CN105598435A - Method for preparing nano composite permanent magnetic material by adding phosphorus to magnetic steel waste - Google Patents
Method for preparing nano composite permanent magnetic material by adding phosphorus to magnetic steel waste Download PDFInfo
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Abstract
The invention provides a method for preparing a nano composite permanent magnetic material by adding phosphorus to magnetic steel waste. 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, the obtained preprocessed magnetic material is directly subjected to hydrogen decrepitation and pulverization, and rare earth hydrogen decrepitation magnetic powder is obtained; then the rare earth hydrogen decrepitation magnetic powder is sampled and analyzed, phosphorus is added into the rare earth hydrogen decrepitation magnetic powder according to needs to obtain mixed powder, and finally the needed nano composite permanent magnetic material is prepared through static pressing, sintering and annealing. 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 recycling time can be saved; process steps for extracting rare earth elements are reduced; phosphorus is added into the rare earth hydrogen decrepitation magnetic powder, magnetic facilitation axis orientation of Nd2Fe1B phase grains in the nano composite permanent magnetic material is changed easily, and the magnetic energy product is increased; magnetic properties are high, and the content of rare earth is low.
Description
Technical field
The present invention relates to nano composite permanent magnetic material technical field, relate in particular to one and add in steel refuse by magneticPhosphorate and prepare the method for nano composite permanent magnetic material.
Background technology
In recent years, along with the continuous expansion of nano composite permanent magnetic material application, to raw-material demandIncreasing, but because the cost of rare earth mining is higher and along with the increasing of national regulation and control dynamics, its material becomesThis also strengthens gradually. And in the situation that present price amount of increase is excessive, the price endurance of down-stream enterpriseThe material such as ferrite or aluminium nickel cobalt, SmCo more limited, therefore portion downstream enterprise choice for use is more cheapMaterial replaces the rare earth in neodymium iron boron magnetic body raw material, and it is larger unstable that this brings to neodymium iron boron magnetic body marketProperty. Simultaneously, because Nd-Fe-B magnetic material fragility is high, specification is assorted, in electroplating process, very easily occur unfilled corner andThe problems such as size is bad; And then the learies that causes electroplating rear neodymium iron boron magnetic body is very large, is only outside finished productSee and the scrappage of size just between 2～5%, and because other aspect particular/special requirements of client are also led oftenCause the bad phenomenon of scrapping occurs.
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 nano composite permanent magnetic material of required preparationAgain process. Although this process recycles waste and old magnet steel, it extracts workOrder complexity, and need be for the various technological parameters of different rare earth element fusing points adjustment returnable, to meetThe extraction process requirement of different rare earth elements, this equipment to returnable has put forward higher requirement.Again add man-hour, recovery is obtained to single rare-earth oxide, Hou road is through proportioning smelting simultaneouslyAfter Lian Dengge road technique, obtain requiring the permanent-magnet material of preparation, and the permanent magnet that adopts this technique to make hasMany defects, production process is difficult to control, and human factor is more, and then the quality of impact batch production.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.
In addition, nano composite permanent magnetic powder is mainly by fast quenching, mechanical alloying or high-energy ball milling at presentObtain etc. approach, but the shortcoming that these methods all exist some to be difficult to overcome conventionally, improves nano combinedThe spin-exchange-coupled efficiency of permanent-magnet material, need to be optimized from two aspects, and the one, control soft magnetism phase size,The yardstick that it has been generally acknowledged that soft magnetism phase should be less than the twice for Hard Magnetic phase domain wall width; The 2nd, obtain and be evenly distributedThe soft magnetism Hard Magnetic phase that is harmonious. But although these methods also can regulate the micro-structural of composite, veryDifficult crystallite dimension and the distribution of accurately controlling Hard Magnetic phase and soft magnetism phase, is particularly difficult to control respectively two kinds of phasesYardstick and composition. Therefore be also difficult to improve the maximum magnetic energy product of isotropism nano material. Therefore, asWhere do not change under the prerequisite of permanent-magnet material characteristic and improve permanent-magnet material maximum magnetic energy product, become abilityThe major issue that field technique personnel are urgently to be resolved hurrily.
Summary of the invention
Technical problem solved by the invention is to provide a kind of phosphorus that adds in steel refuse by magnetic to prepare nanometer againClose the method for 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 steel refuse by magnetic, add phosphorus and prepare the method for nano composite 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 the nano composite permanent magnetic material of preparation, to step 1) the middle pretreatment magnet material obtainingDirectly carry 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 phosphorus and obtain mixed powder, the quality per distribution ratio of mixed powder: the broken magnetic of 99.5～100% rare earth hydrogen, 0～0.5% phosphorus;
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, then adoptSeparation by precipitation is removed pressed compact and is reacted remaining metal nanoparticle, cleans 3～5 times, and ultrasonic oscillation,Then dry, obtain nano permanent magnetic material base substrate;
7) by step 6) in obtain nano permanent magnetic material base substrate be placed in vacuum sintering furnace sintering and carry outInsulation;
8) by step 7) in nano permanent magnetic material base substrate after sintering in vacuum sintering furnace, be cooled to300 DEG C～360 DEG C, then be warming up to first paragraph heat treatment and be incubated, then continue to be cooled to 300 DEG C～360 DEG C, be finally warming up to second segment heat treatment and be incubated, and two sections of heat treatments are carried out respectively to tempering,To obtain nano composite permanent magnetic material.
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 6) in, cleaning solution is alcohol, acetone and deionized water.
In the present invention, described step 6) in, be dried as vacuum drying.
In the present invention, described step 7) in, sintering temperature is 1070 DEG C～1095 DEG C.
In the present invention, described step 7) in, temperature retention time is 200 minutes.
In the present invention, described step 8) in, first paragraph heat treatment temperature is 900 DEG C～920 DEG C, 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 nano composite permanent magnetic material later process of the equal model of waste and old magnet steel and facilitate; Adding of phosphorus hasBe beneficial to the micro-structural and the intrinsic magnetic properties that change nano composite permanent magnetic material hard magnetic phase, simultaneously Substitute For Partial ironConsumption; And the nano composite permanent magnetic material magnetic property that utilizes separation by precipitation to obtain is high, content of rare earth is low.
A kind of nano composite permanent magnetic material, comprises neodymium, praseodymium, gadolinium, boron, copper, aluminium, yttrium, phosphorus and iron;Each constituent mass percentage is: 10～20% neodymiums, and 8～15% praseodymiums, 5～20% gadoliniums, 0.8～1.2% boron,0～0.25% bronze medal, 0～0.8% aluminium, 0.2～3% yttrium, 0～0.5% phosphorus, 39～76% iron, and iron is ironAnd 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 phosphorus and obtain mixed powder, haveEffect reduces the production cost of enterprise, and the fusing point difference that has solved each component in traditional fusion process is with artificialOperation factors and cause after melting alloy pig produce the problem of segregation, receive the adding to be conducive to change of phosphorusNd in rice composite permanent-magnetic material2Fe14The magnetic facilitation axle orientation of B phase crystal grain, thus magnetic energy product improved; And profitWith separation by precipitation obtain nano composite permanent magnetic material magnetic property high, content of rare earth is low.
Detailed description of the invention
Describe the present invention below by following specific embodiment.
Embodiment 1
A kind of nano composite permanent magnetic material, by preparing burden as following table 1-1:
Table 1-1 embodiment 1 formula table
| Component | Neodymium | Praseodymium | Gadolinium | Yttrium | Phosphorus | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 4.2 | 3.2 | 1.1 | 0.04 | 0 | 0.17 | 0 | 0 | 12.4 | 21.11 |
| Mass percent/% | 20 | 15 | 5 | 0.2 | 0 | 0.8 | 0 | 0 | 59 | 100 |
The preparation method of the above-mentioned nano composite 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 nano combined according to what preparePermanent-magnet material, directly carries out the broken powder process of hydrogen to the pretreatment magnet material obtaining, and obtains the broken magnetic of rare earth hydrogen;The broken magnetic of rare earth hydrogen obtaining is carried out to sample analysis simultaneously, obtain rare-earth magnetic component parameter, then according to dividingAnalyse the rare-earth magnetic component parameter obtaining, in the broken magnetic of rare earth hydrogen obtaining, add phosphorus and obtain mixed powder,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, adopt precipitate and separateMethod is removed pressed compact and is reacted remaining metal nanoparticle, and pressed compact is cleaned to 3～5 times in deionized water,Ultrasonic oscillation, then vacuum drying, obtains nano permanent magnetic material base substrate, then by nano permanent magnetic material base substrateBe placed in vacuum sintering furnace sintering, sintering temperature is 1070 DEG C, and is incubated 200 minutes; Then willPressed compact after sintering is cooled to 300 DEG C in vacuum sintering furnace, then is warming up to 900 DEG C and be incubated 90Minute, be again cooled to 300 DEG C, being warming up to 530 DEG C and be incubated 200 minutes, obtain nanometerComposite 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 | 455 | 78 |
Embodiment 2
A kind of nano composite permanent magnetic material, by preparing burden as following table 2-1:
Table 2-1 embodiment 2 formula tables
| Component | Neodymium | Praseodymium | Gadolinium | Yttrium | Phosphorus | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 3.8 | 2.5 | 1.68 | 0.14 | 0.01 | 0.2 | 0.02 | 0.04 | 12.6 | 21.0 |
| Mass percent/% | 18 | 12 | 8 | 0.65 | 0.05 | 1 | 0.1 | 0.2 | 60 | 100 |
The preparation method of the above-mentioned nano composite 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 nano combined according to what preparePermanent-magnet material, directly carries out the broken powder process of hydrogen to the pretreatment magnet material obtaining, and obtains the broken magnetic of rare earth hydrogen;The broken magnetic of rare earth hydrogen obtaining is carried out to sample analysis simultaneously, obtain rare-earth magnetic component parameter, then according to dividingAnalyse the rare-earth magnetic component parameter obtaining, in the broken magnetic of rare earth hydrogen obtaining, add phosphorus and obtain mixed powder,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, adopt precipitate and separateMethod is removed pressed compact and is reacted remaining metal nanoparticle, and pressed compact is cleaned to 3～5 times in deionized water,Ultrasonic oscillation, then vacuum drying, obtains nano permanent magnetic material base substrate, then by nano permanent magnetic material base substrateBe placed in vacuum sintering furnace sintering, sintering temperature is 1080 DEG C, and is incubated 200 minutes; Then willPressed compact after sintering is cooled to 310 DEG C in vacuum sintering furnace, then is warming up to 900 DEG C and be incubated 90Minute, be again cooled to 310 DEG C, being warming up to 550 DEG C and be incubated 200 minutes, obtain nanometerComposite permanent-magnetic material; 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 | 89 |
Embodiment 3
A kind of nano composite permanent magnetic material, by preparing burden as following table 3-1:
Table 3-1 embodiment 3 formula tables
| Component | Neodymium | Praseodymium | Gadolinium | Yttrium | Phosphorus | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 2.7 | 2.1 | 2.52 | 0.23 | 0.2 | 0.5 | 0.04 | 0.1 | 13.1 | 21.49 |
| Mass percent/% | 13 | 10 | 12 | 1.1 | 0.1 | 1.1 | 0.2 | 0.5 | 62 | 100 |
The preparation method of the above-mentioned nano composite 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 nano combined according to what preparePermanent-magnet material, directly carries out the broken powder process of hydrogen to the pretreatment magnet material obtaining, and obtains the broken magnetic of rare earth hydrogen;The broken magnetic of rare earth hydrogen obtaining is carried out to sample analysis simultaneously, obtain rare-earth magnetic component parameter, then according to dividingAnalyse the rare-earth magnetic component parameter obtaining, in the broken magnetic of rare earth hydrogen obtaining, add phosphorus and obtain mixed powder,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, adopt precipitate and separateMethod is removed pressed compact and is reacted remaining metal nanoparticle, and pressed compact is cleaned to 3～5 times in deionized water,Ultrasonic oscillation, then vacuum drying, obtains nano permanent magnetic material base substrate, then by nano permanent magnetic material base substrateBe placed in vacuum sintering furnace sintering, sintering temperature is 1085 DEG C, and is incubated 200 minutes; Then willPressed compact after sintering is cooled to 320 DEG C in vacuum sintering furnace, then is warming up to 910 DEG C and be incubated 90Minute, be again cooled to 320 DEG C, being warming up to 570 DEG C and be incubated 200 minutes, obtain nanometerComposite permanent-magnetic material; 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 | 534 | 103 |
Embodiment 4
A kind of nano composite permanent magnetic material, by preparing burden as following table 4-1:
Table 4-1 embodiment 4 formula tables
| Component | Neodymium | Praseodymium | Gadolinium | Yttrium | Phosphorus | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 2.1 | 1.7 | 2.1 | 0.38 | 0.04 | 0.6 | 0.04 | 0.2 | 14.3 | 21.46 |
| Mass percent/% | 10 | 8 | 10 | 1.8 | 0.2 | 1.2 | 0.2 | 0.6 | 68 | 100 |
The preparation method of the above-mentioned nano composite 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 nano combined according to what preparePermanent-magnet material, directly carries out the broken powder process of hydrogen to the pretreatment magnet material obtaining, and obtains the broken magnetic of rare earth hydrogen;The broken magnetic of rare earth hydrogen obtaining is carried out to sample analysis simultaneously, obtain rare-earth magnetic component parameter, then according to dividingAnalyse the rare-earth magnetic component parameter obtaining, in the broken magnetic of rare earth hydrogen obtaining, add phosphorus and obtain mixed powder,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, adopt precipitate and separateMethod is removed pressed compact and is reacted remaining metal nanoparticle, and pressed compact is cleaned to 3～5 times in deionized water,Ultrasonic oscillation, then vacuum drying, obtains nano permanent magnetic material base substrate, then by nano permanent magnetic material base substrateBe placed in vacuum sintering furnace sintering, sintering temperature is 1090 DEG C, and is incubated 200 minutes; Then willPressed compact after sintering is cooled to 330 DEG C in vacuum sintering furnace, then is warming up to 915 DEG C and be incubated 90Minute, be again cooled to 330 DEG C, being warming up to 590 DEG C and be incubated 200 minutes, obtain nanometerComposite permanent-magnetic material; 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 | 11.0 | 570 | 95 |
Embodiment 5
A kind of nano composite permanent magnetic material, by preparing burden as following table 5-1:
Table 5-1 embodiment 5 formula tables
| Component | Neodymium | Praseodymium | Gadolinium | Yttrium | Phosphorus | Boron | Copper | Aluminium | Iron | Add up to |
| Weight/kg | 2.1 | 1.7 | 3.2 | 0.5 | 0.08 | 0.6 | 0.04 | 0.2 | 13.0 | 21.42 |
| Mass percent/% | 10 | 8 | 15 | 2.4 | 0.4 | 1.2 | 0.2 | 0.8 | 62 | 100 |
The preparation method of the above-mentioned nano composite 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 nano combined according to what preparePermanent-magnet material, directly carries out the broken powder process of hydrogen to the pretreatment magnet material obtaining, and obtains the broken magnetic of rare earth hydrogen;The broken magnetic of rare earth hydrogen obtaining is carried out to sample analysis simultaneously, obtain rare-earth magnetic component parameter, then according to dividingAnalyse the rare-earth magnetic component parameter obtaining, in the broken magnetic of rare earth hydrogen obtaining, add phosphorus and obtain mixed powder,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, nano combined for required preparationPermanent-magnet material rare earth component and proportion requirement are added appropriate rare earth component to satisfy the demands, and are carrying out air-flowWhen mill, put into quantitative air and carry out passivation, and the powder that front and back are ground carries out mix and blend; Successively will be thinPowder adds isostatic pressing method by mold pressing and is pressed into pressed compact, and etc. the pressure of static pressure be 270MPa, green densityFor 4.5g/cm3; After treating that fine powder is all suppressed, adopt separation by precipitation to remove pressed compact and react remainingMetal nanoparticle, and pressed compact is cleaned in deionized water 3～5 times to ultrasonic oscillation, and final vacuumDry, obtain nano permanent magnetic material base substrate, then nano permanent magnetic material base substrate is placed in to vacuum sintering furnace sintering,Sintering temperature is 1095 DEG C, and is incubated 200 minutes; Then by the pressed compact after sintering in vacuum-sinteringIn stove, be cooled to 350 DEG C, then be warming up to 920 DEG C and be incubated 90 minutes, be again cooled to 350 DEG C,Being warming up to 600 DEG C and be incubated 200 minutes, obtain nano composite permanent magnetic material; Its performance testData are 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 | 617 | 92 |
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 (9)
1. in steel refuse by magnetic, add the method that phosphorus is prepared nano composite 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 the nano composite permanent magnetic material of preparation, to step 1) the middle pretreatment magnet material obtainingDirectly carry 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 phosphorus and obtain mixed powder, the quality per distribution ratio of mixed powder: the broken magnetic of 99.5～100% rare earth hydrogen, 0～0.5% phosphorus;
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, then adoptSeparation by precipitation is removed pressed compact and is reacted remaining metal nanoparticle, cleans 3～5 times, and ultrasonic oscillation,Then dry, obtain nano permanent magnetic material base substrate;
7) by step 6) in obtain nano permanent magnetic material base substrate be placed in vacuum sintering furnace sintering and carry outInsulation;
8) by step 7) in nano permanent magnetic material base substrate after sintering in vacuum sintering furnace, be cooled to300 DEG C～360 DEG C, then be warming up to first paragraph heat treatment and be incubated, then continue to be cooled to 300 DEG C～360 DEG C, be finally warming up to second segment heat treatment and be incubated, and two sections of heat treatments are carried out respectively to tempering,To obtain nano composite permanent magnetic material.
2. the phosphorus that adds in steel refuse by magnetic according to claim 1 is prepared nano composite 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 phosphorus that adds in steel refuse by magnetic according to claim 1 is prepared nano composite permanent magnetic materialMethod, is characterized in that, described step 6) in, the pressure that waits static pressure is 230～280MPa.
4. the phosphorus that adds in steel refuse by magnetic according to claim 1 is prepared nano composite permanent magnetic materialMethod, is characterized in that, described step 6) in, cleaning solution is alcohol, acetone and deionized water.
5. the phosphorus that adds in steel refuse by magnetic according to claim 1 is prepared nano composite permanent magnetic materialMethod, is characterized in that, described step 6) in, be dried as vacuum drying.
6. the phosphorus that adds in steel refuse by magnetic according to claim 1 is prepared nano composite permanent magnetic materialMethod, is characterized in that, described step 7) in, sintering temperature is 1070 DEG C～1095 DEG C.
7. the phosphorus that adds in steel refuse by magnetic according to claim 1 is prepared nano composite permanent magnetic materialMethod, is characterized in that, described step 7) in, temperature retention time is 200 minutes.
8. the phosphorus that adds in steel refuse by magnetic according to claim 1 is prepared nano composite 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.
9. prepare nano combined according to the phosphorus that adds in steel refuse by magnetic described in claim 1～8 any oneThe method of permanent-magnet material, the nano composite permanent magnetic material of preparation, is characterized in that, comprise neodymium, praseodymium, gadolinium,Boron, copper, aluminium, yttrium, phosphorus and iron; Each constituent mass percentage is: 10～20% neodymiums, and 8～15% praseodymiums,5～20% gadoliniums, 0.8～1.2% boron, 0～0.25% bronze medal, 0～0.8% aluminium, 0.2～3% yttrium, 0～0.5%Phosphorus, 39～76% iron, and iron is iron and inevitable impurity.
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