 | 0.02 | 0.04 | 13.3 | 21.07 |
| Mass percent/% | 20 | 15 | 0.5 | 0.2 | 0.5 | 0.1 | 0.2 | 63.5 | 100 |
The preparation method of the above-mentioned rare earth permanent-magnetic material of the present embodiment is as follows:
The criteria for classification that the waste and old magnet steel collected is classified as a class according to the waste and old magnet steel identical with rare earth element contained by batch same model is presorted, obtains pretreatment magnet material, then according to the rare earth permanent-magnetic material of preparation, the broken powder process of hydrogen is directly carried out to the pretreatment magnet material obtained, obtains the broken magnetic of rare earth hydrogen, sample analysis is carried out to the broken magnetic of rare earth hydrogen obtained simultaneously, obtain rare-earth magnetic component parameter, again according to analyzing the rare-earth magnetic component parameter obtained, in the broken magnetic of rare earth hydrogen obtained, add liquid phase cerium obtain mixed powder, finally by broken by hydrogen for the mixed powder obtained, airflow milling is broken into fine powder, and put into quantitative air when carrying out airflow milling and carry out passivation, and mix and blend is carried out to the powder that front and back grind, the particle mean size of fine powder is 2.4 μm, successively fine powder is added isostatic pressing method by mold pressing and be pressed into pressed compact, and the pressure of isostatic pressed is 230MPa, green density is 4.3g/cm
3, after treating that fine powder is all suppressed, pressed compact is placed in vacuum sintering furnace and sinters, sintering temperature is 1070 DEG C, and carries out insulation 200 minutes, then the pressed compact after sintering is cooled to 300 DEG C in vacuum sintering furnace, be warming up to 900 DEG C again and carry out insulation 90 minutes, again be cooled to 300 DEG C, be warming up to 530 DEG C and carrying out insulation 200 minutes, namely rare earth permanent-magnetic material base substrate is obtained, finally carry out machining cutting to permanent-magnet material base substrate according to the actual requirements and refine, reserved size of carrying out electroplating, obtains rare earth permanent-magnetic material simultaneously, its performance test data is see table 1-2.
Wherein, Br is remanent magnetism, and Hcb is coercivity, and (B.H) max is magnetic energy product, and MPa is bending strength.
Table 1-2 embodiment 1 properties of product test chart
| Project | Br/kGs | Hcb/KOe | MPa | (B.H)max/MGOe |
| Test value | 13.9 | 10.4 | 458 | 54 |
Embodiment 2
A kind of rare earth permanent-magnetic material, prepare burden by such as following table 2-1:
Table 2-1 embodiment 2 formula table
| Component | Neodymium | Praseodymium | Cerium | Yttrium | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 3.8 | 2.5 | 0.17 | 0.15 | 0.2 | 0.02 | 0.04 | 14.1 | 20.98 |
| Mass percent/% | 18 | 12 | 0.8 | 0.7 | 1 | 0.1 | 0.2 | 67.2 | 100 |
The preparation method of the above-mentioned rare earth permanent-magnetic material of the present embodiment is as follows:
The criteria for classification that the waste and old magnet steel collected is classified as a class according to the waste and old magnet steel identical with rare earth element contained by batch same model is presorted, obtains pretreatment magnet material; Then according to the rare earth permanent-magnetic material of preparation, the broken powder process of hydrogen is directly carried out to the pretreatment magnet material obtained, obtains the broken magnetic of rare earth hydrogen; Sample analysis is carried out to the broken magnetic of rare earth hydrogen obtained simultaneously, obtain rare-earth magnetic component parameter, again according to analyzing the rare-earth magnetic component parameter obtained, in the broken magnetic of rare earth hydrogen obtained, add liquid phase cerium obtain mixed powder, finally broken by hydrogen for the mixed powder of acquisition, airflow milling are broken into fine powder, and put into quantitative air when carrying out airflow milling and carry out passivation, and mix and blend is carried out to the powder that front and back grind, the particle mean size of fine powder is 2.5 μm; Successively fine powder is added isostatic pressing method by mold pressing and be pressed into pressed compact, and the pressure of isostatic pressed is 240MPa, green density is 4.4g/cm
3; After treating that fine powder is all suppressed, pressed compact is placed in vacuum sintering furnace and sinters, sintering temperature is 1080 DEG C, and carries out insulation 200 minutes; Then the pressed compact after sintering is cooled to 310 DEG C in vacuum sintering furnace, be warming up to 900 DEG C again and carry out insulation 90 minutes, again be cooled to 310 DEG C, be warming up to 550 DEG C and carrying out insulation 200 minutes, namely rare earth permanent-magnetic material base substrate is obtained, finally carry out machining cutting to rare earth permanent-magnetic material base substrate according to the actual requirements and refine, reserved size of carrying out electroplating, obtains rare earth permanent-magnetic material simultaneously; Its performance test data is see table 2-2.
Table 2-2 embodiment 2 properties of product test chart
| Project | Br/kGs | Hcb/KOe | MPa | (B.H)max/MGOe |
| Test value | 14.3 | 10.7 | 490 | 54 |
Embodiment 3
A kind of rare earth permanent-magnetic material, prepare burden by such as following table 3-1:
Table 3-1 embodiment 3 formula table
| Component | Neodymium | Praseodymium | Cerium | Yttrium | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 2.7 | 2.1 | 0.25 | 0.25 | 0.5 | 0.04 | 0.1 | 15.3 | 21.24 |
| Mass percent/% | 13 | 10 | 1.2 | 1.2 | 1.1 | 0.2 | 0.5 | 72.8 | 100 |
The preparation method of the above-mentioned rare earth permanent-magnetic material of the present embodiment is as follows:
The criteria for classification that the waste and old magnet steel collected is classified as a class according to the waste and old magnet steel identical with rare earth element contained by batch same model is presorted, obtains pretreatment magnet material; Then according to the rare earth permanent-magnetic material of preparation, the broken powder process of hydrogen is directly carried out to the pretreatment magnet material obtained, obtains the broken magnetic of rare earth hydrogen; Sample analysis is carried out to the broken magnetic of rare earth hydrogen obtained simultaneously, obtain rare-earth magnetic component parameter, again according to analyzing the rare-earth magnetic component parameter obtained, in the broken magnetic of rare earth hydrogen obtained, add liquid phase cerium obtain mixed powder, finally broken by hydrogen for the mixed powder of acquisition, airflow milling are broken into fine powder, and put into quantitative air when carrying out airflow milling and carry out passivation, and mix and blend is carried out to the powder that front and back grind, the particle mean size of fine powder is 2.6 μm; Successively fine powder is added isostatic pressing method by mold pressing and be pressed into pressed compact, and the pressure of isostatic pressed is 250MPa, green density is 4.4g/cm
3; After treating that fine powder is all suppressed, pressed compact is placed in vacuum sintering furnace and sinters, sintering temperature is 1085 DEG C, and carries out insulation 200 minutes; Then the pressed compact after sintering is cooled to 320 DEG C in vacuum sintering furnace, be warming up to 910 DEG C again and carry out insulation 90 minutes, again be cooled to 320 DEG C, be warming up to 570 DEG C and carrying out insulation 200 minutes, namely rare earth permanent-magnetic material base substrate is obtained, finally carry out machining cutting to rare earth permanent-magnetic material base substrate according to the actual requirements and refine, reserved size of carrying out electroplating, obtains rare earth permanent-magnetic material simultaneously; Its performance test data is see table 3-2.
Table 3-2 embodiment 3 properties of product test chart
| Project | Br/kGs | Hcb/KOe | MPa | (B.H)max/MGOe |
| Test value | 14.5 | 11.2 | 530 | 54 |
Embodiment 4
A kind of rare earth permanent-magnetic material, prepare burden by such as following table 4-1:
Table 4-1 embodiment 4 formula table
| Component | Neodymium | Praseodymium | Cerium | Yttrium | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 2.1 | 1.7 | 0.3 | 2.94 | 0.6 | 0.04 | 0.2 | 16.2 | 24.08 |
| Mass percent/% | 10 | 8 | 1.5 | 1.4 | 1.2 | 0.2 | 0.6 | 77.1 | 100 |
The preparation method of the above-mentioned rare earth permanent-magnetic material of the present embodiment is as follows:
The criteria for classification that the waste and old magnet steel collected is classified as a class according to the waste and old magnet steel identical with rare earth element contained by batch same model is presorted, obtains pretreatment magnet material; Then according to the rare earth permanent-magnetic material of preparation, the broken powder process of hydrogen is directly carried out to the pretreatment magnet material obtained, obtains the broken magnetic of rare earth hydrogen; Sample analysis is carried out to the broken magnetic of rare earth hydrogen obtained simultaneously, obtain rare-earth magnetic component parameter, again according to analyzing the rare-earth magnetic component parameter obtained, in the broken magnetic of rare earth hydrogen obtained, add liquid phase cerium obtain mixed powder, finally broken by hydrogen for the mixed powder of acquisition, airflow milling are broken into fine powder, and put into quantitative air when carrying out airflow milling and carry out passivation, and mix and blend is carried out to the powder that front and back grind, the particle mean size of fine powder is 2.8 μm; Successively fine powder is added isostatic pressing method by mold pressing and be pressed into pressed compact, and the pressure of isostatic pressed is 240MPa, green density is 4.5g/cm
3; After treating that fine powder is all suppressed, pressed compact is placed in vacuum sintering furnace and sinters, sintering temperature is 1090 DEG C, and carries out insulation 200 minutes; Then the pressed compact after sintering is cooled to 330 DEG C in vacuum sintering furnace, be warming up to 915 DEG C again and carry out insulation 90 minutes, again be cooled to 330 DEG C, be warming up to 590 DEG C and carrying out insulation 200 minutes, namely rare earth permanent-magnetic material base substrate is obtained, finally carry out machining cutting to rare earth permanent-magnetic material base substrate according to the actual requirements and refine, reserved size of carrying out electroplating, obtains rare earth permanent-magnetic material simultaneously; Its performance test data is see table 4-2.
Table 4-2 embodiment 4 properties of product test chart
| Project | Br/kGs | Hcb/KOe | MPa | (B.H)max/MGOe |
| Test value | 14.6 | 10.7 | 570 | 53 |
Embodiment 5
A kind of rare earth permanent-magnetic material, prepare burden by such as following table 5-1:
Table 5-1 embodiment 5 formula table
| Component | Neodymium | Praseodymium | Cerium | Yttrium | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 2.1 | 1.7 | 0.4 | 0.59 | 0.6 | 0.04 | 0.2 | 15.8 | 21.43 |
| Mass percent/% | 10 | 8 | 1.8 | 2.8 | 1.2 | 0.2 | 0.8 | 75.2 | 100 |
The preparation method of the above-mentioned rare earth permanent-magnetic material of the present embodiment is as follows:
The criteria for classification that the waste and old magnet steel collected is classified as a class according to the waste and old magnet steel identical with rare earth element contained by batch same model is presorted, obtains pretreatment magnet material, then according to the rare earth permanent-magnetic material of preparation, the broken powder process of hydrogen is directly carried out to the pretreatment magnet material obtained, obtains the broken magnetic of rare earth hydrogen, sample analysis is carried out to the broken magnetic of rare earth hydrogen obtained simultaneously, obtain rare-earth magnetic component parameter, again according to analyzing the rare-earth magnetic component parameter obtained, in the broken magnetic of rare earth hydrogen obtained, add liquid phase cerium obtain mixed powder, finally by broken by hydrogen for the mixed powder obtained, airflow milling is broken into fine powder, and put into quantitative air when carrying out airflow milling and carry out passivation, and mix and blend is carried out to the powder that front and back grind, the particle mean size of fine powder is 3.0 μm, simultaneously can per sample in rare earth component comparison value, appropriate rare earth component is added to satisfy the demands for the rare earth permanent-magnetic material rare earth component of required preparation and proportion requirement, and put into quantitative air when carrying out airflow milling and carry out passivation, and mix and blend is carried out to the powder that front and back grind, successively fine powder is added isostatic pressing method by mold pressing and be pressed into pressed compact, and the pressure of isostatic pressed is 270MPa, green density is 4.5g/cm
3, after treating that fine powder is all suppressed, pressed compact is placed in vacuum sintering furnace and sinters, sintering temperature is 1095 DEG C, and carries out insulation 200 minutes, then the pressed compact after sintering is cooled to 350 DEG C in vacuum sintering furnace, be warming up to 920 DEG C again and carry out insulation 90 minutes, again be cooled to 350 DEG C, be warming up to 600 DEG C and carrying out insulation 200 minutes, namely rare earth permanent-magnetic material base substrate is obtained, finally carry out machining cutting to rare earth permanent-magnetic material base substrate according to the actual requirements and refine, reserved size of carrying out electroplating, obtains rare earth permanent-magnetic material simultaneously, its performance test data is see table 5-2.
Table 5-2 embodiment 5 properties of product test chart
| Project | Br/kGs | Hcb/KOe | MPa | (B.H)max/MGOe |
| Test value | 14.3 | 10.8 | 614 | 52 |
More than show and describe general principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (7)
1. in waste and old magnet steel, add the method that liquid phase cerium prepares rare earth permanent-magnetic material, it is characterized in that, concrete steps are as follows:
1) presorted according to rare earth element contained in magnet steel by the waste and old magnet steel collected, the standard of presorting is classified as a class for the waste and old magnet steel identical with rare earth element contained by batch same model, obtains pretreatment magnet material;
2) according to preparation rare earth permanent-magnetic material, to step 1) in obtain pretreatment magnet material directly carry out the broken powder process of hydrogen, obtain the broken magnetic of rare earth hydrogen;
3) to step 2) in obtain the broken magnetic of rare earth hydrogen carry out sample analysis, obtain rare-earth magnetic component parameter;
4) according to step 3) in analyze the rare-earth magnetic component parameter that obtains, in the broken magnetic of rare earth hydrogen obtained, add liquid phase cerium obtain mixed powder, the percent mass proportioning of mixed powder: the broken magnetic of 98 ~ 99.5% rare earth hydrogen, 0.5 ~ 2% liquid phase cerium;
5) by step 4) in mixed powder, the airflow milling broken by hydrogen that obtain be broken into fine powder, and put into quantitative air when carrying out airflow milling and carry out passivation, and mix and blend is carried out to the powder that front and back grind;
6) by step 5) in the fine powder that obtains add isostatic pressing method by mold pressing and be pressed into pressed compact;
7) by step 6) in the pressed compact that obtains be placed in vacuum sintering furnace and sinter and be incubated;
8) by step 7) in sintering after pressed compact in vacuum sintering furnace, be cooled to 300 DEG C ~ 350 DEG C, be warming up to first paragraph heat treatment again and be incubated, then continue to be cooled to 300 DEG C ~ 350 DEG C, finally be warming up to second segment heat treatment and be incubated, and respectively tempering is carried out to two sections of heat treatments, to obtain rare earth permanent-magnetic material base substrate;
9) by step 8) the middle rare earth permanent-magnetic material base substrate obtained, carry out machining cutting according to the actual requirements and refine, reserved size of carrying out electroplating, obtains rare earth permanent-magnetic material simultaneously.
2. the method for adding liquid phase cerium and preparing rare earth permanent-magnetic material in waste and old magnet steel according to claim 1, is characterized in that, described step 5) in, fine powder particle mean size is 2.4 ~ 3.2 μm.
3. the method for adding liquid phase cerium and preparing rare earth permanent-magnetic material in waste and old magnet steel according to claim 1, is characterized in that, described step 6) in, the pressure of isostatic pressed is 230 ~ 280MPa.
4. the method for adding liquid phase cerium and preparing rare earth permanent-magnetic material in waste and old magnet steel according to claim 1, is characterized in that, described step 7) in, sintering temperature is 1070 DEG C ~ 1095 DEG C.
5. the method for adding liquid phase cerium and preparing rare earth permanent-magnetic material in waste and old magnet steel according to claim 1, is characterized in that, described step 7) in, temperature retention time is 200 minutes.
6. the method for adding liquid phase cerium and preparing rare earth permanent-magnetic material in waste and old magnet steel according to claim 1, is characterized in that, described step 8) in, first paragraph heat treatment temperature is 900 DEG C ~ 920 DEG C, and temperature retention time is 90 minutes; Second segment heat treatment temperature is 530 DEG C ~ 620 DEG C, and temperature retention time is 200 minutes.
7. according to any one of claim 1 ~ 6, add the method that liquid phase cerium prepares rare earth permanent-magnetic material in waste and old magnet steel, the rare earth permanent-magnetic material of preparation, is characterized in that, comprises neodymium, praseodymium, cerium, boron, copper, aluminium, yttrium and iron; Each constituent mass percentage is: 10 ~ 20% neodymiums, 8 ~ 15% praseodymiums, 0.5 ~ 2% cerium, 0.5 ~ 1.2% boron, 0 ~ 0.25% bronze medal, 0 ~ 0.8% aluminium, 0.2 ~ 3% yttrium, 57 ~ 81% iron, and iron is iron and inevitable impurity.
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| CN105551788A (en) * | 2016-02-02 | 2016-05-04 | 中磁科技股份有限公司 | Method for improving coercive force of rare earth permanent magnet |
| CN106971802A (en) * | 2017-04-14 | 2017-07-21 | 钢铁研究总院 | A kind of recycled sinter Nd-Fe-B permanent magnetic preparation |
| CN109087802A (en) * | 2018-07-11 | 2018-12-25 | 宁波市合美达新材料有限公司 | A kind of rare-earth permanent magnet recoverying and utilizing method |
| CN112385006A (en) * | 2018-06-18 | 2021-02-19 | Abb瑞士股份有限公司 | Method for producing magnetic powder |
| CN115376810A (en) * | 2022-09-01 | 2022-11-22 | 沭阳康顺磁性器材有限公司 | Magnetic material with high magnetic stability and production process thereof |
| CN115954202A (en) * | 2023-02-22 | 2023-04-11 | 宁波恒盛磁业有限公司 | Method for preparing neodymium-iron-boron magnet from neodymium-iron-boron reclaimed material |
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