CN105598440A - Method for preparing dysprosium-containing rare earth permanent magnetic material by adding metal powder to waste magnetic steel - Google Patents
Method for preparing dysprosium-containing rare earth permanent magnetic material by adding metal powder to waste magnetic steel Download PDFInfo
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Abstract
A method for preparing a dysprosium-containing rare earth permanent magnetic material by adding metal powder to waste magnetic steel includes the steps that collected waste magnetic steel is pre-classified according to the classification standard that waste magnetic steel containing same rare earth elements in the same batch and same model is regarded as one category, a preprocessed magnetic material is obtained, a sample is extracted from the preprocessed magnetic material, and rare earth components in the sample are detected and recorded; then the obtained preprocessed magnetic material and prepared iron powder are put into a common electrolytic furnace for smelting so that the mixture can form molten alloy. The method effectively solves the problem that due to different melting points of components and manual operation factors, segregation of alloy ingots obtained after smelting is caused, and pre-classification is conducted so that time for recycling the waste magnetic steel can be saved; process steps for extracting rare earth elements are reduced; the metal powder is added into the preprocessed magnetic material, so that bending strength, hardness and impact toughness of the rare earth permanent magnetic material are improve; dysprosium is added so that actual coercivity of the alloy ingots is improved easily.
Description
Technical field
The present invention relates to rare-earth permanent-magnet material technical field, relate in particular to a kind of gold that adds in waste and old magnet steelBelong to the method for powder preparation containing dysprosium rare earth permanent-magnetic material.
Background technology
In recent years, along with the continuous expansion of rare earth permanent-magnetic material application, more next to raw-material demandLarger, but because the cost of rare earth mining is higher and along with the increasing of national regulation and control dynamics, its material cost alsoStrengthen gradually. And in the situation that present price amount of increase is excessive, the price endurance comparison of down-stream enterpriseThe material generation such as ferrite or aluminium nickel cobalt, SmCo limited, therefore portion downstream enterprise choice for use is more cheapFor the rare earth in neodymium iron boron magnetic body raw material, this brings larger unstability to neodymium iron boron magnetic body market.Because Nd-Fe-B magnetic material fragility is high, specification is assorted, very easily occurs unfilled corner and size in electroplating process simultaneouslyThe problem such as bad; And then the learies that causes electroplating rear neodymium iron boron magnetic body is very large, be only finished product outward appearance withThe scrappage of size is just between 2～5%, and because other aspect particular/special requirements of client also cause sending out oftenThe raw bad phenomenon of scrapping.
At present for the recovery of waste and old magnet steel and the process of recycling be: by all waste and old magnetic of collectingSteel reinforced concrete is integrated, presort, and unified be back to returnable, in returnable by waste and old magneticVarious rare earth elements contained in steel extract one by one, then according to the rare earth permanent-magnetic material of required preparation againProcess. Although this process recycles waste and old magnet steel, its abstraction process is multipleAssorted, and need be for the various technological parameters of different rare earth element fusing points adjustment returnable, to meet differenceThe extraction process requirement of rare earth element, this equipment to returnable has put forward higher requirement. SimultaneouslyAgain add man-hour, recovery is obtained to single rare-earth oxide, Hou road is through proportioning smelting etc.After each road technique, obtain requiring the permanent-magnet material of preparation, and that the permanent magnet that adopts this technique to make has is manyDefect, production process is difficult to control, human factor is more, and then the quality of impact batch production. WithNeodymium iron boron is example, after the praseodymium going out, neodymium and iron, boron and other compositions are mixed, is added into through extract and separateVacuum melting furnace melting, obtains alloy pig after melting, in this process because the fusing point difference of each composition,And be subject to the factor shadow such as the time interval and the control of amount whether front road mix and blend evenly and manually addsRing, certainly will cause the alloy pig material segregation after melting, even affect the performance of alloy pig material and follow-upTechnological effect, simultaneously higher to operating personnel's technical requirement in process of production, hand labor intensity is large.In addition, the actual coercivity of permanent-magnet material of existing production technology production is low, service temperature stability is lower,And a little less than corrosion resistance, become the principal element that limits its development and application.
The rare earth permanent-magnetic material of preparing by rare earth element, have high catalytic activity, high magnetic, superconductivity,The characteristics such as photoelectric conversion, optomagnetic memory, high weight of hydrogen, corrosion-proof wear, but should by rare earth permanent-magnetic materialBe used in thermal pressing sintering diamond tool carcass material, glass saw blade and plating diamond tool field, it is anti-Curved intensity, hardness and toughness obviously reduce; Therefore, how not change rare earth permanent-magnetic material spyUnder the prerequisite of property, improve bending strength, hardness and the toughness of rare earth permanent-magnetic material, after avoiding simultaneouslyAlloy pig material production segregation when continuous melting, and reduction has become this to the technical requirement of production equipmentThe 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 and in waste and old magnet steel, adds metal powder preparation and containThe method of dysprosium rare earth permanent-magnetic material, 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 metal powder preparation method containing dysprosium rare earth permanent-magnetic material, its concrete steps asUnder:
1) the waste and old magnet steel of collecting is presorted according to contained rare earth element in magnet steel, the mark of presortingAccurate for being classified as a class with the identical waste and old magnet steel of the contained rare earth element of batch same model, obtain pretreatment magnet materialMaterial, pretreatment magnet material comprises neodymium, praseodymium, dysprosium and yttrium, extracts sample from pretreatment magnet material simultaneouslyProduct, and the rare earth component in sample is carried out to detection record be worth as comparison;
2) by step 1) the middle pretreatment magnet material obtaining and the metal powder having prepared, according to qualityPer distribution ratio: 95～97% pretreatment magnet materials, 3～5% metal powders, drop in common electrolytic furnace and carry outMelting makes it form the aluminium alloy of melting, then the aluminium alloy of melting is cast and is cooled to alloy pig;
3) by step 2) the middle alloy pig obtaining is broken by hydrogen, airflow milling is broken into fine powder, and is enteringWhen row airflow milling, put into quantitative air and carry out passivation, and the powder that front and back are ground carries out mix and blend;
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 obtain pressed compact be placed in vacuum sintering furnace sintering and be incubated;
6) by step 5) in pressed compact after sintering 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 continuing to be cooled to 300 DEG C～350 DEG C, finally heating upTo second segment heat treatment and be incubated, and two sections of heat treatments are carried out respectively to tempering, rare to obtain containing dysprosiumSoil permanent-magnet material base substrate;
7) by step 6) in obtain containing dysprosium rare earth permanent-magnetic material base substrate, carry out according to the actual requirements machineryProcessing is cut and is refined, and reserved size of 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, metal powder is iron powder, utilizes iron powder to replace rare earth element cobalt,The rare-earth iron-based diamond tool composite of preparing, through its actual serviceability is tested, its bending strength,Hardness, impact flexibility all have a more substantial increase, and porosity has obvious reduction; Improving glass saw bladeCutting ability aspect, effectively increased the fragility of cutter head carcass material, realized diamond and carcassSynchronous wearing and tearing, and adamantine degree of exfoliation obviously reduces; Aspect plating diamond tool development, effectivelyThe bond strength of coating and matrix and the grinding ratio of diamond tool are improved.
In the present invention, described step 2) in, the alloy pig of producing is detected, and with step 1)In sample rare earth component comparison value compare, in the time not being inconsistent with the value of comparison, according to containing of required preparationDysprosium rare earth permanent-magnetic material component is allocated again.
In the present invention, described step 3) in, fine powder particle mean size is 2.4～3.0 μ m.
In the present invention, described step 4) in, the pressure that waits static pressure 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, protectsThe temperature 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 of collecting is divided in advance according to contained rare earth element in magnet steelClass, the content of various rare earth elements in the waste and old magnet steel that can obtain being about to process, and then effectively for notAdjust with rare earth element fusing point, not only save the time of reclaiming waste and old magnet steel, and it is waste and old to reduce extractionIn magnet steel, the processing step of different rare earth elements and the requirement reducing returnable equipment, also make a living simultaneouslyProduce with the rare earth permanent-magnetic material later process of the equal model of waste and old magnet steel and facilitate.
In the present invention, dysprosium adds the actual coercivity that is conducive to improve alloy pig, the permanent magnetism that it is preparedMaterial product, more superior at aspects such as corrosion resistance, heat endurance, processing characteristicies; And pass through pre-Process magnet material and the metal powder molten alloy ingot preparing, no longer need vacuum reduction smelting furnace,Effectively reduce the production cost of enterprise, and the fusing point difference and the people that have solved each component in traditional fusion processFor causing the alloy pig obtaining after melting, operation factors produces the problem of segregation; Adding of yttrium is conducive to improveThe actual coercivity of alloy pig reduces neodymium, praseodymium consumption simultaneously.
A kind of containing dysprosium rare earth permanent-magnetic material, comprise neodymium, praseodymium, dysprosium, boron, copper, aluminium, yttrium, iron and metalPowder; Each constituent mass percentage is: 10～20% neodymiums, 8～15% praseodymiums, 3～12% dysprosiums, 0.8～1.2%Boron, 0～0.25% bronze medal, 0～0.8% aluminium, 0.1～3% yttrium, 56～79% iron, 3～5% metal powders, andIron is iron and inevitable impurity.
Beneficial effect: the present invention divides the waste and old magnet steel of collecting in advance according to contained rare earth element in magnet steelClass, and then effectively adjust for different rare earth element fusing points, not only save reclaim waste and old magnet steel timeBetween, and reduce the processing step that extracts different rare earth elements in waste and old magnet steel, simultaneously also for producing with waste and oldThe rare earth permanent-magnetic material later process of the equal model of magnet steel facilitates; And pass through pretreatment magnet materialMetal powder molten alloy ingot with preparing, no longer needs vacuum reduction smelting furnace, effectively reduces enterpriseProduction cost, and solved the different and manual operation factor of the fusing point of each component in traditional fusion process andCause after melting alloy pig produce the problem of segregation, dysprosium adds the reality that is conducive to improve alloy pig to rectifyStupid power; Yttrium add the actual coercivity that is conducive to improve alloy pig, reduce neodymium, praseodymium consumption, gold simultaneouslyBelong to the interpolation of powder, improve bending strength, hardness and toughness containing dysprosium rare earth permanent-magnetic material.
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, by preparing burden as following table 1-1:
Table 1-1 embodiment 1 formula table
| Component | Neodymium | Praseodymium | Dysprosium | Yttrium | Boron | Copper | Aluminium | Iron | Iron powder | Add up to |
| Weight/kg | 4.2 | 3.2 | 0.63 | 0.02 | 0.2 | 0.0 | 0.0 | 12 | 0.65 | 20.9 |
| Mass percent/% | 20 | 15 | 3 | 0.1 | 0.8 | 0 | 0 | 58 | 3.1 | 100 |
The preparation method of the above-mentioned rare earth permanent-magnetic material of the present embodiment is as follows:
The waste and old magnet steel of collecting is classified as according to the same identical waste and old magnet steel of the contained rare earth element of batch same modelThe criteria for classification of one class is presorted, and obtains pretreatment magnet material, simultaneously from pretreatment magnet materialExtract sample, and the rare earth component in sample is carried out to detection record be worth as comparison; Pre-by what obtain againProcessing magnet material and the iron powder having prepared drops into and in common electrolytic furnace, carries out melting and make it form meltingAluminium alloy, smelting temperature is 1495 DEG C, then the aluminium alloy of melting is cast and is cooled to alloy pig, logicalCross that hydrogen is broken, alloy pig is broken into the fine powder that particle mean size is 2.4 μ m by airflow milling, simultaneously can be according to sampleRare earth component comparison value in product, for rare earth permanent-magnetic material rare earth component and the proportion requirement of required preparationAdd appropriate rare earth component to satisfy the demands, and in the time carrying out airflow milling, put into quantitative air and carry out passivation,And the powder that front and back are ground carries out mix and blend; Successively fine powder being added to isostatic pressing method by mold pressing is pressed intoPressed compact, and etc. the pressure of static pressure be 230MPa, green density is 4.3g/cm3; Treat that fine powder all suppressesAfter, pressed compact is placed in to vacuum sintering furnace sintering, sintering temperature is 1070 DEG C, and is incubated 180Minute; Then the pressed compact after sintering is cooled to 300 DEG C in vacuum sintering furnace, is being warming up to 900 DEG C alsoBe incubated 90 minutes, be again cooled to 300 DEG C, be warming up to 530 DEG C and be incubated 180 minutes,Obtain containing dysprosium rare earth permanent-magnetic material base substrate, finally according to the actual requirements permanent-magnet material base substrate is carried out to machineryProcessing is cut and is refined, and reserved size of electroplating, obtains containing dysprosium rare earth permanent-magnetic material simultaneously; Its propertyEnergy test data is referring to table 1-2.
Wherein, Br is remanent magnetism, and Hcb is coercivity, and (B.H) max is magnetic energy product, and MPa is that bending resistance is strongDegree.
Table 1-2 embodiment 1 properties of product test chart
| Project | Br/kGs | Hcb/KOe | MPa | (B.H)max/MGOe |
| Test value | 14.7 | 10.4 | 460 | 54 |
Embodiment 2
A kind of containing dysprosium rare earth permanent-magnetic material, by preparing burden as following table 2-1:
Table 2-1 embodiment 2 formula tables
| Component | Neodymium | Praseodymium | Dysprosium | Yttrium | Boron | Copper | Aluminium | Iron | Iron powder | Add up to |
| Weight/kg | 3.8 | 2.7 | 1 | 0.12 | 0.3 | 0.02 | 0.02 | 12 | 0.7 | 20.66 |
| Mass percent/% | 18 | 13 | 5 | 0.6 | 0.9 | 0.1 | 0.1 | 59 | 3.3 | 100 |
The preparation method of the above-mentioned rare earth permanent-magnetic material of the present embodiment is as follows:
The waste and old magnet steel of collecting is classified as according to the same identical waste and old magnet steel of the contained rare earth element of batch same modelThe criteria for classification of one class is presorted, and obtains pretreatment magnet material, simultaneously from pretreatment magnet materialExtract sample, and the rare earth component in sample is carried out to detection record be worth as comparison; Pre-by what obtain againProcessing magnet material and the iron powder having prepared drops into and in common electrolytic furnace, carries out melting and make it form meltingAluminium alloy, smelting temperature is 1500 DEG C, then the aluminium alloy of melting is cast and is cooled to alloy pig, logicalCross that hydrogen is broken, alloy pig is broken into the fine powder that particle mean size is 2.5 μ m by airflow milling, simultaneously can be according to sampleRare earth component comparison value in product, for rare earth permanent-magnetic material rare earth component and the proportion requirement of required preparationAdd appropriate rare earth component to satisfy the demands, and in the time carrying out airflow milling, put into quantitative air and carry out passivation,And the powder that front and back are ground carries out mix and blend; Successively fine powder being added to isostatic pressing method by mold pressing is pressed intoPressed compact, and etc. the pressure of static pressure be 240MPa, green density is 4.4g/cm3; Treat that fine powder all suppressesAfter, pressed compact is placed in to vacuum sintering furnace sintering, sintering temperature is 1080 DEG C, and is incubated 180Minute; Then the pressed compact after sintering is cooled to 310 DEG C in vacuum sintering furnace, is being warming up to 900 DEG C alsoBe incubated 90 minutes, be again cooled to 310 DEG C, be warming up to 550 DEG C and be incubated 180 minutes,Obtain containing dysprosium rare earth permanent-magnetic material base substrate, finally according to the actual requirements to containing dysprosium rare earth permanent-magnetic material base substrateCarry out machining cutting fine grinding, reserved size of electroplating, obtains containing dysprosium rare earth permanent magnet material simultaneouslyMaterial; Its performance test data is referring to table 2-2.
Table 2-2 embodiment 2 properties of product test charts
| Project | Br/kGs | Hcb/KOe | MPa | (B.H)max/MGOe |
| Test value | 14.3 | 10.6 | 490 | 54 |
Embodiment 3
A kind of containing dysprosium rare earth permanent-magnetic material, by preparing burden as following table 3-1:
Table 3-1 embodiment 3 formula tables
| Component | Neodymium | Praseodymium | Dysprosium | Yttrium | Boron | Copper | Aluminium | Iron | Iron powder | Add up to |
| Weight/kg | 3.1 | 2.5 | 1.47 | 0.2 | 0.4 | 0.04 | 0.06 | 12 | 0.74 | 20.51 |
| Mass percent/% | 15 | 12 | 7 | 1 | 1 | 0.2 | 0.3 | 60 | 3.5 | 100 |
The preparation method of the above-mentioned rare earth permanent-magnetic material of the present embodiment is as follows:
The waste and old magnet steel of collecting is classified as according to the same identical waste and old magnet steel of the contained rare earth element of batch same modelThe criteria for classification of one class is presorted, and obtains pretreatment magnet material, simultaneously from pretreatment magnet materialExtract sample, and the rare earth component in sample is carried out to detection record be worth as a comparison; Pre-by what obtain againProcessing magnet material and the iron powder having prepared drops into and in common electrolytic furnace, carries out melting and make it form meltingAluminium alloy, smelting temperature is 1520 DEG C, then the aluminium alloy of melting is cast and is cooled to alloy pig, logicalCross that hydrogen is broken, alloy pig is broken into the fine powder that particle mean size is 2.6 μ m by airflow milling, simultaneously can be according to sampleRare earth component comparison value in product, for rare earth permanent-magnetic material rare earth component and the proportion requirement of required preparationAdd appropriate rare earth component to satisfy the demands, and in the time carrying out airflow milling, put into quantitative air and carry out passivation,And the powder that front and back are ground carries out mix and blend; Successively fine powder being added to isostatic pressing method by mold pressing is pressed intoPressed compact, and etc. the pressure of static pressure be 250MPa, green density is 4.4g/cm3; Treat that fine powder all suppressesAfter, pressed compact is placed in to vacuum sintering furnace sintering, sintering temperature is 1085 DEG C, and is incubated 180Minute; Then the pressed compact after sintering is cooled to 320 DEG C in vacuum sintering furnace, is being warming up to 910 DEG C alsoBe incubated 90 minutes, be again cooled to 320 DEG C, be warming up to 570 DEG C and be incubated 180 minutes,Obtain containing dysprosium rare earth permanent-magnetic material base substrate, finally according to the actual requirements to containing dysprosium rare earth permanent-magnetic material base substrateCarry out machining cutting fine grinding, reserved size of electroplating, obtains containing dysprosium rare earth permanent magnet material simultaneouslyMaterial; Its performance test data is referring to table 3-2.
Table 3-2 embodiment 3 properties of product test charts
| Project | Br/kGs | Hcb/KOe | MPa | (B.H)max/MGOe |
| Test value | 14.5 | 10.9 | 530 | 54 |
Embodiment 4
A kind of containing dysprosium rare earth permanent-magnetic material, by preparing burden as following table 4-1:
Table 4-1 embodiment 4 formula tables
| Component | Neodymium | Praseodymium | Dysprosium | Yttrium | Boron | Copper | Aluminium | Iron | Iron powder | Add up to |
| Weight/kg | 2.7 | 2.1 | 1.89 | 0.3 | 0.5 | 0.04 | 0.1 | 12 | 0.99 | 20.62 |
| Mass percent/% | 13 | 10 | 9 | 1.5 | 1.1 | 0.2 | 0.5 | 60 | 4.7 | 100 |
The preparation method of the above-mentioned rare earth permanent-magnetic material of the present embodiment is as follows:
The waste and old magnet steel of collecting is classified as according to the same identical waste and old magnet steel of the contained rare earth element of batch same modelThe criteria for classification of one class is presorted, and obtains pretreatment magnet material, simultaneously from pretreatment magnet materialExtract sample, and the rare earth component in sample is carried out to detection record be worth as comparison; Pre-by what obtain againProcessing magnet material and the iron powder having prepared drops into and in common electrolytic furnace, carries out melting and make it form meltingAluminium alloy, smelting temperature is 1540 DEG C, then the aluminium alloy of melting is cast and is cooled to alloy pig, logicalCross that hydrogen is broken, alloy pig is broken into the fine powder that particle mean size is 2.8 μ m by airflow milling, simultaneously can be according to sampleRare earth component comparison value in product, for rare earth permanent-magnetic material rare earth component and the proportion requirement of required preparationAdd appropriate rare earth component to satisfy the demands, and in the time carrying out airflow milling, put into quantitative air and carry out passivation,And the powder that front and back are ground carries out mix and blend; Successively fine powder being added to isostatic pressing method by mold pressing is pressed intoPressed compact, and etc. the pressure of static pressure be 240MPa, green density is 4.5g/cm3; Treat that fine powder all suppressesAfter, pressed compact is placed in to vacuum sintering furnace sintering, sintering temperature is 1090 DEG C, and is incubated 180Minute; Then the pressed compact after sintering is cooled to 330 DEG C in vacuum sintering furnace, is being warming up to 915 DEG C alsoBe incubated 90 minutes, be again cooled to 330 DEG C, be warming up to 590 DEG C and be incubated 180 minutes,Obtain containing dysprosium rare earth permanent-magnetic material base substrate, finally according to the actual requirements to containing dysprosium rare earth permanent-magnetic material base substrateCarry out machining cutting fine grinding, reserved size of electroplating, obtains containing dysprosium rare earth permanent magnet material simultaneouslyMaterial; Its performance test data is referring to table 4-2.
Table 4-2 embodiment 4 properties of product test charts
| Project | Br/kGs | Hcb/KOe | MPa | (B.H)max/MGOe |
| Test value | 14.6 | 11.3 | 570 | 53 |
Embodiment 5
A kind of containing dysprosium rare earth permanent-magnetic material, by preparing burden as following table 5-1:
Table 5-1 embodiment 5 formula tables
| Component | Neodymium | Praseodymium | Dysprosium | Yttrium | Boron | Copper | Aluminium | Iron | Iron powder | Add up to |
| Weight/kg | 2.1 | 1.7 | 2.1 | 0.5 | 0.6 | 0.04 | 0.2 | 13 | 0.92 | 21.16 |
| Mass percent/% | 10 | 8 | 10 | 2.4 | 1.2 | 0.2 | 0.8 | 63 | 4.4 | 100 |
The preparation method of the above-mentioned rare earth permanent-magnetic material of the present embodiment is as follows:
The waste and old magnet steel of collecting is classified as according to the same identical waste and old magnet steel of the contained rare earth element of batch same modelThe criteria for classification of one class is presorted, and obtains pretreatment magnet material, simultaneously from pretreatment magnet materialExtract sample, and the rare earth component in sample is carried out to detection record be worth as comparison; Pre-by what obtain againProcessing magnet material and the iron powder having prepared drops into and in common electrolytic furnace, carries out melting and make it form meltingAluminium alloy, smelting temperature is 1540 DEG C, then the aluminium alloy of melting is cast and is cooled to alloy pig, logicalCross that hydrogen is broken, alloy pig is broken into the fine powder that particle mean size is 3.0 μ m by airflow milling, simultaneously can be according to sampleRare earth component comparison value in product, for rare earth permanent-magnetic material rare earth component and the proportion requirement of required preparationAdd appropriate rare earth component to satisfy the demands, and in the time carrying out airflow milling, put into quantitative air and carry out passivation,And the powder that front and back are ground carries out mix and blend; Successively fine powder being added to isostatic pressing method by mold pressing is pressed intoPressed compact, and etc. the pressure of static pressure be 270MPa, green density is 4.5g/cm3; Treat that fine powder all suppressesAfter, pressed compact is placed in to vacuum sintering furnace sintering, sintering temperature is 1095 DEG C, and is incubated 180Minute; Then the pressed compact after sintering is cooled to 340 DEG C in vacuum sintering furnace, is being warming up to 920 DEG C alsoBe incubated 90 minutes, be again cooled to 340 DEG C, be warming up to 600 DEG C and be incubated 180 minutes,Obtain containing dysprosium rare earth permanent-magnetic material base substrate, finally according to the actual requirements to containing dysprosium rare earth permanent-magnetic material base substrateCarry out machining cutting fine grinding, reserved size of electroplating, obtains containing dysprosium rare earth permanent magnet material simultaneouslyMaterial; Its performance test data is referring to table 5-2.
Table 5-2 embodiment 5 properties of product test charts
| Project | Br/kGs | Hcb/KOe | MPa | (B.H)max/MGOe |
| Test value | 14.3 | 10.8 | 630 | 52 |
In above-described embodiment 1～5, the waste and old magnet steel of just collecting is according to the same contained rare earth of batch same modelThe waste and old magnet steel that element is identical is classified as the criteria for classification of a class and presorts, and obtains pretreatment magnet material,From pretreatment magnet material, extract sample, and the rare earth component in sample is carried out to detection record simultaneously;Again the pretreatment magnet material of acquisition and the iron powder having prepared are dropped into and in common electrolytic furnace, carry out melting and makeIt forms the aluminium alloy of melting, efficiently solves the different and manual operation factor of the fusing point of each component and causesThe alloy pig obtaining after melting produces segregation problem; Dysprosium adds the actual coercivity that is conducive to improve alloy pig;Yttrium add the actual coercivity that is conducive to improve alloy pig, reduce neodymium, praseodymium consumption simultaneously, metal powderAdd, improve bending strength, hardness and toughness containing dysprosium rare earth permanent-magnetic material.
More than show and described general principle of the present invention and principal character and advantage of the present invention. One's own professionThe technical staff of industry should understand, and the present invention is not restricted to the described embodiments, above-described embodiment and explanationThat in book, describes 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 into claimed model of the present inventionIn enclosing. The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (10)
1. in waste and old magnet steel, add the method for 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 of collecting is presorted according to contained rare earth element in magnet steel, the mark of presortingAccurate for being classified as a class with the identical waste and old magnet steel of the contained rare earth element of batch same model, obtain pretreatment magnet materialMaterial, pretreatment magnet material comprises neodymium, praseodymium, dysprosium and yttrium, extracts sample from pretreatment magnet material simultaneouslyProduct, and the rare earth component in sample is carried out to detection record be worth as comparison;
2) by step 1) the middle pretreatment magnet material obtaining and the metal powder having prepared, according to qualityPer distribution ratio: 95～97% pretreatment magnet materials, 3～5% metal powders, drop in common electrolytic furnace and carry outMelting makes it form the aluminium alloy of melting, then the aluminium alloy of melting is cast and is cooled to alloy pig;
3) by step 2) the middle alloy pig obtaining is broken by hydrogen, airflow milling is broken into fine powder, and is enteringWhen row airflow milling, put into quantitative air and carry out passivation, and the powder that front and back are ground carries out mix and blend;
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 obtain pressed compact be placed in vacuum sintering furnace sintering and be incubated;
6) by step 5) in pressed compact after sintering 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 continuing to be cooled to 300 DEG C～350 DEG C, finally heating upTo second segment heat treatment and be incubated, and two sections of heat treatments are carried out respectively to tempering, rare to obtain containing dysprosiumSoil permanent-magnet material base substrate;
7) by step 6) in obtain containing dysprosium rare earth permanent-magnetic material base substrate, carry out according to the actual requirements machineryProcessing is cut and is refined, and reserved size of electroplating, obtains containing dysprosium rare earth permanent-magnetic material simultaneously.
2. the metal powder that adds in waste and old magnet steel according to claim 1 is prepared containing dysprosium rare earth permanent magnet materialMaterial method, it is characterized in that described step 2) in, to produce alloy pig detect, and with stepRapid 1) the sample rare earth component comparison value in is compared, in the time not being inconsistent with the value of comparison, according to required preparationAgain allocate containing dysprosium rare earth permanent-magnetic material component.
3. the metal powder that adds in waste and old magnet steel according to claim 1 is prepared containing dysprosium rare earth permanent magnet materialThe method of material, is characterized in that described step 2) in, smelting temperature is 1495 DEG C～1550 DEG C.
4. the metal powder that adds in waste and old magnet steel according to claim 1 is prepared containing dysprosium rare earth permanent magnet materialThe method of material, is characterized in that described step 2) in, metal powder is iron powder.
5. the metal powder that adds in waste and old magnet steel according to claim 1 is prepared containing dysprosium rare earth permanent magnet materialThe method of material, is characterized in that described step 3) in, fine powder particle mean size is 2.4～3.0 μ m.
6. the metal powder that adds in waste and old magnet steel according to claim 1 is prepared containing dysprosium rare earth permanent magnet materialThe method of material, is characterized in that described step 4) in, the pressure that waits static pressure is 230～280MPa.
7. the metal powder that adds in waste and old magnet steel according to claim 1 is prepared containing dysprosium rare earth permanent magnet materialThe method of material, is characterized in that described step 5) in, sintering temperature is 1070 DEG C～1095 DEG C.
8. the metal powder that adds in waste and old magnet steel according to claim 1 is prepared containing dysprosium rare earth permanent magnet materialThe method of material, is characterized in that described step 5) in, temperature retention time is 180 minutes.
9. the metal powder that adds in waste and old magnet steel according to claim 1 is prepared containing dysprosium rare earth permanent magnet materialThe method of material, is characterized in that described step 6) in, first paragraph heat treatment temperature is 900 DEG C～920 DEG C,Temperature retention time is 90 minutes; Second segment heat treatment temperature is 530 DEG C～620 DEG C, and temperature retention time is 180 pointsClock.
10. contain dysprosium according to the metal powder preparation of adding described in claim 1～9 any one in waste and old magnet steelThe method of rare earth permanent-magnetic material, the rare earth permanent-magnetic material of preparation, is characterized in that, comprise neodymium, praseodymium, dysprosium,Boron, copper, aluminium, yttrium, iron and metal powder; Each constituent mass percentage is: 10～20% neodymiums, 8～15%Praseodymium, 3～12% dysprosiums, 0.8～1.2% boron, 0～0.25% bronze medal, 0～0.8% aluminium, 0.1～3% yttrium, 56～79% iron, 3～5% metal powders, and iron is iron and inevitable impurity.
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Application publication date: 20160525 |