CN105251987A - Method for preparing dysprosium-contained rare earth permanent magnetic material by adding nanocrystalline metal powder in magnetic steel waste - Google Patents
Method for preparing dysprosium-contained rare earth permanent magnetic material by adding nanocrystalline metal powder in magnetic steel waste Download PDFInfo
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 111
- 239000000696 magnetic material Substances 0.000 title claims abstract description 65
- 239000000843 powder Substances 0.000 title claims abstract description 61
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 52
- 239000010959 steel Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 37
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 35
- 239000002699 waste material Substances 0.000 title claims abstract description 34
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 31
- 239000002184 metal Substances 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 61
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 32
- 239000000956 alloy Substances 0.000 claims abstract description 32
- 238000005245 sintering Methods 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000005520 cutting process Methods 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- 238000003754 machining Methods 0.000 claims abstract description 8
- -1 dysprosium rare earth Chemical class 0.000 claims description 64
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 61
- 238000002844 melting Methods 0.000 claims description 30
- 230000008018 melting Effects 0.000 claims description 30
- 238000002360 preparation method Methods 0.000 claims description 29
- 229910052693 Europium Inorganic materials 0.000 claims description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 18
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical group [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 18
- 229910000838 Al alloy Inorganic materials 0.000 claims description 15
- 238000003801 milling Methods 0.000 claims description 14
- 239000000758 substrate Substances 0.000 claims description 14
- 238000010792 warming Methods 0.000 claims description 14
- 238000003723 Smelting Methods 0.000 claims description 9
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims description 9
- 238000009713 electroplating Methods 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 229910052771 Terbium Inorganic materials 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- 239000004411 aluminium Substances 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 238000001514 detection method Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims description 8
- 238000000462 isostatic pressing Methods 0.000 claims description 7
- 239000002105 nanoparticle Substances 0.000 claims description 7
- 238000002161 passivation Methods 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- 230000014759 maintenance of location Effects 0.000 claims description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 5
- 229910052779 Neodymium Inorganic materials 0.000 claims description 5
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 5
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 5
- 229910000906 Bronze Inorganic materials 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052689 Holmium Inorganic materials 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 239000010974 bronze Substances 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 238000005496 tempering Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 abstract description 2
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- 230000003213 activating effect Effects 0.000 abstract 1
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- 229910001172 neodymium magnet Inorganic materials 0.000 description 3
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- 230000009467 reduction Effects 0.000 description 3
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 2
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- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
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- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The invention relates to a method for preparing a dysprosium-contained rare earth permanent magnetic material by adding nanocrystalline metal powder in 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 provided with same rear earth elements are classified as one class to obtain a preprocessed magnet material; the obtained pre-processed magnet material and the well prepared nanocrystalline metal powder are put into a common electrolytic furnace to be smelted to form molten alloy liquid; the molten alloy liquid is cast and cooled to form an alloy ingot, and the alloy ingot is subjected to hydrogen decrepition and airflow abrasion to be smashed into fine powder; the fine powder is subjected to static pressure, sintering and two-section heat treatment to obtain a dysprosium-contained rare earth permanent magnetic material; and finally, according to the actual requirements, machining for cutting and accurate grinding is carried out, and then the dysprosium-contained rare earth permanent magnetic material is obtained. Through adding of the nanocrystalline metal powder, the fluorescent lifetime of the dysprosium-contained rare earth permanent magnetic material is effectively prolonged, and the dysprosium-contained rare earth permanent magnetic material has the higher activating agent critical concentration; and through presorting, the time for recovering the waste magnetic steel can be saved, and the process step of extraction is omitted.
Description
Technical field
The present invention relates to rare-earth permanent-magnet material technical field, particularly relate to a kind of method of adding Nano metal powder preparation and containing dysprosium rare earth permanent-magnetic material in steel refuse by magnetic.
Background technology
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, and also often cause occurring badly scrapping 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 alloy permanent-magnet material of required preparation again.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 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.For neodymium iron boron, vacuum melting furnace melting is added into by after the praseodymium gone out through extract and separate, neodymium and iron, boron and the mixing of other compositions, alloy pig is obtained after melting, fusing point in the process because of each composition is different, and be subject to front road mix and blend whether evenly and the factor such as the control of artificial time interval of adding and amount affect, the alloy pig material segregation after melting certainly will be caused, even affect performance and the subsequent technique effect of alloy pig material, simultaneously higher to the technical requirement of operating personnel in process of production, hand labor intensity is large; 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.
Along with the develop rapidly of science and technology, increasing new technology is used in prepares permanent-magnet material field, particularly applications to nanostructures, nano material particle has quantum size effect, skin effect and macro quanta tunnel effect, by the impact of these architectural characteristics, nano material is used in other field and shows peculiar physics and chemistry characteristic, and spectrum and fluorescence property are wherein very important aspects, nano material fluorescence properties a large amount of is at present relevant with semi-conducting material, and the important component part of semi-conducting material is permanent-magnet material; Therefore, under the prerequisite not changing permanent-magnet material characteristic, how to improve the actual coercivity of permanent-magnet material, and by Application of micron in permanent-magnet material field, to improve permanent-magnet material in spectrum and fluorescence, avoid alloy pig material during follow-up melting to produce segregation, and the use cost reducing raw material has become those skilled in the art's major issue urgently to be resolved hurrily simultaneously.
Summary of the invention
Technical problem solved by the invention is that provide a kind of adds the method for Nano metal powder preparation containing dysprosium rare earth permanent-magnetic material, to solve the shortcoming in above-mentioned background technology in steel refuse by magnetic.
Technical problem solved by the invention realizes by the following technical solutions:
In steel refuse by magnetic, add the method for Nano metal powder preparation containing dysprosium rare earth permanent-magnetic material, its concrete steps are as follows:
1) the waste and old magnet steel collected is presorted according to rare earth element contained in magnet steel, the standard of the presorting waste and old magnet steel that rare earth element is identical contained by same batch same model is classified as a class, obtain pretreatment magnet material, pretreatment magnet material comprises neodymium, praseodymium, dysprosium and terbium, from pretreatment magnet material, extract sample simultaneously, and detection record is carried out as comparison value to the rare earth component in sample;
2) by step 1) in the pretreatment magnet material obtained and the Nano metal powder to have prepared, according to percent mass proportioning: 95 ~ 97% pretreatment magnet materials, 3 ~ 5% Nano metal powders, obtain mixing match material, making it form the aluminium alloy of melting by carrying out melting in mixing match material input general electrolytic stove simultaneously, then the aluminium alloy of melting being cast and being cooled to alloy pig;
3) by step 2) in alloy pig, 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;
4) by step 3) in the fine powder that obtains add isostatic pressing method by mold pressing and be pressed into pressed compact;
5) by step 4) in the pressed compact that obtains be placed in vacuum sintering furnace and sinter and be incubated;
6) by step 5) 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 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 containing dysprosium rare earth permanent-magnetic material base substrate;
7) by step 6) in obtain containing dysprosium rare earth permanent-magnetic material base substrate, carry out machining cutting according to the actual requirements and refine, reserved size of carrying out electroplating, obtains containing dysprosium rare earth permanent-magnetic material simultaneously.
In the present invention, described step 2) in, smelting temperature is 1495 DEG C ~ 1550 DEG C.
In the present invention, described step 2) in, Nano metal powder is europium nanoparticle, and by adding europium nanoparticle in pretreatment magnet material, the dysprosium element of europium nanoparticle in pretreatment magnet material is combined and generates nanometer Y
2o
3: Eu
3+through carrying out fluorometric investigation to it, when aluminium: time europium=10:1 (mol ratio), there is best green glow and strengthen effect, when aluminium: during europium=50:1, luminous intensity is the strongest, and the interpolation of europium nanoparticle changes permanent-magnet material rare earth elements dot matrix case, effectively enhance the fluorescence lifetime containing dysprosium rare earth permanent-magnetic material, and make, containing dysprosium rare earth permanent-magnetic material, there is higher critical concentration.
In the present invention, described step 2) in, to produce alloy pig detect, and with step 1) in sample rare earth component comparison value compare, when not being inconsistent with comparison value, again allocating containing holmium rare earth permanent-magnetic material component according to required preparation.
In the present invention, described step 3) in, fine powder particle mean size is 2.4 ~ 2.8 μm.
In the present invention, described step 4) in, the pressure of isostatic pressed is 230 ~ 280MPa.
In the present invention, described step 5) in, sintering temperature is 1070 DEG C ~ 1095 DEG C.
In the present invention, described step 5) in, temperature retention time is 180 minutes.
In the present invention, described step 6) 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 180 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 permanent-magnet material later process of the equal model of waste and old magnet steel simultaneously.
In the present invention, dysprosium adds the actual coercivity being conducive to improving alloy pig, and its permanent-magnet material product prepared is more superior in corrosion resistance, heat endurance, processing characteristics etc.; By by pretreatment magnet material and the Nano metal powder molten alloy ingot prepared, no longer need vacuum reduction smelting furnace, effectively reduce the production cost of enterprise; The interpolation of terbium can improve containing dysprosium rare earth permanent-magnetic material as the activation performance preparing fluorescence raw material, and under excited state, fluorescent material evenly can send green light.
A kind of containing dysprosium rare earth permanent-magnetic material, comprise neodymium, praseodymium, dysprosium, boron, copper, aluminium, terbium, iron and Nano metal powder; Each constituent mass percentage is: 7 ~ 15% neodymiums, 4 ~ 10% praseodymiums, 3 ~ 15% dysprosiums, 0.8 ~ 1.2% boron, 0 ~ 0.25% bronze medal, 0.3 ~ 6% aluminium, 0.1 ~ 3% terbium, 45 ~ 82% iron, 3 ~ 5% Nano metal powders, and iron is iron and inevitable impurity.
Beneficial effect: the waste and old magnet steel collected is presorted according to rare earth element contained in magnet steel by the present invention, 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, also provide convenient for producing with the permanent-magnet material later process of the equal model of waste and old magnet steel simultaneously; And pass through pretreatment magnet material and the Nano metal powder molten alloy ingot prepared, no longer need vacuum reduction smelting furnace, 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, dysprosium adds the actual coercivity being conducive to improving alloy pig, the interpolation of terbium and Nano metal powder, effectively enhance containing dysprosium rare earth permanent-magnetic material fluorescence lifetime, and make, containing dysprosium rare earth permanent-magnetic material, there is higher critical concentration.
Detailed description of the invention
Describe the present invention below by following specific embodiment.
Embodiment 1
A kind of containing dysprosium rare earth permanent-magnetic material, prepare burden by such as following table 1-1:
Table 1-1 embodiment 1 formula table
| Component | Neodymium | Praseodymium | Dysprosium | Terbium | Boron | Copper | Aluminium | Iron | Europium | Add up to |
| Weight/kg | 3.1 | 2.1 | 0.6 | 0.1 | 0.2 | 0.0 | 0.06 | 14 | 0.8 | 20.96 |
| Mass percent/% | 15 | 10 | 3 | 0.1 | 0.8 | 0 | 0.3 | 67 | 3.8 | 100 |
The above-mentioned preparation method containing dysprosium 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, obtain pretreatment magnet material, from pretreatment magnet material, extract sample simultaneously, and detection record is carried out as comparison value to the rare earth component in sample, again the pretreatment magnet material of acquisition and the europium particulate to have prepared are dropped in general electrolytic stove and carry out melting and make it form the aluminium alloy of melting, smelting temperature is 1495 DEG C, then the aluminium alloy of melting cast and be cooled to alloy pig, broken by hydrogen, alloy pig is broken into the fine powder that particle mean size is 2.4 μm by airflow milling, 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 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 180 minutes, then the pressed compact after sintering is cooled to 300 DEG C in vacuum sintering furnace, be warming up to 900 DEG C and carrying out insulation 90 minutes, again be cooled to 300 DEG C, be warming up to 530 DEG C and carrying out insulation 180 minutes, namely obtain containing dysprosium rare earth permanent-magnetic material base substrate, finally carry out machining cutting to containing dysprosium rare earth permanent-magnetic material base substrate and refine according to the actual requirements, reserved size of carrying out electroplating, obtains containing dysprosium 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 MPa is bending strength, and CD is luminous intensity, and (B.H) max is magnetic energy product.
Table 1-2 embodiment 1 properties of product test chart
| Project | Br/kGs | Hcb/KOe | MPa | CD | (B.H)max/MGOe |
| Test value | 14.6 | 11.2 | 460 | 850 | 54 |
Embodiment 2
A kind of containing dysprosium rare earth permanent-magnetic material, prepare burden by such as following table 2-1:
| Component | Neodymium | Praseodymium | Dysprosium | Terbium | Boron | Copper | Aluminium | Iron | Europium | Add up to |
| Weight/kg | 2.5 | 1.7 | 1.1 | 0.1 | 0.3 | 0.02 | 1 | 13 | 0.8 | 20.52 |
| Mass percent/% | 12 | 8 | 5 | 0.1 | 0.9 | 0.1 | 5 | 65 | 3.9 | 100 |
Table 2-1 embodiment 2 formula table
The above-mentioned preparation method containing dysprosium 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, obtain pretreatment magnet material, simultaneously from pretreatment magnet material, extract sample, and detection record is carried out to the rare earth component in sample be worth as a comparison, again the pretreatment magnet material of acquisition and the europium particulate to have prepared are dropped in general electrolytic stove and carry out melting and make it form the aluminium alloy of melting, smelting temperature is 1500 DEG C, then the aluminium alloy of melting cast and be cooled to alloy pig, broken by hydrogen, alloy pig is broken into the fine powder that particle mean size is 2.4 μm by airflow milling, 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 240MPa, 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 1080 DEG C, and carries out insulation 180 minutes, then the pressed compact after sintering is cooled to 310 DEG C in vacuum sintering furnace, be warming up to 910 DEG C and carrying out insulation 90 minutes, again be cooled to 310 DEG C, be warming up to 550 DEG C and carrying out insulation 180 minutes, namely obtain containing dysprosium rare earth permanent-magnetic material base substrate, finally carry out machining cutting to containing dysprosium rare earth permanent-magnetic material base substrate and refine according to the actual requirements, reserved size of carrying out electroplating, obtains containing dysprosium 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 | CD | (B.H)max/MGOe |
| Test value | 14.3 | 11.6 | 490 | 1180 | 54 |
Embodiment 3
A kind of containing dysprosium rare earth permanent-magnetic material, prepare burden by such as following table 3-1:
| Component | Neodymium | Praseodymium | Dysprosium | Terbium | Boron | Copper | Aluminium | Iron | Europium | Add up to |
| Weight/kg | 2.1 | 1.3 | 1.4 | 0.3 | 0.4 | 0.04 | 0.3 | 14 | 0.9 | 20.74 |
| Mass percent/% | 10 | 6 | 7 | 1 | 1 | 0.2 | 1.5 | 69 | 4.3 | 100 |
Table 3-1 embodiment 3 formula table
The above-mentioned preparation method containing dysprosium 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, obtain pretreatment magnet material, simultaneously from pretreatment magnet material, extract sample, and detection record is carried out to the rare earth component in sample be worth as a comparison, again the pretreatment magnet material of acquisition and the europium particulate to have prepared are dropped in general electrolytic stove and carry out melting and make it form the aluminium alloy of melting, smelting temperature is 1520 DEG C, then the aluminium alloy of melting cast and be cooled to alloy pig, broken by hydrogen, alloy pig is broken into the fine powder that particle mean size is 2.5 μm by airflow milling, 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 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 180 minutes, then the pressed compact after sintering is cooled to 320 DEG C in vacuum sintering furnace, be warming up to 915 DEG C and carrying out insulation 90 minutes, again be cooled to 320 DEG C, be warming up to 570 DEG C and carrying out insulation 180 minutes, namely obtain containing dysprosium rare earth permanent-magnetic material base substrate, finally carry out machining cutting to containing dysprosium rare earth permanent-magnetic material base substrate and refine according to the actual requirements, reserved size of carrying out electroplating, obtains containing dysprosium 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 | CD | (B.H)max/MGOe |
| Test value | 14.4 | 11.7 | 500 | 870 | 53 |
Embodiment 4
A kind of containing dysprosium rare earth permanent-magnetic material, prepare burden by such as following table 4-1:
| Component | Neodymium | Praseodymium | Dysprosium | Terbium | Boron | Copper | Aluminium | Iron | Europium | Add up to |
| Weight/kg | 2.1 | 1.3 | 1.4 | 0.1 | 0.4 | 0.04 | 0.84 | 14 | 1.0 | 21.18 |
| Mass percent/% | 8 | 5 | 9 | 0.4 | 1.1 | 0.1 | 4 | 68 | 4.4 | 100 |
Table 4-1 embodiment 4 formula table
The above-mentioned preparation method containing dysprosium 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, obtain pretreatment magnet material, from pretreatment magnet material, extract sample simultaneously, and detection record is carried out to the rare earth component in sample, again the pretreatment magnet material of acquisition and the europium particulate to have prepared are dropped in general electrolytic stove and carry out melting and make it form the aluminium alloy of melting, smelting temperature is 1540 DEG C, then the aluminium alloy of melting cast and be cooled to alloy pig, broken by hydrogen, alloy pig is broken into the fine powder that particle mean size is 2.5 μm by airflow milling, simultaneously can per sample in rare earth component carry out detection record, appropriate rare earth component is added to satisfy the demands for the permanent-magnet 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 260MPa, 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 180 minutes, then the pressed compact after sintering is cooled to 340 DEG C in vacuum sintering furnace, be warming up to 915 DEG C and carrying out insulation 90 minutes, again be cooled to 340 DEG C, be warming up to 600 DEG C and carrying out insulation 180 minutes, namely obtain containing dysprosium rare earth permanent-magnetic material base substrate, finally carry out machining cutting to containing dysprosium rare earth permanent-magnetic material base substrate and refine according to the actual requirements, reserved size of carrying out electroplating, obtains containing dysprosium 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 | CD | (B.H)max/MGOe |
| Test value | 14.7 | 10.9 | 580 | 992 | 52 |
Embodiment 5
A kind of containing dysprosium rare earth permanent-magnetic material, prepare burden by such as following table 5-1:
Table 5-1 embodiment 5 formula table
| Component | Neodymium | Praseodymium | Dysprosium | Terbium | Boron | Copper | Aluminium | Iron | Europium | Add up to |
| Weight/kg | 1.5 | 0.9 | 2.0 | 0.7 | 0.6 | 0.04 | 0.06 | 12 | 1.0 | 18.8 |
| Mass percent/% | 7 | 4 | 12 | 3 | 1.2 | 0.2 | 5 | 63 | 4.6 | 100 |
The above-mentioned preparation method containing dysprosium 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, obtain pretreatment magnet material, simultaneously from pretreatment magnet material, extract sample, and detection record is carried out to the rare earth component in sample be worth as a comparison, again the pretreatment magnet material of acquisition and the europium particulate to have prepared are dropped in general electrolytic stove and carry out melting and make it form the aluminium alloy of melting, smelting temperature is 1550 DEG C, then the aluminium alloy of melting cast and be cooled to alloy pig, broken by hydrogen, alloy pig is broken into the fine powder that particle mean size is 2.6 μm by airflow milling, 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 1090 DEG C, and carries out insulation 180 minutes, then the pressed compact after sintering is cooled to 350 DEG C in vacuum sintering furnace, be warming up to 915 DEG C and carrying out insulation 90 minutes, again be cooled to 350 DEG C, be warming up to 610 DEG C and carrying out insulation 180 minutes, namely obtain containing dysprosium rare earth permanent-magnetic material base substrate, finally carry out machining cutting to containing dysprosium rare earth permanent-magnetic material base substrate and refine according to the actual requirements, reserved size of carrying out electroplating, obtains containing dysprosium 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 | CD | (B.H)max/MGOe |
| Test value | 14.2 | 10.7 | 660 | 920 | 52 |
In above-described embodiment 1 ~ 5, 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, obtain pretreatment magnet material, again the pretreatment magnet material of acquisition and the europium particulate to have prepared are dropped in general electrolytic stove and carry out melting and make it form the aluminium alloy of melting, efficiently solve the different and manual operation factor of the fusing point of each component and to cause after melting must alloy pig generation segregation problems; And adding of dysprosium is conducive to improving the actual coercivity of alloy pig, its permanent-magnet material product prepared; And europium particulate is added in pretreatment magnet material, the dysprosium element of europium nanoparticle in pretreatment magnet material is combined and generates nanometer Y
2o
3: Eu
3+, through carrying out fluorometric investigation, when aluminium to it: time europium=10:1 (mol ratio), i.e. embodiment 4, has best green glow and strengthens effect; When aluminium: time europium=50:1 (mol ratio), i.e. embodiment 2, luminous intensity is the strongest, and the interpolation of europium nanoparticle changes permanent-magnet material rare earth elements dot matrix case, effectively enhance fluorescence lifetime, and make permanent-magnet material have higher critical concentration.
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 (10)
1. in steel refuse by magnetic, add the method for Nano metal powder preparation containing dysprosium rare earth permanent-magnetic material, it is characterized in that, concrete steps are as follows:
1) the waste and old magnet steel collected is presorted according to rare earth element contained in magnet steel, the standard of the presorting waste and old magnet steel that rare earth element is identical contained by same batch same model is classified as a class, obtain pretreatment magnet material, pretreatment magnet material comprises neodymium, praseodymium, dysprosium and terbium, from pretreatment magnet material, extract sample simultaneously, and detection record is carried out as comparison value to the rare earth component in sample;
2) by step 1) in the pretreatment magnet material obtained and the Nano metal powder to have prepared, according to percent mass proportioning: 95 ~ 97% pretreatment magnet materials, 3 ~ 5% Nano metal powders, obtain mixing match material, making it form the aluminium alloy of melting by carrying out melting in mixing match material input general electrolytic stove simultaneously, then the aluminium alloy of melting being cast and being cooled to alloy pig;
3) by step 2) in alloy pig, 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;
4) by step 3) in the fine powder that obtains add isostatic pressing method by mold pressing and be pressed into pressed compact;
5) by step 4) in the pressed compact that obtains be placed in vacuum sintering furnace and sinter and be incubated;
6) by step 5) 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 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 containing dysprosium rare earth permanent-magnetic material base substrate;
7) by step 6) in obtain containing dysprosium rare earth permanent-magnetic material base substrate, carry out machining cutting according to the actual requirements and refine, reserved size of carrying out electroplating, obtains containing dysprosium rare earth permanent-magnetic material simultaneously.
2. the method for adding Nano metal powder preparation and containing dysprosium rare earth permanent-magnetic material in steel refuse by magnetic according to claim 1, is characterized in that, described step 2) in, smelting temperature is 1495 DEG C ~ 1550 DEG C.
3. the method for adding Nano metal powder preparation and containing dysprosium rare earth permanent-magnetic material in steel refuse by magnetic according to claim 1, is characterized in that, described step 2) in, Nano metal powder is europium nanoparticle.
4. the method for adding Nano metal powder preparation and containing dysprosium rare earth permanent-magnetic material in steel refuse by magnetic according to claim 1, it is characterized in that, the alloy pig produced is detected, and with step 1) in sample rare earth component comparison value compare, when not being inconsistent with comparison value, again allocating containing holmium rare earth permanent-magnetic material component according to required preparation.
5. the method for adding Nano metal powder preparation and containing dysprosium rare earth permanent-magnetic material in steel refuse by magnetic according to claim 1, is characterized in that, described step 3) in, fine powder particle mean size is 2.4 ~ 2.8 μm.
6. the method for adding Nano metal powder preparation and containing dysprosium rare earth permanent-magnetic material in steel refuse by magnetic according to claim 1, is characterized in that, described step 4) in, the pressure of isostatic pressed is 230 ~ 280MPa.
7. the method for adding Nano metal powder preparation and containing dysprosium rare earth permanent-magnetic material in steel refuse by magnetic according to claim 1, is characterized in that, described step 5) in, sintering temperature is 1070 DEG C ~ 1095 DEG C.
8. the method for adding Nano metal powder preparation and containing dysprosium rare earth permanent-magnetic material in steel refuse by magnetic according to claim 1, is characterized in that, described step 5) in, temperature retention time is 180 minutes.
9. the method for adding Nano metal powder preparation and containing dysprosium rare earth permanent-magnetic material in steel refuse by magnetic according to claim 1, is characterized in that, described step 6) 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 180 minutes.
10. according to claim 1ly in steel refuse by magnetic, add Nano metal powder preparation containing the method for dysprosium rare earth permanent-magnetic material, preparation containing dysprosium rare earth permanent-magnetic material, it is characterized in that, comprise neodymium, praseodymium, dysprosium, boron, copper, aluminium, terbium, iron and Nano metal powder; Each constituent mass percentage is: 7 ~ 15% neodymiums, 4 ~ 10% praseodymiums, 4 ~ 10% dysprosiums, 0.8 ~ 1.2% boron, 0 ~ 0.25% bronze medal, 0.3 ~ 6% aluminium, 0.1 ~ 3% terbium, 50 ~ 80% iron, 3 ~ 5% Nano metal powders, and iron is iron and inevitable impurity.
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