CN101045256A - Synthesizing process for regenerating rare earth permanent magnet alloy from waste alloy - Google Patents
Synthesizing process for regenerating rare earth permanent magnet alloy from waste alloy Download PDFInfo
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- CN101045256A CN101045256A CNA2006100664629A CN200610066462A CN101045256A CN 101045256 A CN101045256 A CN 101045256A CN A2006100664629 A CNA2006100664629 A CN A2006100664629A CN 200610066462 A CN200610066462 A CN 200610066462A CN 101045256 A CN101045256 A CN 101045256A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
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Abstract
A technology for regenerating magnetism of the rejected permanent-magnet RE alloy or its leftover includes such steps as adding intermediate alloy Pr18Nd15B6.5Al0.8Cu0.8 B6.5Fe58.9 or Pr13Nd20Al0.8Cu0.8B6.5Fe58.9, smelting, powdering, shaping in (1.2-2.0)-T magnetic field, vacuum microwave sintering, ageing, cooling, post-processing, and magnetizing in a 4.5-T or higher magnetic field.
Description
Technical field
The present invention relates to a kind of synthetic method of RE permanent magnetic alloy, particularly relate to a kind of waste material magnetic regeneration synthesis technique of regenerating rare earth permanent magnet alloy from waste alloy.
Background technology
Permanent-magnet alloy is a permanent-magnet material, has become one of sign of weighing country's civilization and development degree.What the magnetic property up-to-date in the permanent-magnet material, that performance is best was the highest is rare earth permanent-magnetic material.It is the intermetallic compound by combinations such as rare earth element especially Ce, Pr, Nd, Sm and magnesium-yttrium-transition metal: Co, Fe, Ni and Al, Cu, Nb, Ga and nonmetalloid C, B, obtains after suitably processing processing.
Synthesized SmCo in 1987
5Permanent-magnet alloy because the valency of Co is expensive, partly replaces Part of Co with Cu, Fe, Zr again, forms Sm, (Co, Cu, Fe, Zr)
7-8Intermetallic compound.Add that for Co B forms the new intermetallic compound of rare-earth iron-boron with Fe again after nineteen eighty-three, become third generation rare earth permanent-magnetic material, through the development of two more than ten years, the rare earth permanent-magnetic material output of China has occupied position first of the world.
In the time of among permanent-magnet material successfully is applied to computer, motor, electroacoustic apparatus, NMR, engine, transformer, people extremely are concerned about the cost problem of material, promptly under the prerequisite of excellent performance, how to reduce cost also is one of research focus, the cost of raw material accounts for variable cost 86%, accounts for 45% of total production cost.When reducing cost, people consider how to reduce utilization rate of raw materials, and existing conventional production process waste material accounts for 20-30%.Alloy from waste become product again and produce in cut down the consumption of energy, improve uniformity, the uniformity of material, this also is the several problems that exist in the current rare earth permanent-magnetic material development.
Summary of the invention
The present invention is directed to the problem in the existing above-mentioned synthesis technique, the new technique for synthesizing of provide a kind of, alloy from waste regeneration lower, saving raw material, reduce cost than energy consumption in the traditional processing technology.
New technological flow mainly comprises:
1. preparing raw material
Alloy melting rare earth metal difficulty is bigger, because rare earth metal is volatile, is earlier the rare earth metal more than 99.5% with purity, the Fe more than 99.8%, and the B-Fe alloy is inserted among the intermediate frequency furnace by prescription requirement batching.Vacuumize again, when vacuum reaches 10
-2Pa-10
-3Heat up behind the Pa again, adopt slowly during intensification and heat up, insulation is 4-9 minute during refining, lowers the temperature 150-300 ℃ again, is poured in the copper crucible of water-cooled, drops to room temperature.
2. powder process is in the pulverizer under the N gas shiled, by broken in thick, hydrogenation powder process, air-flow pulverize, fine grinding is to 3-6 micron powder.
3. the powder of above-mentioned powder process is packed in the mould, make the blank piece at the magnetic field compacted under.
4. above-mentioned blank piece is inserted microwave agglomerating furnace.Use microwave 0.1-500GH
2The micro-wave oven of frequency adds Zr in stove
84Al
16Powder and Ce, La, Pr, Nd, Pm, Ho, Tm, Yb, Lu, Sc, Sm, Eu, Ga, Tb, Dy, one or more proportionings of Er, Y.Blank after getter and the permanent magnetic alloy powder moulding is put into microwave agglomerating furnace simultaneously, extracts some out and contains the many gas of oxygen.Synthesis temperature 550-1135 ℃, be incubated 0.1-1.5 hour.Sintering is based on microwave electromagnetic field directly and the interaction of heated medium molecule in microwave agglomerating furnace, make under the effect of medium molecule in microwave electromagnetic field, produce fierce motion, form similar frictional heat, thereby the temperature that forms on the heating object macroscopic view raises.
5. timeliness: timeliness in vacuum sintering furnace, aging temp: 490-1090 ℃, time 1-2 hour.
6. sintering success, processing through the product of overaging enters after again is by the size of user's needs, be processed into required product.
7. product magnetization is magnetized in the magnet charger greater than 4.5 Gausses.
8. considerable leftover bits, the underproof waste material in sintering occur in the back processing of product, waste material is converted into product, the technology of the magnet of promptly regenerating is as follows:
(1) carries out analysis of components;
(2) fill a prescription surely according to composition, add following two kinds of any one Pr of prescription alloy
18Nd
15B
6.5Al
0.8Cu
0.8Fe
58.9Or Pr
13Nd
20Al
0.8Cu
0.8B
6.5Fe
58.9, addition is the 5-20% of alloy from waste material.
(3) melting in intermediate frequency furnace adds Zr in the smelting furnace
84Al
16Getter and rare earth metal powder such as Ce, La, Pr, Nd, Pm, Ho, Tm, Yb, Lu, Sc, Sm, Eu, Ga, Tb, Dy, one or more proportionings of Er, Y, addition is 1-7%; Vacuum is not less than 10
-2Pa;
(4) coarse crushing under the N gas shiled, through over hydrogenation powder process, air-flow is crushed to the 3-6 micron;
(5) greater than moulding in the magnetic field of 1.2-2.0T;
(6) (0.1-500GH in micro-wave oven
2) sintering, 450 ℃-1138 ℃ of sintering temperatures, sintering time is 0.2-1.2 hour;
(7) in vacuum greater than 10
-3In the vacuum sintering furnace of Pa, adopt three-stage sintering and aging technique, promptly 950-1080 ℃, 850-900 ℃, 450-650 ℃ three-stage sintering and aging technique technology, every section temperature retention time is 0.8-3 hour, makes the alloy homogenising;
(8) product after the timeliness is carried out machined;
(9) in magnetic field, magnetize, magnetize greater than 4.5 Gausses.
The specific embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
Waste material off quality behind leftover pieces and the sintering after the permanent-magnet alloy machining is mixed, after the analysis, add Pr
15Nd
18B
6.8Al
0.5Cu
0.8Fe
59.2Alloy, addition are 6.9% of molten refining waste material gross weights, insert intermediate frequency furnace, insert Zr in intermediate frequency furnace
84Al
16Getter adds La, Ce, Pr, Nd norium powder again, is evacuated down to 10
-2Pa charges into argon gas, and melting, refining 10 minutes are lowered the temperature 210 ℃, insert in the copper crucible of water-cooled.Behind the cool to room temperature, coarse crushing under the N gas shiled is arrived the 2-6 micron through over hydrogenation powder process, moulding in the magnetic field of 1.2T, and its blank is inserted 480GH
2The micro-vacuum degree greater than 10
-3Sintering temperature is 1080 ℃ in the vacuum sintering furnace of Pa, and sintering 55 minutes behind the cool to room temperature, is being inserted vacuum greater than 10
-3Sintering, timeliness in the vacuum sintering furnace of Pa.620 ℃, 960 ℃, 1060 ℃ of aging temps are timeliness half an hour respectively, cool to room temperature is undertaken magnetizing under 4.5T magnetic field after the machining by the geomery of customer requirements, measures its magnetic property: Br=1.41T, Hci=1026KA/m, (BH) max=356KJ/m
3
Embodiment 2:
With the underproof material of performance in the RE permanent magnetic alloy behind the sintering, add 8.9% Pr by analysis
18Nd
15B
6.5Al
0.8Cu
0.8Fe
58.9Alloy is inserted the intermediate frequency furnace melting, and other process conditions and method are with embodiment 1, and the measuring method of gained final products is identical with example 1, and the magnetic property that records is as follows: Br=1.26T, Hci=1426.6KA/m, (BH) max=276.8KJ/m
3
Embodiment 3:
With the leftover bits of the RE permanent magnetic alloy behind the sintering after machined, add 12.6%Pr by analysis
13Nd
20Al
0.8Cu
0.8B
6.5Fe
58.9Insert melting in the intermediate frequency furnace, other technologies are identical with embodiment 3, and it is as follows that product is measured magnetic property: Br=1.38T, Hci=1123KA/m, (BH) max=365.8KJ/m
3
Embodiment 4:
With purity is 99.5% metal Pr, Nd, and 99.8% electrical pure iron and boracic are lower than 20% ferro-boron, and chloride Dy at 0.001-2% contains 99.8% Al, Cu by Pr
1.5Nd
11.9Dy
0.5Fe
79.4Al
0.3Cu
0.3B
6.5Cl
0.1Prescription requires to prepare alloy 50kg, and alloy material is inserted in the intermediate frequency furnace, is evacuated down to 10
-3Pa, roasting refining under argon shield, refining is after 8 minutes; cooling is cast in the crystallizer of water-cooled slightly, and alloy pig is inserted coarse crushing (under the N gas shiled); being crushed to the 3-6 micron through over hydrogenation powder process, chlorine stream, is moulding in the magnetic field of 1.2T in magnetic field, and briquetting pressure is 2T/cm
2, the blank after the moulding is put into microwave (480GH
2) in the sintering furnace, put into getter around in the blank material, the getter total amount is to be sintered 2.5% of blank material.Getter is by Zr
86Al
14With La, Ce, Pr, Nd mishmetal powder constituent, shut stove, 1090 ℃ of insulations 0.45 hour, behind the taking-up material, again it is inserted the vacuum sintering furnace timeliness, 585 ℃ of aging temps, aging time 1.6 hours, 950 ℃ of timeliness 1 hour, dropping to room temperature processes after by customer requirements, magnetize under 4-5T magnetic field, obtain high performance permanent-magnet material, 20kg result is as follows in measurement: residual magnetic flux density Br=1.44T.Hci＝1000KA/m，(BH)
m＝397KJ/m
3。
But the underproof waste magnet of 30kg is arranged, its heat demagnetization back is added 20kg leftover bits 50kg altogether.By analysis, allocate Pr18Nd15B6 into.5Al0.8Cu0.8Fe58.9 alloy 3.5kg inserts in the intermediate frequency furnace, smelting technology condition and permanent-magnet alloy technology such as embodiment 1, and the magnetic property that obtains alloy is Br=1.40T, Hci=1024KA/m, (BH)
Max=388KJ/m
3
Claims (5)
1. the synthesis technique of a regenerating rare earth permanent magnet alloy from waste alloy; it is characterized in that; with underproof waste material in the leftover bits processed behind the permanent-magnet alloy and the sintering by analysis; allocate the intermediate alloy of rich rare earth into; again the material for preparing is inserted in the intermediate frequency furnace that getter and rare earth metal powder composition are housed; vacuumize applying argon gas; 1300-1460 ℃ of melting; the ingot that refining is good; under the N gas shiled, use hydrogenation powder process and airslide disintegrating mill; powder process is to the 3-5 micron; this powder is inserted moulding in the hydraulic press in 1.2-2.0T magnetic field; the blank of moulding is put into the micro-wave oven sintering, insert again and adopt three sections aging techniques to be as cold as room temperature in the vaccum sensitive stove, promptly obtain having the permanent magnet of magnetic regeneration.
2. the synthesis technique of a kind of regenerating rare earth permanent magnet alloy from waste alloy according to claim 1 is characterized in that, the rich rare earth intermediate alloy that adds in the melting forward direction waste material is Pr
18Nd
15B
6.5Al
0.8Cu
0.8Fe
58.9Or Pr
13Nd
20Al
0.8Cu
0.8B
6.5Fe
58.9, addition is alloy from waste 5-20%.
3. the synthesis technique of a kind of regenerating rare earth permanent magnet alloy from waste alloy according to claim 1 is characterized in that, its getter is by Zr
84Al
16With rare-earth elements La, Ce, Pr, Nd, Pm, Sm, Eu, Ga, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, Se one or more, addition is 1-7%.
4. the synthesis technique of a kind of regenerating rare earth permanent magnet alloy from waste alloy according to claim 1 is characterized in that, the micro-wave oven that makes in the melting is 450-1138 ℃ of the microwave agglomerating furnace sintering temperature of 0.1-500GH2 frequency, and sintering time is 0.2-1.2 hour.
5. the synthesis technique of a kind of regenerating rare earth permanent magnet alloy from waste alloy according to claim 1, it is characterized in that, when vacuum sintering furnace, adopt three-stage sintering and timeliness, be 950-1080 ℃, 850-900 ℃, 450-650 ℃ three-stage sintering and aging technique technology, every section temperature retention time is 0.8-3 hour.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508022B (en) * | 2009-01-15 | 2013-05-01 | 高为鑫 | Powder high-frequency electromagnetic wave forming method |
| CN103205543A (en) * | 2013-05-05 | 2013-07-17 | 沈阳中北真空磁电科技有限公司 | Vacuum heat treatment method and equipment for permanent NdFeB rare earth magnet device |
| CN112385006A (en) * | 2018-06-18 | 2021-02-19 | Abb瑞士股份有限公司 | Method for producing magnetic powder |
| CN114101686A (en) * | 2021-11-09 | 2022-03-01 | 中磁科技股份有限公司 | Treatment method of neodymium iron boron oxidation blank |
-
2006
- 2006-03-31 CN CNA2006100664629A patent/CN101045256A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508022B (en) * | 2009-01-15 | 2013-05-01 | 高为鑫 | Powder high-frequency electromagnetic wave forming method |
| CN103205543A (en) * | 2013-05-05 | 2013-07-17 | 沈阳中北真空磁电科技有限公司 | Vacuum heat treatment method and equipment for permanent NdFeB rare earth magnet device |
| CN112385006A (en) * | 2018-06-18 | 2021-02-19 | Abb瑞士股份有限公司 | Method for producing magnetic powder |
| CN114101686A (en) * | 2021-11-09 | 2022-03-01 | 中磁科技股份有限公司 | Treatment method of neodymium iron boron oxidation blank |
| CN114101686B (en) * | 2021-11-09 | 2023-07-25 | 中磁科技股份有限公司 | Treatment method of neodymium iron boron oxidized blank |
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Open date: 20071003 |