CN105489333A - Rare earth permanent magnet material utilizing recycled waste materials and preparation method - Google Patents
Rare earth permanent magnet material utilizing recycled waste materials and preparation method Download PDFInfo
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- CN105489333A CN105489333A CN201610001430.4A CN201610001430A CN105489333A CN 105489333 A CN105489333 A CN 105489333A CN 201610001430 A CN201610001430 A CN 201610001430A CN 105489333 A CN105489333 A CN 105489333A
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- H—ELECTRICITY
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
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- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
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- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/32—Ferrous alloys, e.g. steel alloys containing chromium with boron
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/059—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2
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Abstract
The invention provides a rare earth permanent magnet material utilizing recycled waste materials. An alloy material is high in coercivity. The preparation method is simple in process, low in production cost and suitable for industrial production. The permanent magnet material comprises the following components in percentage by mass: 18-22% of Nd, 7.2-8.8% of Y, 3.6-4.4% of Eu, 3.6-4.4% of Dy, 2-6% of B, 0.1-0.5% of P, 0.15-0.20% of Ag, 0.45-0.60% of Ni, 0.01-0.04% of Si, 0.45-0.60% of Ti and the balance of Fe; the mass ratio of Nd to Y to Eu to Dy in the permanent magnet material is 10:4:2:2; and the permanent magnet material also comprises 0.045-0.060% of N in percentage by mass.
Description
Technical field
The invention belongs to metal material field, relate to a kind of waste material reuse rare earth permanent-magnetic material and preparation method.
Background technology
CN201410725480.8 application relates to a kind of preparation method of rare earth permanent-magnetic material, this preparation method comprises the following steps: provide Re-Fe-B quenched powder and Ce base quenched powder respectively, wherein said Re-Fe-B quenched powder middle rare earth Re is Nd, Pr, Dy, one or more in Tb, the chemical formula of described Ce base quenched powder is Ce<sub>x</subGre atT.GreaT.GTFe<sub> (100-x-y-z) </sub>B<subGreat T.GreaT.GTy</sub>MLEssT.LTssT .LTsub>z</sub>, M is selected from Ga, Co, Al, Zn, Cu, one or more in Nb and Zr, x, y and z is the mass percentage of corresponding element, and 28%≤x≤35%, 0.8%≤y≤1.5%, 0%≤z≤2%, mixed with described Re-Fe-B quenched powder by described Ce base quenched powder and obtain mixing magnetic, wherein, the mass percent described in described mixing magnetic shared by Ce base quenched powder is 10-50%, described mixing magnetic is carried out successively hot-forming, thermoforming and temper, obtain rare earth permanent-magnetic material, rare earth permanent-magnetic material is many principal phases structure, and it is primarily of nano-grade crystalline substance composition.But material coercive force prepared by the method is high not enough.
Summary of the invention
Object of the present invention is exactly for above-mentioned technological deficiency, and provide waste material reuse rare earth permanent-magnetic material, this alloy material has high coercive force.
Another object of the present invention is to provide waste material reuse rare earth permanent-magnetic material preparation method, and this preparation method's technique is simple, and production cost is low, is suitable for suitability for industrialized production.
The object of the invention is to be achieved through the following technical solutions:
A kind of waste material reuse rare earth permanent-magnetic material, in this permanent magnetic material, the mass percent of each composition is: Nd18-22%, Y7.2-8.8%, Eu3.6-4.4%, Dy3.6-4.4%, B2-6%, P0.1-0.5%, Ag0.15-0.20%, Ni0.45-0.60%, Si0.01-0.04%, Ti0.45-0.60%, all the other are Fe; In this permanent magnetic material, the mass ratio of Nd, Y, Eu, Dy is 10:4:2:2; Also containing mass percentage in this permanent magnetic material is the N of 0.045-0.060%.
A preparation method for waste material reuse rare earth permanent-magnetic material, the method comprises the steps:
1) waste disposal:
A) first fluorescent powder scrap is placed in baking furnace in 500-650 DEG C of preliminary treatment 1-2 hour, ball milling obtains the fluorescent powder scrap of calcination process; By the fluorescent powder scrap of process and Na
2o mixes, and carries out high temperature alkali fuse process and obtain alkali fusion product, wherein Na in 2-4 hour under 680-710 DEG C of condition
2the fluorescent powder scrap mass ratio that O and calcination process are crossed is 4: 1-1.5; In gained alkali fusion product, add hydrochloric acid, the mass ratio of alkali fusion product and hydrochloric acid is (1-2): 1; By the mixed liquor of joining put into 65-70 DEG C of constant temperature water bath and heat 2-3h, filter afterwards, obtain the leachate containing rare earth element; Precipitation compounds after the oxalic acid solution of 125-180g/L is mixed with leachate, oxalic acid solution consumption is the 35-45% of the quality of the fluorescent powder scrap of calcination process, after washing 3-5 time with water to the compound of separating out, collecting precipitation thing 120 DEG C dries 1h, obtains sediment A stand-by;
B) by permanent magnet waste material Na
2cO
3waste oil in solution removing permanent magnet spent material, Na
2cO
3be (0.01-0.03) with the mass ratio of permanent magnet waste material: 1, the permanent magnet waste material after process after filtration and water washing 3-5 all over after under 120-125 DEG C of condition, dry 1-2 hour, the waste material after process of must deoiling; Running water is added in molten hopper, drop into the waste material after process of deoiling and stir, the waste material 0.4-0.5kg after process is dropped in every premium on currency, continue to add sulfuric acid, the waste material after process of deoiling and the mass ratio of sulfuric acid are 1: (1.1-1.4), and temperature controls at 90-95 DEG C, flood filtration in 1-3 hour, and with tap water 3-5 time, filter residue abandons, filtrate and washing lotion merge; Feed liquid after merging is placed in stirred reactor, stirs 1-2 hour at 150-200 DEG C; Then evenly add saltcake to stir and form double salt precipitation thing in 1-2 hour, the addition of saltcake is the 19-22% of the waste material quality after process of deoiling; Preparation 125-180g/L oxalic acid solution and after being warming up to 80-90 DEG C, then above-mentioned double salt precipitation thing is evenly added, make it be converted into oxalate compound to separate out, the addition of oxalic acid solution is the 45-55% of waste material quality deoiled after process, after filtration and washing 2-5 all over after, solution discards, collecting precipitation thing, dry 1 hour at the temperature of 120 DEG C, after cooling, obtain sediment B, stand-by;
C) by sediment A and sediment B with 1:(0.5-2) mass ratio mix, at the temperature of 1100-1170 DEG C, be incubated 1-2 hour, the mixed rare-earth oxide be precipitated after cooling, for subsequent use;
2) grinding batching: Nd, Y, Eu, Dy assay is carried out to the mixed rare-earth oxide that upper step obtains, measure in backward mixed rare-earth oxide and add corresponding rare earth oxide and carry out composition adjustment, after adjustment, in mixed rare-earth oxide, the mass ratio of Nd, Y, Eu, Dy is 10:4:2:2; After adjusting, mixing is ground to particle diameter is that 0.5-0.8mm obtains mixed rare-earth oxide powder;
3) electrolytic preparation mishmetal permanent magnetic material alloy: above-mentioned mixed rare-earth oxide powder is put into electrolytic furnace, and wherein electroanalysis solvent is LiF-CaF2-NaF-Na3AlF6 mixture, LiF, CaF in electroanalysis solvent
2, NaF, Na
3alF
6mass fraction be respectively 60-65%, 20-25%, 0.1-0.4%, surplus; The mass ratio of electroanalysis solvent and mixed rare-earth oxide powder is (5-6): 1, and the current strength of electrolytic furnace is 75A, and working temperature is 960-1200 DEG C, electrolysis 20-30 minute, obtains mishmetal permanent magnetic material alloy;
4) mishmetal permanent magnetic material alloy pig is prepared: prepare burden according to following mass percent: Nd18-22%, Y7.2-8.8%, Eu3.6-4.4%, Dy3.6-4.4%, B2-6%, P0.1-0.5%, Ag0.15-0.20%, Ni0.45-0.60%, Si0.01-0.04%, Ti0.45-0.60%, all the other are Fe, and wherein Ag, Ni, Ti add in simple metal mode, B is being that the ferroboron mode of 25% adds containing B mass percent, Si adds in pure monocrystalline silicon mode, and P adds with the form of the ferrorphosphorus of phosphorus content mass fraction 25%, and surplus Fe adds in simple metal mode; Nd, Y, Eu, Dy add with the mishmetal permanent magnetic material alloy form of above-mentioned electrolytic preparation; Joined by the raw material prepared in the crucible in vaccum sensitive stove, be heated to 1540-1590 DEG C, be incubated and pour in ingot mould after 20 minutes, cooling obtains mishmetal permanent magnetic material alloy pig naturally;
5) make band, nitriding, powder process, die mould, sintering: by above-mentioned mishmetal permanent magnetic material alloy pig through making band, namely nitriding, powder process, compressing, sintering process obtain waste material reuse rare earth permanent-magnetic material.
Further design of the present invention is:
In step 1, the concentration of hydrochloric acid used is 6-10mol/L; Na used
2cO
3the mass fraction of solution is 10-15%; The concentration of sulfuric acid used is 10mol/L.
In step 5), during system band, first the remelting tubular type crucible that mishmetal permanent magnetic material alloy pig step 4) obtained puts into vacuum induction forming furnace carries out remelting, remelting temperature is 1570-1590 DEG C, the bottom of remelting tubular type crucible is placed in 2-4mm place on vacuum induction quick quenching furnace runner wheel rim, the aluminium alloy of melting under ar gas acting from the hole of crucible bottom ejection and with the runner EDGE CONTACT rotated, formation thickness is 550-650 μm, width is the alloy strip of 12-15mm, and the linear velocity of runner wheel rim is 16-19m/s.
In step 5), when nitriding and powder process, alloy strip is put into nitriding furnace, the ammonia flow of nitriding furnace is 5-10L/min, is warming up to 400-450 DEG C, insulation 10-15min, takes out with after stove cooling; After alloy band stirs, put into nitriding furnace again, be warming up to 400-450 DEG C, insulation 10-15min, the ammonia flow of nitriding furnace is 5-10L/min, and cooling after process, then to cooled nitro-alloy band coarse crushing 2-4mm, then put it into the ball mill grinding 18-22 hour being filled with nitrogen, obtain particle mean size at the powder of 3-5 μm.
In step 5), during compressing, sintering process, above-mentioned obtained powder is put into press die, makes type at 2-3T pressure, the sintering furnace that compacting base is placed in 1080-1190 DEG C is sintered 2-5 hour, sintering furnace vacuum level requirements is less than 0.1Pa, be warming up to 750-950 DEG C again after cooling, insulation 3-10h tempering, is then cooled to room temperature, finally being again warming up to 400-680 DEG C carries out 3-6h Ageing Treatment, is cooled to room temperature and obtains magnet after process; Then magnet is placed in the heat-treatment furnace that magnetic field intensity is 5-7T, cools with stove after 1050-1120 DEG C of temperature 1-3h under vacuum condition, namely obtain waste material reuse rare earth permanent-magnetic material.
Compared with prior art, remarkable advantage of the present invention is:
Owing to there being the existence of multiple rare earth element in material of the present invention, therefore form Nd in the tissue
2fe
14b, Eu
2fe
14b, Dy
2fe
14b, Y
2fe
14multiple magnetic principal phase such as B.When the mass ratio of Nd, Y, Eu, Dy is 10:4:2:2, principal crystalline phase Nd
2fe
14can by principal crystalline phases different in addition as Dy between B crystal grain
2fe
14b, Eu
2fe
14b, Y
2fe
14b etc. separated, and so just can change single principal phase Nd
2fe
14direct exchange interaction between B crystal grain.In addition, the existence of multiple principal phase, can improve exchange coupling pinning field H, reduces the loose magnetic field of material internal, improves magnet serviceability at high temperature.This effect can make magnet coercive force improve.
Nonmagnetic Nd-rich phase in magnetic material plays a part to dilute whole magnet magnetic moment, and its existence in magnet actually reduces the magnetic property of the unit volume of permanent magnet.And the effect being solid-solubilized in Dy, Eu in iron-based body in material of the present invention makes uniform crystal particles, refinement, regularization.This makes nonmagnetic Nd-rich phase can be evenly distributed on the crystal boundary of principal phase, avoids Nd-rich phase with large block appearance.P, Ti, Y can crystal grain thinnings, thus improve remanent magnetism and coercive force.
In material of the present invention, give full play to the complementary effect of N and B.Due to the introducing of nitrogen, make ferroelectric son free and accelerate localization, magnetic moment increases, and Curie temperature also rises, and anisotropy is strengthened.Nitrogen occupies specific gap crystal site in the structure, can regulate the crystal field effect of rare earth 4f electronics and the band structure of iron 3d electronics delicately, thus the atomic magnetic moment of iron is increased, and makes the crystal field effect generation basic change of rare earth 4f electronics.N and Nd can form new phase, is in Nd
2fe
14the border of B principal crystalline phase, has and improves the coercitive effect of magnet.
Ni, Si itself have high stability, have high-temperature oxidation resistance.Add Ni element significantly to improve the temperature stability of material and expand operating temperature range.Y and Ag combines the corrosion resistance not only can improving material, and can improve exchange coupling pinning field H, ensures the stability of material.
Compared with prior art, permanent magnetic material of the present invention has uniform tissue, and strong strong structure, both can improve the anti-corrosion capability of material, and magnetic property makes moderate progress.Permanent magnetic material of the present invention has good stability and practicality, can be widely used in the every field such as electronic device, aeronautical and space technology, computer equipment, magnetic separator, communication apparatus, Medical Devices, electric bicycle, electronic toy.
The preparation method of permanent magnetic material of the present invention takes full advantage of waste material directly as alloy raw material, composition proportion is flexible, quality control puts in place, and can reduce costs, technique utilizes hyperoxic powder scrap simply, fully, environmental protection, effectively environmental protect, have very high social value.
Accompanying drawing explanation
Fig. 1 is the waste material reuse rare earth permanent-magnetic material organization chart that the embodiment of the present invention one obtains.
As seen from Figure 1, material structure dense uniform of the present invention.
Embodiment
Raw materials used as follows in following instance:
1, fluorescent powder scrap used derives from the cathodic ray-tube fluorescent powder waste material of recovery.
In this waste material, the mass fraction of each composition is: Y
2o
324-26%, Eu
2o
31-2.5%, Al
2o
34-6%, PbO1-2.5%, all the other ZnS.
2, permanent magnet waste material used derives from the waste material that manufacturer production permanent magnet product produces.
In this permanent magnet waste material, the mass fraction of each composition is: neodymium 9%-32.5%, boron 2.8-3.6%, protactinium 0.6-1.2%, palladium 0.05-0.08%, and surplus is iron.
Embodiment one:
The preparation method of waste material reuse rare earth permanent-magnetic material of the present invention, the method comprises the steps:
1) waste disposal:
A) first fluorescent powder scrap is placed in baking furnace in 620 DEG C of preliminary treatment 2 hours, is then milled to 20-80 micron, obtains the fluorescent powder scrap of calcination process; By the fluorescent powder scrap of process and Na
2o mixes, and carries out high temperature alkali fuse process and obtain alkali fusion product, wherein Na in 3 hours under 700 DEG C of conditions
2the fluorescent powder scrap mass ratio that O and calcination process are crossed is 4: 1.5; In gained alkali fusion product, add 8mol/L(concentration is 6-10mol/L) hydrochloric acid, the mass ratio of alkali fusion product and hydrochloric acid is 1:1; By the mixed liquor of joining put into 65 DEG C of constant temperature water baths and heat 2h, filter afterwards, obtain the leachate containing rare earth element; The oxalic acid solution getting 130g/L mixes rear precipitation compounds with leachate, oxalic acid solution consumption is 35% of the quality of the fluorescent powder scrap of calcination process, and after washing 3 times with water to the compound of separating out, collecting precipitation thing 120 DEG C dries 1h, obtains sediment A stand-by;
B) be the Na of 15% by permanent magnet waste material mass fraction
2cO
3waste oil in solution cleaning removing permanent magnet spent material, Na
2cO
3be 0.03:1 with the mass ratio of permanent magnet waste material, the permanent magnet waste material after process is dried 2 hours after filtration and after water washing 5 times under 125 DEG C of conditions, the waste material after process of must deoiling; Running water is added in molten hopper, drop into the waste material after process of deoiling and stir, the waste material 0.5kg after process is dropped in every premium on currency, continue to add sulfuric acid, the waste material after process of deoiling and the mass ratio of sulfuric acid (concentration 10mol/L) are 1: 1.4, and temperature controls at 95 DEG C, flood filtration in 2 hours, and with tap water 5 times, filter residue abandons, and filtrate and washing lotion merge; Feed liquid after merging is placed in stirred reactor, stirs 2 hours at 180 DEG C; Then evenly add saltcake and stir 2 hours formation double salt precipitation things, the addition of saltcake is 22% of the waste material quality after processing of deoiling; Preparation 150g/L oxalic acid solution and after being warming up to 80 DEG C, then above-mentioned double salt precipitation thing is evenly added, make it be converted into oxalate compound to separate out, the addition of oxalic acid solution be deoil process after waste material quality 50%, after filtration and washing 3 times after, solution discards, collecting precipitation thing, dry 1 hour at the temperature of 120 DEG C, after cooling, obtain sediment B, stand-by;
C) sediment A and sediment B are mixed with the mass ratio of 1:2, at the temperature of 1150 DEG C, be incubated 2 hours, after cooling, be precipitated mixed rare-earth oxide, for subsequent use;
2) grinding batching: Nd, Y, Eu, Dy assay is carried out to the mixed rare-earth oxide that upper step obtains, measure in backward mixed rare-earth oxide and add corresponding rare earth oxide (dysprosia powder, neodymia powder, yittrium oxide powder and europium oxide) and carry out composition adjustment, after adjustment, in mixed rare-earth oxide, the mass ratio of Nd, Y, Eu, Dy is 10:4:2:2; After adjusting, mixing is ground to particle diameter is that 0.5-0.8mm obtains mixed rare-earth oxide powder;
3) electrolytic preparation mishmetal permanent magnetic material alloy: above-mentioned mixed rare-earth oxide powder is put into electrolytic furnace, wherein electroanalysis solvent is LiF-CaF2-NaF-Na3AlF6 mixture, (LiF, CaF in electroanalysis solvent
2, NaF, Na
3alF
6mass fraction be respectively 60-65%, 20-25%, 0.1-0.4%, surplus); The mass ratio of electroanalysis solvent and mixed rare-earth oxide powder is 5:1, and the current strength of electrolytic furnace is 75A, and working temperature is 1000 DEG C, and electrolysis 30 minutes obtains mishmetal permanent magnetic material alloy;
4) prepare mishmetal permanent magnetic material alloy pig: prepare burden according to following mass percent: Nd18%, Y7.2%, Eu3.6%, Dy3.6%, B2%, P0.1%, Ag0.15%, Ni0.45%, Si0.01%, Ti0.45%, all the other are Fe.Wherein Ag, Ni, Ti add in simple metal mode, and B is to be that the ferroboron mode of 25% adds containing B mass percent, and Si adds in pure monocrystalline silicon mode, and P adds with the form of the ferrorphosphorus of phosphorus content mass fraction 25%, and surplus Fe adds in simple metal mode; Nd, Y, Eu, Dy add with the mishmetal permanent magnetic material alloy form of above-mentioned electrolytic preparation, and wherein the mass ratio of Nd, Y, Eu, Dy is 10:4:2:2; Joined by the raw material prepared in the crucible in vaccum sensitive stove, be heated to 1550 DEG C, be incubated and pour in ingot mould after 20 minutes, cooling obtains mishmetal permanent magnetic material alloy pig naturally;
5) make band, nitriding, powder process, die mould, sintering: by above-mentioned mishmetal permanent magnetic material alloy pig through making band, namely nitriding, powder process, compressing, sintering process obtain waste material reuse rare earth permanent-magnetic material.
During system band, first the remelting tubular type crucible that mishmetal permanent magnetic material alloy pig step 4) obtained puts into vacuum induction forming furnace carries out remelting, remelting temperature is 1580 DEG C, the bottom of remelting tubular type crucible is placed in 2-4mm place on vacuum induction quick quenching furnace runner wheel rim, the aluminium alloy of melting under ar gas acting from the hole of crucible bottom ejection and with the runner EDGE CONTACT rotated, formation thickness is 550-650 μm, width is the alloy strip of 12-15mm, and the linear velocity of runner wheel rim is 18m/s.
When nitriding and powder process, alloy strip is put into nitriding furnace, the ammonia flow of nitriding furnace is 8L/min, is warming up to 450 DEG C, insulation 15min, takes out with after stove cooling; After alloy band stirs, put into nitriding furnace again, be warming up to 450 DEG C, insulation 15min, the ammonia flow of nitriding furnace is 5L/min, and cooling after process, then by cooled nitro-alloy band coarse crushing 2-4mm, then put it into the ball mill grinding 20 hours being filled with nitrogen, obtain particle mean size at the powder of 3-5 μm.In material after process, N mass percentage is 0.045%.
During compressing, sintering process, above-mentioned obtained powder is put into press die, type is made at 2.5T pressure, the sintering furnace that compacting base is placed in 1180 DEG C is sintered 4 hours, and sintering furnace vacuum level requirements is less than 0.1Pa, is warming up to 850 DEG C again after cooling, insulation 10h tempering, then be cooled to room temperature, be finally again warming up to 600 DEG C and carry out 5h Ageing Treatment, be cooled to room temperature after process and obtain magnet; Then magnet is placed in the heat-treatment furnace that magnetic field intensity is 6T, with stove cooling after the lower 1100 DEG C of temperature 2h of vacuum condition, namely obtains waste material reuse rare earth permanent-magnetic material.
Embodiment two:
The preparation method of waste material reuse rare earth permanent-magnetic material of the present invention, the method comprises the steps:
1) waste disposal:
A) first fluorescent powder scrap is placed in baking furnace in 550 DEG C of preliminary treatment 1 hour, is then milled to 20-80 micron, obtains the fluorescent powder scrap of calcination process; By the fluorescent powder scrap of process and Na
2o mixes, and carries out high temperature alkali fuse process and obtain alkali fusion product, wherein Na in 2 hours under 690 DEG C of conditions
2the fluorescent powder scrap mass ratio that O and calcination process are crossed is 4: 1; In gained alkali fusion product, add 6mol/L hydrochloric acid, the mass ratio of alkali fusion product and hydrochloric acid is 1:1; By the mixed liquor of joining put into 65 DEG C of constant temperature water baths and heat 2h, filter afterwards, obtain the leachate containing rare earth element; Precipitation compounds after the oxalic acid solution of 125g/L is mixed with leachate, oxalic acid solution consumption is 35% of the quality of the fluorescent powder scrap of calcination process, and after washing 3 times with water to the compound of separating out, collecting precipitation thing 120 DEG C dries 1h, obtains sediment A stand-by;
B) be the Na of 10 by permanent magnet waste material mass fraction
2cO
3waste oil in solution removing permanent magnet spent material, Na
2cO
3be 0.01:1 with the mass ratio of permanent magnet waste material, the permanent magnet waste material after process is dried 1 hour after filtration and after water washing 3 times under 120 DEG C of conditions, the waste material after process of must deoiling; Running water is added in molten hopper, drop into the waste material after process of deoiling and stir, the waste material 0.4kg after process is dropped in every premium on currency, continue to add 10mol/L sulfuric acid, the waste material after process of deoiling and the mass ratio of sulfuric acid are 1: 1.2, and temperature controls at 90 DEG C, flood filtration in 1 hour, and with tap water 3 times, filter residue abandons, and filtrate and washing lotion merge; Feed liquid after merging is placed in stirred reactor, stirs 1 hour at 150 DEG C; Then evenly add saltcake and stir 1 hour formation double salt precipitation thing, the addition of saltcake is 20% of the waste material quality after processing of deoiling; Preparation 125g/L oxalic acid solution and after being warming up to 90 DEG C, then above-mentioned double salt precipitation thing is evenly added, make it be converted into oxalate compound to separate out, the addition of oxalic acid solution be deoil process after waste material quality 45%, after filtration and washing 2 times after, solution discards, collecting precipitation thing, dry 1 hour at the temperature of 120 DEG C, after cooling, obtain sediment B, stand-by;
C) sediment A and sediment B are mixed with 1:0.8 mass ratio, at the temperature of 1120 DEG C, be incubated 1 hour, the mixed rare-earth oxide be precipitated after cooling, for subsequent use;
2) grinding batching: Nd, Y, Eu, Dy assay is carried out to the mixed rare-earth oxide that upper step obtains, measure in backward mixed rare-earth oxide and add corresponding rare earth oxide (dysprosia powder, neodymia powder, yittrium oxide powder and europium oxide) and carry out composition adjustment, after adjustment, in mixed rare-earth oxide, the mass ratio of Nd, Y, Eu, Dy is 10:4:2:2; After adjusting, mixing is ground to particle diameter is that 0.5-0.8mm obtains mixed rare-earth oxide powder;
3) electrolytic preparation mishmetal permanent magnetic material alloy: above-mentioned mixed rare-earth oxide powder is put into electrolytic furnace, wherein electroanalysis solvent is LiF-CaF2-NaF-Na3AlF6 mixture (LiF, CaF in electroanalysis solvent
2, NaF, Na
3alF
6mass fraction be respectively 60-65%, 20-25%, 0.1-0.4%, surplus); The mass ratio of electroanalysis solvent and mixed rare-earth oxide powder is 6:1, and the current strength of electrolytic furnace is 75A, and working temperature is 960 DEG C, and electrolysis 20 minutes obtains mishmetal permanent magnetic material alloy;
4) prepare mishmetal permanent magnetic material alloy pig: prepare burden according to following mass percent: Nd22%, Y8.8%, Eu4.4%, Dy4.4%, B6%, P0.5%, Ag0.20%, Ni0.60%, Si0.04%, Ti0.60%, all the other are Fe.Wherein Ag, Ni, Ti add in simple metal mode, and B is to be that the ferroboron mode of 25% adds containing B mass percent, and Si adds in pure monocrystalline silicon mode, and P adds with the form of the ferrorphosphorus of phosphorus content mass fraction 25%, and surplus Fe adds in simple metal mode; Nd, Y, Eu, Dy add with the mishmetal permanent magnetic material alloy form of above-mentioned electrolytic preparation, and wherein the mass ratio of Nd, Y, Eu, Dy is 10:4:2:2; Joined by the raw material prepared in the crucible in vaccum sensitive stove, be heated to 1550 DEG C, be incubated and pour in ingot mould after 20 minutes, cooling obtains mishmetal permanent magnetic material alloy pig naturally;
5) make band, nitriding, powder process, die mould, sintering: by above-mentioned mishmetal permanent magnetic material alloy pig through making band, namely nitriding, powder process, compressing, sintering process obtain waste material reuse rare earth permanent-magnetic material.
During system band, first the remelting tubular type crucible that mishmetal permanent magnetic material alloy pig step 4) obtained puts into vacuum induction forming furnace carries out remelting, remelting temperature is 1570 DEG C, the bottom of remelting tubular type crucible is placed in 2-4mm place on vacuum induction quick quenching furnace runner wheel rim, the aluminium alloy of melting under ar gas acting from the hole of crucible bottom ejection and with the runner EDGE CONTACT rotated, formation thickness is 550-650 μm, width is the alloy strip of 12-15mm, and the linear velocity of runner wheel rim is 16m/s.
When nitriding and powder process, alloy strip is put into nitriding furnace, the ammonia flow of nitriding furnace is 10L/min, is warming up to 430 DEG C, insulation 15min, takes out with after stove cooling; After alloy band stirs, put into nitriding furnace again, be warming up to 420 DEG C, insulation 10min, the ammonia flow of nitriding furnace is 10L/min, and cooling after process, then to cooled nitro-alloy band coarse crushing 2-4mm, then put it into the ball mill grinding 20 hours being filled with nitrogen, obtain particle mean size at the powder of 3-5 μm.In material after process, N mass percentage is 0.060%.
During compressing, sintering process, above-mentioned obtained powder is put into press die, type is made at 2T pressure, the sintering furnace that compacting base is placed in 1080 DEG C is sintered 2 hours, and sintering furnace vacuum level requirements is less than 0.1Pa, is warming up to 750 DEG C again after cooling, insulation 3h tempering, then be cooled to room temperature, be finally again warming up to 580 DEG C and carry out 35h Ageing Treatment, be cooled to room temperature after process and obtain magnet; Then magnet is placed in the heat-treatment furnace that magnetic field intensity is 5T, with stove cooling after the lower 1050 DEG C of temperature 2h of vacuum condition, namely obtains waste material reuse rare earth permanent-magnetic material.
Embodiment three:
Mishmetal permanent magnetic material alloy pig in this example: prepare burden according to following mass percent: Nd20%, Y8%, Eu4%, Dy4%, B4%, P0.3%, Ag0.175%, Ni0.5%, Si0.025%, Ti0.5%, all the other are Fe.All the other conditions and preparation process are with embodiment one.In material after process, N mass percentage is 0.050%.
Embodiment four: this example proportioning components is not in scope of design of the present invention
Mishmetal permanent magnetic material alloy pig in this example: prepare burden according to following mass percent: Nd16%, Y6.4%, Eu3.2%, Dy3.2%, B1.5%, P0.05%, Ag0.10%, Ni0.40%, Si0.005%, Ti0.35%, all the other are Fe.All the other conditions and preparation process are with embodiment one.In material after process, N mass percentage is 0.040%.
Embodiment five: this example proportioning components is not in scope of design of the present invention
Mishmetal permanent magnetic material alloy pig in this example: prepare burden according to following mass percent: Nd25%, Y10%, Eu5%, Dy5%, B7%, P0.6%, Ag0.3%, Ni0.70%, Si0.05%, Ti0.7%, all the other are Fe.All the other conditions and preparation process are with embodiment two.In material after process, N mass percentage is 0.070%.
Material property of the present invention sees the following form:
As can be seen from the above table, material of the present invention increases with Nd, Y, Eu, Dy, P, B, N, Ag, Ni, Si, and the magnetic performance of material is all in raising.But the mutual restraint between element can be caused too much, have impact on the combination property of material on the contrary.
Claims (6)
1. a waste material reuse rare earth permanent-magnetic material, it is characterized in that: in this permanent magnetic material, the mass percent of each composition is: Nd18-22%, Y7.2-8.8%, Eu3.6-4.4%, Dy3.6-4.4%, B2-6%, P0.1-0.5%, Ag0.15-0.20%, Ni0.45-0.60%, Si0.01-0.04%, Ti0.45-0.60%, all the other are Fe; In this permanent magnetic material, the mass ratio of Nd, Y, Eu, Dy is 10:4:2:2; Also containing mass percentage in this permanent magnetic material is the N of 0.045-0.060%.
2. a preparation method for waste material reuse rare earth permanent-magnetic material, is characterized in that: the method comprises the steps:
1) waste disposal:
A) first fluorescent powder scrap is placed in baking furnace in 500-650 DEG C of preliminary treatment 1-2 hour, ball milling obtains the fluorescent powder scrap of calcination process; By the fluorescent powder scrap of process and Na
2o mixes, and carries out high temperature alkali fuse process and obtain alkali fusion product, wherein Na in 2-4 hour under 680-710 DEG C of condition
2the fluorescent powder scrap mass ratio that O and calcination process are crossed is 4: 1-1.5; In gained alkali fusion product, add hydrochloric acid, the mass ratio of alkali fusion product and hydrochloric acid is (1-2): 1; By the mixed liquor of joining put into 65-70 DEG C of constant temperature water bath and heat 2-3h, filter afterwards, obtain the leachate containing rare earth element; Precipitation compounds after the oxalic acid solution of 125-180g/L is mixed with leachate, oxalic acid solution consumption is the 35-45% of the quality of the fluorescent powder scrap of calcination process, after washing 3-5 time with water to the compound of separating out, collecting precipitation thing 120 DEG C dries 1h, obtains sediment A stand-by;
B) by permanent magnet waste material Na
2cO
3waste oil in solution removing permanent magnet spent material, Na
2cO
3be (0.01-0.03) with the mass ratio of permanent magnet waste material: 1, the permanent magnet waste material after process after filtration and water washing 3-5 all over after under 120-125 DEG C of condition, dry 1-2 hour, the waste material after process of must deoiling; Running water is added in molten hopper, drop into the waste material after process of deoiling and stir, the waste material 0.4-0.5kg after process is dropped in every premium on currency, continue to add sulfuric acid, the waste material after process of deoiling and the mass ratio of sulfuric acid are 1: (1.1-1.4), and temperature controls at 90-95 DEG C, flood filtration in 1-3 hour, and with tap water 3-5 time, filter residue abandons, filtrate and washing lotion merge; Feed liquid after merging is placed in stirred reactor, stirs 1-2 hour at 150-200 DEG C; Then evenly add saltcake to stir and form double salt precipitation thing in 1-2 hour, the addition of saltcake is the 19-22% of the waste material quality after process of deoiling; Preparation 125-180g/L oxalic acid solution and after being warming up to 80-90 DEG C, then above-mentioned double salt precipitation thing is evenly added, make it be converted into oxalate compound to separate out, the addition of oxalic acid solution is the 45-55% of waste material quality deoiled after process, after filtration and washing 2-5 all over after, solution discards, collecting precipitation thing, dry 1 hour at the temperature of 120 DEG C, after cooling, obtain sediment B, stand-by;
C) by sediment A and sediment B with 1:(0.5-2) mass ratio mix, at the temperature of 1100-1170 DEG C, be incubated 1-2 hour, the mixed rare-earth oxide be precipitated after cooling, for subsequent use;
2) grinding batching: Nd, Y, Eu, Dy assay is carried out to the mixed rare-earth oxide that upper step obtains, measure in backward mixed rare-earth oxide and add corresponding rare earth oxide and carry out composition adjustment, after adjustment, in mixed rare-earth oxide, the mass ratio of Nd, Y, Eu, Dy is 10:4:2:2; After adjusting, mixing is ground to particle diameter is that 0.5-0.8mm obtains mixed rare-earth oxide powder;
3) electrolytic preparation mishmetal permanent magnetic material alloy: above-mentioned mixed rare-earth oxide powder is put into electrolytic furnace, wherein electroanalysis solvent is LiF-CaF2-NaF-Na3AlF6 mixture; The mass ratio of electroanalysis solvent and mixed rare-earth oxide powder is (5-6): 1, and the current strength of electrolytic furnace is 75A, and working temperature is 960-1200 DEG C, electrolysis 20-30 minute, obtains mishmetal permanent magnetic material alloy;
4) mishmetal permanent magnetic material alloy pig is prepared: prepare burden according to following mass percent: Nd18-22%, Y7.2-8.8%, Eu3.6-4.4%, Dy3.6-4.4%, B2-6%, P0.1-0.5%, Ag0.15-0.20%, Ni0.45-0.60%, Si0.01-0.04%, Ti0.45-0.60%, all the other are Fe, and wherein Ag, Ni, Ti add in simple metal mode, B is being that the ferroboron mode of 25% adds containing B mass percent, Si adds in pure monocrystalline silicon mode, and P adds with the form of the ferrorphosphorus of phosphorus content mass fraction 25%, and surplus Fe adds in simple metal mode; Nd, Y, Eu, Dy add with the mishmetal permanent magnetic material alloy form of above-mentioned electrolytic preparation; Joined by the raw material prepared in the crucible in vaccum sensitive stove, be heated to 1540-1590 DEG C, be incubated and pour in ingot mould after 20 minutes, cooling obtains mishmetal permanent magnetic material alloy pig naturally;
5) make band, nitriding, powder process, die mould, sintering: by above-mentioned mishmetal permanent magnetic material alloy pig through making band, namely nitriding, powder process, compressing, sintering process obtain waste material reuse rare earth permanent-magnetic material.
3. the preparation method of waste material reuse rare earth permanent-magnetic material according to claim 2, it is characterized in that: in step 1, the concentration of hydrochloric acid used is 6-10mol/L; Na used
2cO
3the mass fraction of solution is 10-15%; The concentration of sulfuric acid used is 10mol/L.
4. the preparation method of waste material reuse rare earth permanent-magnetic material according to claim 2, it is characterized in that: in step 5), during system band, first the remelting tubular type crucible that mishmetal permanent magnetic material alloy pig step 4) obtained puts into vacuum induction forming furnace carries out remelting, remelting temperature is 1570-1590 DEG C, the bottom of remelting tubular type crucible is placed in 2-4mm place on vacuum induction quick quenching furnace runner wheel rim, the aluminium alloy of melting under ar gas acting from the hole of crucible bottom ejection and with the runner EDGE CONTACT rotated, formation thickness is 550-650 μm, width is the alloy strip of 12-15mm, the linear velocity of runner wheel rim is 16-19m/s.
5. the preparation method of waste material reuse rare earth permanent-magnetic material according to claim 4, is characterized in that: in step 5), when nitriding and powder process, alloy strip is put into nitriding furnace, and the ammonia flow of nitriding furnace is 5-10L/min, is warming up to 400-450 DEG C, insulation 10-15min, takes out with after stove cooling; After alloy band stirs, put into nitriding furnace again, be warming up to 400-450 DEG C, insulation 10-15min, the ammonia flow of nitriding furnace is 5-10L/min, and cooling after process, then to cooled nitro-alloy band coarse crushing 2-4mm, then put it into the ball mill grinding 18-22 hour being filled with nitrogen, obtain particle mean size at the powder of 3-5 μm.
6. the preparation method of waste material reuse rare earth permanent-magnetic material according to claim 5, it is characterized in that: in step 5), during compressing, sintering process, above-mentioned obtained powder is put into press die, type is made at 2-3T pressure, the sintering furnace that compacting base is placed in 1080-1190 DEG C is sintered 2-5 hour, sintering furnace vacuum level requirements is less than 0.1Pa, 750-950 DEG C is warming up to again after cooling, insulation 3-10h tempering, then be cooled to room temperature, be finally again warming up to 400-680 DEG C and carry out 3-6h Ageing Treatment, be cooled to room temperature after process and obtain magnet; Then magnet is placed in the heat-treatment furnace that magnetic field intensity is 5-7T, cools with stove after 1050-1120 DEG C of temperature 1-3h under vacuum condition, namely obtain waste material reuse rare earth permanent-magnetic material.
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