CN105598436A - Method for adding liquid phase gadolinium to waste magnetic steel to prepare rare earth permanent magnetic material - Google Patents
Method for adding liquid phase gadolinium to waste magnetic steel to prepare rare earth permanent magnetic material Download PDFInfo
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Abstract
The invention provides a method for adding liquid phase gadolinium to waste magnetic steel to prepare a rare earth permanent magnetic material. According to the method, collected waste magnetic steel is classified in advance according to the classification standard of classifying the same batch and the same type of the waste magnetic steel containing the same rare earth element into one class to obtain a pretreated magnetic body material, and the obtained pretreated magnetic body material is directly smashed in a hydrogen mode and prepared into powder, so that rare earth hydrogen-smashed magnetic power is obtained; the rare earth hydrogen-smashed magnetic power is sampled and analyzed, and liquid phase gadolinium is added into the rare earth hydrogen-smashed magnetic power according to needs, so that mixed powder is obtained; finally, the needed rare earth permanent magnetic material is prepared by means of static pressure, sintering and annealing; the problem that due to the difference among melting points of all the components and man-made operation factors, segregation of alloy ingots obtained in the smelting process is effectively solved; pre-classifying is carried out, so that time for recovering the waste magnetic steel is saved; moreover, the process step of extracting the rare earth element is omitted; liquid phase gadolinium is added into the pretreated magnetic body material, which is beneficial for improving heat stability of the alloy ingots, magnetic performance of the permanent magnetic material is kept unchanged, and the ability to resist interference of an external magnetic field.
Description
Technical field
The present invention relates to rare-earth permanent-magnet material technical field, relate in particular to one annex solution in waste and old magnet steelPhase gadolinium is prepared the method for 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. ThisOutward, the actual coercivity of permanent-magnet material of existing production technology production is low, service temperature stability is lower, andA 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; Therefore, how do not change rareUnder the prerequisite of soil permanent-magnet material characteristic, improve bending strength, hardness and the toughness of rare earth permanent-magnetic material,Alloy pig material production segregation while simultaneously avoiding follow-up melting, and reduce the technical requirement to production equipmentBecome those skilled in the art's major issue 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 liquid phase gadolinium and prepare rareThe method of soil permanent-magnet 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 liquid phase gadolinium and prepare the method for rare earth permanent-magnetic material, its 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;
2) according to preparation rare earth permanent-magnetic material, to step 1) in obtain pretreatment magnet material directCarry out the broken powder process of hydrogen, obtain the broken magnetic of rare earth hydrogen;
3) to step 2) in the broken magnetic of rare earth hydrogen that obtains carry out sample analysis, obtain rare-earth magnetic component ginsengNumber;
4) according to step 3) the middle rare-earth magnetic component parameter obtaining of analyzing, the broken magnetic of rare earth hydrogen obtainingIn powder, add liquid phase gadolinium and obtain mixed powder, the quality per distribution ratio of mixed powder: the broken magnetic of 95～97% rare earth hydrogen,3～5% liquid phase gadoliniums;
5) by step 4) the middle mixed powder 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;
6) by step 5) in the fine powder that obtains add isostatic pressing method by mold pressing and be pressed into pressed compact;
7) by step 6) in obtain pressed compact be placed in vacuum sintering furnace sintering and be incubated;
8) by step 7) in pressed compact after sintering in vacuum sintering furnace, be cooled to 300 DEG C～360 DEG C, thenBe warming up to first paragraph heat treatment and be incubated, then continuing to be cooled to 300 DEG C～360 DEG C, finally heating upTo second segment heat treatment and be incubated, and two sections of heat treatments are carried out respectively to tempering, to obtain rare earth foreverMagnetic body of material;
9) by step 8) the middle rare earth permanent-magnetic material base substrate obtaining, carries out machining according to the actual requirementsCut and refine, reserved size of electroplating, obtains rare earth permanent-magnetic material simultaneously.
In the present invention, described step 5) in, fine powder particle mean size is 2.4～3.0 μ m.
In the present invention, described step 6) in, the pressure that waits static pressure is 230～280MPa.
In the present invention, described step 7) in, sintering temperature is 1070 DEG C～1095 DEG C.
In the present invention, described step 7) in, temperature retention time is 200 minutes.
In the present invention, described step 8) in, first paragraph heat treatment temperature is 900 DEG C～920 DEG C, protectsThe temperature 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 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; Adding of gadolinium is conducive toThe heat endurance that improves alloy pig, the permanent-magnet material product that it is prepared, in heat endurance and processing characteristicsEtc. aspect more superior, when ambient temperature produces when larger variation, effectively keep the magnetic property of permanent-magnet materialDo not change, anti-external magnetic field interference performance is strong.
A kind of rare earth permanent-magnetic material, comprises neodymium, praseodymium, gadolinium, boron, copper, aluminium, yttrium and iron; Each component matterAmount percentage is: 10～20% neodymiums, 8～15% praseodymiums, 5～20% gadoliniums, 0.8～1.2% boron, 0～0.25%Copper, 0～0.8% aluminium, 0.2～3% yttrium, 39～76% iron, and iron is iron and inevitable impurity.
Beneficial effect: the present invention by by by collect waste and old magnet steel enter according to contained rare earth element in magnet steelRow is presorted, the content of various rare earth elements in the waste and old magnet steel that can obtain being about to process, and then effectivelyAdjust for different rare earth element fusing points, not only save the time of reclaiming waste and old magnet steel, and reduce and carryGet the processing step and the requirement reducing returnable equipment of different rare earth elements in waste and old magnet steel, simultaneouslyAlso facilitate for producing with the alloy permanent-magnet material later process of the equal model of waste and old magnet steel; And by dividingAnalyse the rare-earth magnetic component parameter obtaining, in the broken magnetic of rare earth hydrogen obtaining, add liquid phase gadolinium and obtain mixed powder,Effectively reduce the production cost of enterprise, and the fusing point difference and the people that have solved each component in traditional fusion processProduce the problem of segregation for operation factors causes the alloy pig obtaining after melting, adding of gadolinium is conducive to improveThe heat endurance of alloy pig; Yttrium add the actual coercivity that is conducive to improve alloy pig, reduce simultaneously neodymium,Praseodymium consumption.
Detailed description of the invention
Describe the present invention below by following specific embodiment.
Embodiment 1
A kind of rare earth permanent-magnetic material, by preparing burden as following table 1-1:
Table 1-1 embodiment 1 formula table
| Component | Neodymium | Praseodymium | Gadolinium | Yttrium | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 4.2 | 3.2 | 1.1 | 0.04 | 0.17 | 0 | 0. | 12.4 | 21.11 |
| Mass percent/% | 20 | 15 | 5 | 0.2 | 0.8 | 0 | 0 | 59 | 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; Then according to the rare earth permanent magnet of preparationMaterial, directly carries out the broken powder process of hydrogen to the pretreatment magnet material obtaining, and obtains the broken magnetic of rare earth hydrogen; SimultaneouslyThe rare earth hydrogen broken magnetic obtaining is carried out to sample analysis, obtain rare-earth magnetic component parameter, then according to analyzingThe rare-earth magnetic component parameter arriving is added liquid phase gadolinium and is obtained mixed powder in the broken magnetic of rare earth hydrogen obtaining,After broken by hydrogen the mixed powder of acquisition, airflow milling are broken into fine powder, and put in the time carrying out airflow millingQuantitative air carries out passivation, and the powder that front and back are ground carries out mix and blend, the particle mean size of fine powderBe 2.4 μ m, successively fine powder added to isostatic pressing method by mold pressing and be pressed into pressed compact, and etc. the pressure of static pressureFor 230MPa, green density is 4.3g/cm3; After treating that fine powder is all suppressed, pressed compact is placed in verySintering in empty sintering furnace, sintering temperature is 1070 DEG C, and is incubated 200 minutes; Then by after sinteringPressed compact in vacuum sintering furnace, be cooled to 300 DEG C, then be warming up to 900 DEG C and be incubated 90 minutes,Again be cooled to 300 DEG C, being warming up to 530 DEG C and be incubated 200 minutes, obtain rare earth permanent magnet materialMaterial base body, finally carries out machining cutting fine grinding to permanent-magnet material base substrate, simultaneously according to the actual requirementsReserved size of electroplating, obtains rare earth permanent-magnetic material; Its performance 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 | 14.6 | 10.5 | 460 | 54 |
Embodiment 2
A kind of rare earth permanent-magnetic material, by preparing burden as following table 2-1:
Table 2-1 embodiment 2 formula tables
| Component | Neodymium | Praseodymium | Gadolinium | Yttrium | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 3.8 | 2.5 | 1.68 | 0.15 | 0.2 | 0.02 | 0.04 | 12.6 | 20.99 |
| Mass percent/% | 18 | 12 | 8 | 0.7 | 1 | 0.1 | 0.2 | 60 | 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; Then according to the rare earth permanent magnet of preparationMaterial, directly carries out the broken powder process of hydrogen to the pretreatment magnet material obtaining, and obtains the broken magnetic of rare earth hydrogen; SimultaneouslyThe rare earth hydrogen broken magnetic obtaining is carried out to sample analysis, obtain rare-earth magnetic component parameter, then according to analyzingThe rare-earth magnetic component parameter arriving is added liquid phase gadolinium and is obtained mixed powder in the broken magnetic of rare earth hydrogen obtaining,After broken by hydrogen the mixed powder of acquisition, airflow milling are broken into fine powder, and put in the time carrying out airflow millingQuantitative air carries out passivation, and the powder that front and back are ground carries out mix and blend, the particle mean size of fine powderBe 2.5 μ m; Successively fine powder is added to isostatic pressing method by mold pressing and is pressed into pressed compact, and etc. the pressure of static pressureFor 240MPa, green density is 4.4g/cm3; After treating that fine powder is all suppressed, pressed compact is placed in verySintering in empty sintering furnace, sintering temperature is 1080 DEG C, and is incubated 200 minutes; Then by after sinteringPressed compact in vacuum sintering furnace, be cooled to 310 DEG C, then be warming up to 900 DEG C and be incubated 90 minutes,Again be cooled to 310 DEG C, being warming up to 550 DEG C and be incubated 200 minutes, obtain rare earth permanent magnet materialMaterial base body, finally carries out machining cutting fine grinding to rare earth permanent-magnetic material base substrate according to the actual requirements,Reserved size of electroplating, obtains rare earth permanent-magnetic material simultaneously; 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 | 14.4 | 10.6 | 490 | 54 |
Embodiment 3
A kind of rare earth permanent-magnetic material, by preparing burden as following table 3-1:
Table 3-1 embodiment 3 formula tables
| Component | Neodymium | Praseodymium | Gadolinium | Yttrium | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 2.7 | 2.1 | 2.52 | 0.25 | 0.5 | 0.04 | 0.1 | 13.0 | 21.21 |
| Mass percent/% | 13 | 10 | 12 | 1.2 | 1.1 | 0.2 | 0.5 | 62 | 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; Then according to the rare earth permanent magnet of preparationMaterial, directly carries out the broken powder process of hydrogen to the pretreatment magnet material obtaining, and obtains the broken magnetic of rare earth hydrogen; SimultaneouslyThe rare earth hydrogen broken magnetic obtaining is carried out to sample analysis, obtain rare-earth magnetic component parameter, then according to analyzingThe rare-earth magnetic component parameter arriving is added liquid phase gadolinium and is obtained mixed powder in the broken magnetic of rare earth hydrogen obtaining,After broken by hydrogen the mixed powder of acquisition, airflow milling are broken into fine powder, and put in the time carrying out airflow millingQuantitative air carries out passivation, and the powder that front and back are ground carries out mix and blend, the particle mean size of fine powderBe 2.6 μ m; Successively fine powder is added to isostatic pressing method by mold pressing and is pressed into pressed compact, and etc. the pressure of static pressureFor 250MPa, green density is 4.4g/cm3; After treating that fine powder is all suppressed, pressed compact is placed in verySintering in empty sintering furnace, sintering temperature is 1085 DEG C, and is incubated 200 minutes; Then by after sinteringPressed compact in vacuum sintering furnace, be cooled to 320 DEG C, then be warming up to 910 DEG C and be incubated 90 minutes,Again be cooled to 320 DEG C, being warming up to 570 DEG C and be incubated 200 minutes, obtain rare earth permanent magnet materialMaterial base body, finally carries out machining cutting fine grinding to rare earth permanent-magnetic material base substrate according to the actual requirements,Reserved size of electroplating, obtains rare earth permanent-magnetic material simultaneously; 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 | 11.2 | 530 | 54 |
Embodiment 4
A kind of rare earth permanent-magnetic material, by preparing burden as following table 4-1:
Table 4-1 embodiment 4 formula tables
| Component | Neodymium | Praseodymium | Gadolinium | Yttrium | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 2.1 | 1.7 | 2.1 | 2.94 | 0.6 | 0.04 | 0.2 | 11.8 | 21.48 |
| Mass percent/% | 10 | 8 | 10 | 14 | 1.2 | 0.2 | 0.6 | 56 | 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; Then according to the rare earth permanent magnet of preparationMaterial, directly carries out the broken powder process of hydrogen to the pretreatment magnet material obtaining, and obtains the broken magnetic of rare earth hydrogen; SimultaneouslyThe rare earth hydrogen broken magnetic obtaining is carried out to sample analysis, obtain rare-earth magnetic component parameter, then according to analyzingThe rare-earth magnetic component parameter arriving is added liquid phase gadolinium and is obtained mixed powder in the broken magnetic of rare earth hydrogen obtaining,After broken by hydrogen the mixed powder of acquisition, airflow milling are broken into fine powder, and put in the time carrying out airflow millingQuantitative air carries out passivation, and the powder that front and back are ground carries out mix and blend, the particle mean size of fine powderBe 2.8 μ m; Successively fine powder is added to isostatic pressing method by mold pressing and is pressed into pressed compact, and etc. the pressure of static pressureFor 240MPa, green density is 4.5g/cm3; After treating that fine powder is all suppressed, pressed compact is placed in verySintering in empty sintering furnace, sintering temperature is 1090 DEG C, and is incubated 200 minutes; Then by after sinteringPressed compact in vacuum sintering furnace, be cooled to 330 DEG C, then be warming up to 915 DEG C and be incubated 90 minutes,Again be cooled to 330 DEG C, being warming up to 590 DEG C and be incubated 200 minutes, obtain rare earth permanent magnet materialMaterial base body, finally carries out machining cutting fine grinding to rare earth permanent-magnetic material base substrate according to the actual requirements,Reserved size of electroplating, obtains rare earth permanent-magnetic material simultaneously; 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 rare earth permanent-magnetic material, by preparing burden as following table 5-1:
Table 5-1 embodiment 5 formula tables
| Component | Neodymium | Praseodymium | Gadolinium | Yttrium | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 2.1 | 1.7 | 3.2 | 0.59 | 0.6 | 0.04 | 0.2 | 13.0 | 21.43 |
| Mass percent/% | 10 | 8 | 15 | 2.8 | 1.2 | 0.2 | 0.8 | 62 | 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; Then according to the rare earth permanent magnet of preparationMaterial, directly carries out the broken powder process of hydrogen to the pretreatment magnet material obtaining, and obtains the broken magnetic of rare earth hydrogen; SimultaneouslyThe rare earth hydrogen broken magnetic obtaining is carried out to sample analysis, obtain rare-earth magnetic component parameter, then according to analyzingThe rare-earth magnetic component parameter arriving is added liquid phase gadolinium and is obtained mixed powder in the broken magnetic of rare earth hydrogen obtaining,After broken by hydrogen the mixed powder of acquisition, airflow milling are broken into fine powder, and put in the time carrying out airflow millingQuantitative air carries out passivation, and the powder that front and back are ground carries out mix and blend, the particle mean size of fine powderBe 3.0 μ m, the rare earth component comparison value in simultaneously can be per sample, for the rare earth permanent magnet of required preparationMaterial rare earth component and proportion requirement are added appropriate rare earth component to satisfy the demands, and in the time carrying out airflow millingPut into quantitative air and carry out passivation, and the powder that front and back are ground carries out mix and blend; Successively by fine powderAdd isostatic pressing method by mold pressing and be pressed into pressed compact, and etc. the pressure of static pressure be 270MPa, green density is4.5g/cm3; After treating that fine powder is all suppressed, pressed compact is placed in to vacuum sintering furnace sintering, sintering temperatureDegree is 1095 DEG C, and is incubated 200 minutes; Then the pressed compact after sintering is fallen in vacuum sintering furnaceTemperature is to 350 DEG C, then is warming up to 920 DEG C and be incubated 90 minutes, is again cooled to 350 DEG C, heating upTo 600 DEG C and be incubated 200 minutes, obtain rare earth permanent-magnetic material base substrate, according to the actual requirements finallyRare earth permanent-magnetic material base substrate is carried out to machining cutting fine grinding, reserved size of electroplating simultaneously,Obtain rare earth permanent-magnetic material; 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 |
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 (7)
1. in waste and old magnet steel, add the method that liquid phase gadolinium is prepared rare earth permanent-magnetic material, it is characterized in that toolBody step is 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;
2) according to preparation rare earth permanent-magnetic material, to step 1) in obtain pretreatment magnet material directCarry out the broken powder process of hydrogen, obtain the broken magnetic of rare earth hydrogen;
3) to step 2) in the broken magnetic of rare earth hydrogen that obtains carry out sample analysis, obtain rare-earth magnetic component ginsengNumber;
4) according to step 3) the middle rare-earth magnetic component parameter obtaining of analyzing, the broken magnetic of rare earth hydrogen obtainingIn powder, add liquid phase gadolinium and obtain mixed powder, the quality per distribution ratio of mixed powder: the broken magnetic of 95～97% rare earth hydrogen,3～5% liquid phase gadoliniums;
5) by step 4) the middle mixed powder 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;
6) by step 5) in the fine powder that obtains add isostatic pressing method by mold pressing and be pressed into pressed compact;
7) by step 6) in obtain pressed compact be placed in vacuum sintering furnace sintering and be incubated;
8) by step 7) in pressed compact after sintering in vacuum sintering furnace, be cooled to 300 DEG C～360 DEG C, thenBe warming up to first paragraph heat treatment and be incubated, then continuing to be cooled to 300 DEG C～360 DEG C, finally heating upTo second segment heat treatment and be incubated, and two sections of heat treatments are carried out respectively to tempering, to obtain rare earth foreverMagnetic body of material;
9) by step 8) the middle rare earth permanent-magnetic material base substrate obtaining, carries out machining according to the actual requirementsCut and refine, reserved size of electroplating, obtains rare earth permanent-magnetic material simultaneously.
2. the liquid phase gadolinium that adds in waste and old magnet steel according to claim 1 is prepared rare earth permanent-magnetic materialMethod, is characterized in that, described step 5) in, fine powder particle mean size is 2.4～3.0 μ m.
3. the liquid phase gadolinium that adds in waste and old magnet steel according to claim 1 is prepared rare earth permanent-magnetic materialMethod, is characterized in that, described step 6) in, the pressure that waits static pressure is 230～280MPa.
4. the liquid phase gadolinium that adds in waste and old magnet steel according to claim 1 is prepared rare earth permanent-magnetic materialMethod, is characterized in that, described step 7) in, sintering temperature is 1070 DEG C～1095 DEG C.
5. the liquid phase gadolinium that adds in waste and old magnet steel according to claim 1 is prepared rare earth permanent-magnetic materialMethod, is characterized in that, described step 7) in, temperature retention time is 200 minutes.
6. the liquid phase gadolinium that adds in waste and old magnet steel according to claim 1 is prepared rare earth permanent-magnetic materialMethod, is characterized in that, described step 8) 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 200 pointsClock.
7. prepare rare earth according to the liquid phase gadolinium that adds described in claim 1～6 any one in waste and old magnet steelThe method of permanent-magnet material, the rare earth permanent-magnetic material of preparation, is characterized in that, comprise neodymium, praseodymium, gadolinium, boron,Copper, aluminium, yttrium and iron; Each constituent mass percentage is: 10～20% neodymiums, 8～15% praseodymiums, 5～20%Gadolinium, 0.8～1.2% boron, 0～0.25% bronze medal, 0～0.8% aluminium, 0.2～3% yttrium, 39～76% iron, andIron is iron and inevitable impurity.
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| 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 |
| CN104036942A (en) * | 2014-06-11 | 2014-09-10 | 北京工业大学 | Method for using bulk sintered neodymium iron boron (NdFeB) machining waste to prepare high-performance regenerated NdFeB magnet |
| CN104064302A (en) * | 2014-07-14 | 2014-09-24 | 陈久昌 | Neodymium, praseodymium, gadolinium and yttrium multi-element rare earth alloy permanent magnet material and preparation method |
| 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 |
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