CN105251985A - Method for preparing nano composite permanent magnet material by adding zirconium into magnetic steel waste - Google Patents
Method for preparing nano composite permanent magnet material by adding zirconium into magnetic steel waste Download PDFInfo
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Abstract
The invention relates to a method for preparing a nano composite permanent magnet material by adding zirconium into magnetic steel waste. Collected waste magnetic steel is presorted according to the classification standard that the waste magnetic steel which is in the same batch and model and is provided with same rare earth elements is classified as one class, and a pre-processed magnet material is obtained; the obtained pre-processed magnet material is directly subjected to hydrogen decrepition pulverizing, and rare earth hydrogen decrepition magnetic powder is obtained; sampling analysis is carried out on the rare earth hydrogen decrepition magnetic powder, and the zirconium is added into the rare earth hydrogen decrepition magnetic powder according to needs to obtain mixed powder; and finally through static pressing, sintering and annealing, the needed nano composite permanent magnet material is prepared. The problem of segregation, caused by factors such as different smelting pints of all compositions and the like, generated by an alloy ingot obtained after smelting can be effectively solved; and through presorting, the time for recovering the waste magnetic steel can be saved, and the process step of extraction is omitted. The zirconium is added into the rare earth hydrogen decrepition magnetic powder, the grain microstructure and the magnetic performance of the nano composite permanent magnet material can be changed, and grain refinement is promoted; and the nano composite permanent magnet material obtained through a precipitation separation method is high in performance and low in rare earth content.
Description
Technical field
The present invention relates to nano composite permanent magnetic material technical field, particularly relate to a kind of method of adding zirconium and preparing nano composite permanent magnetic material in steel refuse by magnetic.
Background technology
In recent years, along with the continuous expansion of nano composite 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 zirconium, samarium zirconium 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 nano composite 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, current nano composite permanent magnetic powder is mainly obtained by approach such as fast quenching, mechanical alloying or high-energy ball millings, but all there are some shortcomings being difficult to overcome in these methods, usually, improve the spin-exchange-coupled efficiency of nano composite permanent magnetic material, need to be optimized from two aspects, one is control soft magnetism phase size, it has been generally acknowledged that the yardstick of soft magnetism phase should be less than the twice for Hard Magnetic phase domain wall width; Two is obtain the soft magnetism that is evenly distributed to be harmonious Hard Magnetic phase.But although these methods also can regulate the micro-structural of composite, be difficult to the crystallite dimension and the distribution that accurately control Hard Magnetic phase and soft magnetism phase, be particularly difficult to the yardstick and the composition that control two kinds of phases respectively.Therefore the maximum magnetic energy product improving isotropism nano material is also difficult to.Therefore, how under the prerequisite not changing permanent-magnet material characteristic, to improve permanent-magnet material maximum magnetic energy product, become the major issue that those skilled in the art are urgently to be resolved hurrily.
Summary of the invention
Technical problem solved by the invention is to provide a kind of method of adding zirconium and preparing nano composite permanent magnetic material in steel refuse by magnetic, to solve the shortcoming in above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
In steel refuse by magnetic, add the method that zirconium prepares nano composite 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 nano composite 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 zirconium obtain mixed powder, the percent mass proportioning of mixed powder: the broken magnetic of 80 ~ 99% rare earth hydrogen, 1 ~ 20% zirconium;
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, adopt separation by precipitation to remove pressed compact again and react remaining metal nanoparticle, clean 3 ~ 5 times, ultrasonic oscillation, then dry, obtain nano permanent magnetic material base substrate;
7) by step 6) in the nano permanent magnetic material base substrate that obtains be placed in vacuum sintering furnace and sinter and be incubated;
8) by step 7) in sintering after nano permanent magnetic material base substrate in vacuum sintering furnace, be cooled to 300 DEG C ~ 360 DEG C, be warming up to first paragraph heat treatment again and be incubated, then continue to be cooled to 300 DEG C ~ 360 DEG C, finally be warming up to second segment heat treatment and be incubated, and respectively tempering is carried out, to obtain nano composite permanent magnetic material to two sections of heat treatments.
In the present invention, described step 5) in, fine powder particle mean size is 2.4 ~ 3.0 μm.
In the present invention, described step 6) in, the pressure of isostatic pressed is 230 ~ 280MPa.
In the present invention, described step 6) in, cleaning solution is alcohol, acetone and deionized water.
In the present invention, described step 6) in, dry is vacuum drying.
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 nano composite permanent magnetic material later process of the equal model of waste and old magnet steel simultaneously; Adding of zirconium is conducive to changing nano composite permanent magnetic material grain microstructure and magnetic property, promotes grain refinement, and then improves the magnetic energy product of nano composite permanent magnetic material; And the nano composite permanent magnetic material magnetic property utilizing separation by precipitation to obtain is high, content of rare earth is low.
A kind of nano composite permanent magnetic material, comprises neodymium, praseodymium, gadolinium, boron, copper, aluminium, yttrium, zirconium and iron; Each constituent mass percentage is: 10 ~ 20% neodymiums, 8 ~ 15% praseodymiums, 4 ~ 20% gadoliniums, 0.3 ~ 1.2% boron, 0 ~ 0.25% bronze medal, 0 ~ 0.8% aluminium, 0.7 ~ 3% yttrium, 1 ~ 20% zirconium, 19 ~ 76% 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 zirconium 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, adding of zirconium is conducive to changing nano composite permanent magnetic material grain microstructure and magnetic property, promote grain refinement, and then improve the magnetic energy product of nano composite permanent magnetic material; And the nano composite permanent magnetic material magnetic property utilizing separation by precipitation to obtain is high, content of rare earth is low.
Detailed description of the invention
Describe the present invention below by following specific embodiment.
Embodiment 1
| Component | Neodymium | Praseodymium | Gadolinium | Yttrium | Zirconium | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 4.2 | 3.2 | 1.1 | 0.15 | 0.21 | 0.06 | 0 | 0 | 12.1 | 21.02 |
| Mass percent/% | 20 | 15 | 5 | 0.7 | 1 | 0.3 | 0 | 0 | 58 | 100 |
A kind of nano composite permanent magnetic material, prepare burden by such as following table 1-1:
Table 1-1 embodiment 1 formula table
The preparation method of the above-mentioned nano composite 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 nano composite 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 zirconium 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, adopt separation by precipitation to remove pressed compact and react remaining metal nanoparticle, and pressed compact is cleaned 3 ~ 5 times in deionized water, ultrasonic oscillation, then vacuum drying, obtains nano permanent magnetic material base substrate, then nano permanent magnetic material base substrate is placed in vacuum sintering furnace 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, then is warming up to 900 DEG C and carries out insulation 90 minutes, be again cooled to 300 DEG C, being warming up to 530 DEG C and carrying out insulation 200 minutes, namely obtain nano composite permanent magnetic material, 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 | 14.6 | 10.4 | 454 | 84 |
Embodiment 2
A kind of nano composite permanent magnetic material, prepare burden by such as following table 2-1:
Table 2-1 embodiment 2 formula table
| Component | Neodymium | Praseodymium | Gadolinium | Yttrium | Zirconium | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 3.8 | 2.5 | 1.68 | 0.21 | 1.1 | 0.1 | 0.02 | 0.04 | 11.9 | 21.35 |
| Mass percent/% | 18 | 12 | 8 | 1 | 5 | 0.5 | 0.1 | 0.2 | 55.2 | 100 |
The preparation method of the above-mentioned nano composite 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 nano composite 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 zirconium 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, adopt separation by precipitation to remove pressed compact and react remaining metal nanoparticle, and pressed compact is cleaned 3 ~ 5 times in deionized water, ultrasonic oscillation, then vacuum drying, obtains nano permanent magnetic material base substrate, then nano permanent magnetic material base substrate is placed in vacuum sintering furnace 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, then is warming up to 900 DEG C and carries out insulation 90 minutes, be again cooled to 310 DEG C, being warming up to 550 DEG C and carrying out insulation 200 minutes, namely obtain nano composite permanent magnetic material; 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 | 14.4 | 10.5 | 487 | 90 |
Embodiment 3
A kind of nano composite permanent magnetic material, prepare burden by such as following table 3-1:
Table 3-1 embodiment 3 formula table
| Component | Neodymium | Praseodymium | Gadolinium | Yttrium | Zirconium | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 2.7 | 2.1 | 2.52 | 0.23 | 2.1 | 0.3 | 0.04 | 0.1 | 10.9 | 20.99 |
| Mass percent/% | 13 | 10 | 12 | 1.1 | 10 | 1.2 | 0.2 | 0.5 | 52 | 100 |
The preparation method of the above-mentioned nano composite 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 nano composite 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 zirconium 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, adopt separation by precipitation to remove pressed compact and react remaining metal nanoparticle, and pressed compact is cleaned 3 ~ 5 times in deionized water, ultrasonic oscillation, then vacuum drying, obtains nano permanent magnetic material base substrate, then nano permanent magnetic material base substrate is placed in vacuum sintering furnace 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, then is warming up to 910 DEG C and carries out insulation 90 minutes, be again cooled to 320 DEG C, being warming up to 570 DEG C and carrying out insulation 200 minutes, namely obtain nano composite permanent magnetic material; 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 | 101 |
Embodiment 4
A kind of nano composite permanent magnetic material, prepare burden by such as following table 4-1:
Table 4-1 embodiment 4 formula table
| Component | Neodymium | Praseodymium | Gadolinium | Yttrium | Zirconium | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 2.1 | 1.7 | 2.1 | 0.42 | 3.15 | 0.4 | 0.04 | 0.2 | 11.1 | 21.21 |
| Mass percent/% | 10 | 8 | 10 | 2 | 15 | 1.2 | 0.2 | 0.6 | 53 | 100 |
The preparation method of the above-mentioned nano composite 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 nano composite 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 zirconium 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, adopt separation by precipitation to remove pressed compact and react remaining metal nanoparticle, and pressed compact is cleaned 3 ~ 5 times in deionized water, ultrasonic oscillation, then vacuum drying, obtains nano permanent magnetic material base substrate, then nano permanent magnetic material base substrate is placed in vacuum sintering furnace 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, then is warming up to 915 DEG C and carries out insulation 90 minutes, be again cooled to 330 DEG C, being warming up to 590 DEG C and carrying out insulation 200 minutes, namely obtain nano composite permanent magnetic material; 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 | 11.3 | 552 | 94 |
Embodiment 5
A kind of nano composite permanent magnetic material, prepare burden by such as following table 5-1:
Table 5-1 embodiment 5 formula table
| Component | Neodymium | Praseodymium | Gadolinium | Yttrium | Zirconium | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 2.1 | 1.7 | 3.2 | 0.59 | 4.2 | 0.6 | 0.04 | 0.2 | 8.8 | 21.43 |
| Mass percent/% | 10 | 8 | 15 | 2.8 | 20 | 1.2 | 0.2 | 0.8 | 42 | 100 |
The preparation method of the above-mentioned nano composite 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 nano composite 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 zirconium 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 nano composite 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, adopt separation by precipitation to remove pressed compact and react remaining metal nanoparticle, and pressed compact is cleaned 3 ~ 5 times in deionized water, ultrasonic oscillation, then vacuum drying, obtains nano permanent magnetic material base substrate, then nano permanent magnetic material base substrate is placed in vacuum sintering furnace 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, then is warming up to 920 DEG C and carries out insulation 90 minutes, be again cooled to 350 DEG C, being warming up to 600 DEG C and carrying out insulation 200 minutes, namely obtain nano composite permanent magnetic material, 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 | 624 | 89 |
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 (9)
1. in steel refuse by magnetic, add the method that zirconium prepares nano composite 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 nano composite 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 zirconium obtain mixed powder, the percent mass proportioning of mixed powder: the broken magnetic of 80 ~ 99% rare earth hydrogen, 1 ~ 20% zirconium;
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, adopt separation by precipitation to remove pressed compact again and react remaining metal nanoparticle, clean 3 ~ 5 times, ultrasonic oscillation, then dry, obtain nano permanent magnetic material base substrate;
7) by step 6) in the nano permanent magnetic material base substrate that obtains be placed in vacuum sintering furnace and sinter and be incubated;
8) by step 7) in sintering after nano permanent magnetic material base substrate in vacuum sintering furnace, be cooled to 300 DEG C ~ 360 DEG C, be warming up to first paragraph heat treatment again and be incubated, then continue to be cooled to 300 DEG C ~ 360 DEG C, finally be warming up to second segment heat treatment and be incubated, and respectively tempering is carried out, to obtain nano composite permanent magnetic material to two sections of heat treatments.
2. the method for adding zirconium and preparing nano composite permanent magnetic material in steel refuse by magnetic according to claim 1, is characterized in that, described step 5) in, fine powder particle mean size is 2.4 ~ 3.0 μm.
3. the method for adding zirconium and preparing nano composite permanent magnetic material in steel refuse by magnetic 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 zirconium and preparing nano composite permanent magnetic material in steel refuse by magnetic according to claim 1, is characterized in that, described step 6) in, cleaning solution is alcohol, acetone and deionized water.
5. the method for adding zirconium and preparing nano composite permanent magnetic material in steel refuse by magnetic according to claim 1, is characterized in that, described step 6) in, dry is vacuum drying.
6. the method for adding zirconium and preparing nano composite permanent magnetic material in steel refuse by magnetic according to claim 1, is characterized in that, described step 7) in, sintering temperature is 1070 DEG C ~ 1095 DEG C.
7. the method for adding zirconium and preparing nano composite permanent magnetic material in steel refuse by magnetic according to claim 1, is characterized in that, described step 7) in, temperature retention time is 200 minutes.
8. the method for adding zirconium and preparing nano composite permanent magnetic material in steel refuse by magnetic 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.
9. according to any one of claim 1 ~ 8, add the method that zirconium prepares nano composite permanent magnetic material in steel refuse by magnetic, the nano composite permanent magnetic material of preparation, is characterized in that, comprises neodymium, praseodymium, gadolinium, boron, copper, aluminium, yttrium, zirconium and iron; Each constituent mass percentage is: 10 ~ 20% neodymiums, 8 ~ 15% praseodymiums, 4 ~ 20% gadoliniums, 0.3 ~ 1.2% boron, 0 ~ 0.25% bronze medal, 0 ~ 0.8% aluminium, 0.7 ~ 3% yttrium, 1 ~ 20% zirconium, 19 ~ 76% iron, and iron is iron and inevitable impurity.
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| CN113948263A (en) * | 2021-10-08 | 2022-01-18 | 宁波市合美达新材料有限公司 | Neodymium iron boron material and preparation method thereof |
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| KR100516512B1 (en) * | 2003-10-15 | 2005-09-26 | 자화전자 주식회사 | The making method of high coercive micro-structured powder for bonded magnets and The magnet powder thereof |
| CN103866127A (en) * | 2014-02-27 | 2014-06-18 | 中铝广西有色金源稀土股份有限公司 | Method for preparing neodymium iron boron through regenerating waste material containing neodymium, iron and boron |
| CN104190943A (en) * | 2014-08-04 | 2014-12-10 | 中磁科技股份有限公司 | Method for recycling sintered neodymium-iron-boron waste materials |
| CN104393691A (en) * | 2014-10-30 | 2015-03-04 | 浙江鑫盛永磁科技有限公司 | Magnetic steel specialized for pure electric automobile drive motor and preparation method thereof |
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| CN113948263A (en) * | 2021-10-08 | 2022-01-18 | 宁波市合美达新材料有限公司 | Neodymium iron boron material and preparation method thereof |
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