CN101615462A - The preparation method who contains trace nitrogen Re-Fe-B series permanent magnetic material - Google Patents
The preparation method who contains trace nitrogen Re-Fe-B series permanent magnetic material Download PDFInfo
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Abstract
The present invention relates to contain the preparation method of trace nitrogen Re-Fe-B series permanent magnetic material; comprise step (1) with raw material by component design requirement batching, (2) rapid hardening scale, (3) hydrogen is pulverized; (4) the middle fragmentation of low temperature nitrogen protection or argon shield; (5) airflow milling of low temperature nitrogen protection or argon shield, (6) batch mixing, (7) moulding; (8) sintering; (9) timeliness, (10) processing detects, and all material conversion processes adopt hermetically sealed control.The Re-Fe-B of the present invention's preparation is that rare-earth permanent magnet only contains trace nitrogen, and the antiseptic property of magnet improves greatly.
Description
Technical field
The present invention relates to a kind of preparation method of rare earth permanent-magnetic material, be specifically related to the method that a kind of preparation contains trace nitrogen Re-Fe-B series permanent magnetic material.
Background technology
With Re
2Fe
14The Type B compound is that the sintering Re-Fe-B of principal phase is a rare earth magnet, as peak performance in the permanent magnetic material and known, has been widely used in fields such as the energy, traffic, machinery, medical treatment, computer, household electrical appliances.For adapting to light, thin, the little development of demand trend of current product, require magnet performance significantly to improve.Be used to adopt the hydrogen crush method to make high performance sintered Re-Fe-B series permanent magnetic material in the prior art at present, nitrogen content can not be controlled in the 300ppm.Employing still has the amounts of hydrogen of 800-2000ppm to be retained in the hydrogenation powder scale strip (SC) alloy is inhaled the hydrogen fragmentation under hydrogen atmosphere after, because of storing, hydrogen greatly reduces the temperature that the neodymium iron boron compound is inhaled nitrogen in the hydrogenation powder, the nitrogen of suction phenomenon is just arranged in the time of 50 ℃ basically, even just begin to react for 30 ℃ with nitrogen at high pressure (during 0.6-0.8Mpa).
The preparation method who adopts is at present: 1 raw material → 2 rapid hardening strips → 3 hydrogen are pulverized broken 5 airflow milling → 6 batch mixings → 7 moulding → 8 sintering → 9 timeliness in → 4 → 10 processing and are detected.In the process of fragmentation since the 4th step, airflow milling, batch mixing, moulding, sintering, the capital contacts with nitrogen and nitrogen content is progressively increased, thereby make magnet reach the nitrogen content of 400-2000ppm, also can only guarantee nitrogen content under the hermetically sealed process conditions in 436-675ppm openly adopting, thereby the performance that influences magnet improves and the improvement of antiseptic property.Just mentioning nitrogen at present in patent documentation is inevitable existence as impurity element at magnet, does not all point out to make magnet to contain trace nitrogen (≤300ppm) effect and make magnet contain trace nitrogen (≤300ppm) manufacture method.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, the Re-Fe-B that a kind of preparation is provided is that rare-earth permanent magnet only contains trace nitrogen, and the preparation method that improves greatly of the antiseptic property of magnet.
The present invention is achieved by the following technical solutions:
The preparation method who contains trace nitrogen Re-Fe-B series permanent magnetic material comprises that step (1) prepares burden raw material by the component design requirement; (2) rapid hardening strip; (3) the rapid hardening strip is put into rotary hydrogenation stove, inhale hydrogen dehydrogenation again, adopt the air-cooled or water-cooled of reactor to make hydrogenation powder cool to room temperature after dehydrogenation is intact; (4) make the hydrogenation powder further levigate to 20 orders with equipment such as paddle-type mill or taper thread grindings; (5) utilize air-flow that powder particle is accelerated to the fine powder that velocity of sound makes it to wear into 2.8-4um; (6) powder compaction is become pressed compact; (7) with pressed compact sintering in vacuum sintering furnace; (8) two-stage in vacuum sintering furnace of the pressed compact behind the sintering is heat-treated, in the described step (3) the rapid hardening strip is put into rotary hydrogenation stove, being warming up to 100～200 ℃ of insulations, to charge into dividing potential drop in 30～60 minutes be that 0.03～0.05 ar gas environment is inhaled hydrogen down, the suction hydrogen pressure is 0.1～0.2MPa, adopt vacuum during dehydrogenation, temperature is 480 ℃～580 ℃ dehydrogenations and the dividing potential drop argon gas that charged into 0.01Mpa-0.05Mpa in 30 minutes, final dehydrogenation is to below the vacuum degree 0.5pa, and the hydrogen content that makes the hydrogenation powder is smaller or equal to 600ppm.
The preparation method who contains trace nitrogen Re-Fe-B series permanent magnetic material, in the described step (4) by recyclegas being less than equal 10 ℃ of nitrogen protections or argon shield makes the hydrogenation powder further levigate with equipment.
The preparation method who contains trace nitrogen Re-Fe-B series permanent magnetic material, the middle protective gas of described step (5) is done the recyclegas protection with argon gas or maintenance less than 10 ℃ nitrogen and is utilized air-flow that powder particle is worn into fine powder.
The preparation method who contains trace nitrogen Re-Fe-B series permanent magnetic material, sintering process charges into the argon gas of 100-500pa 250～600 ℃ of blank contraction phases in the described step (7), and continues to heat up during vacuum degree p in the sintering furnace＜5pa in the time of 600 ℃ again.
The preparation method who contains trace nitrogen Re-Fe-B series permanent magnetic material heat-treated when 2～4 hours and 440～600 ℃ when the two levels of thermal described in the described step (8) is treated to 900～920 ℃ in 2～4 hours.
The preparation method who contains trace nitrogen Re-Fe-B series permanent magnetic material, employing equipment made hydrogenation powder cool to room temperature after described step (3) dehydrogenation was intact.
The preparation method who contains trace nitrogen Re-Fe-B series permanent magnetic material, described step (5) are with pure oxygen or regulate the airflow milling oxygen content through the compressed air of super-dry and make the surface passivation of fine powder fractional inspired oxygen.
The preparation method who contains trace nitrogen Re-Fe-B series permanent magnetic material, the blank contraction phase described in the described step (7), every interval charged into argon gas in 5～30 minutes.
The present invention adopts the nitrogen content of technology such as fragmentation and air-flow grinding process and special sintering dehydrogenation reduction magnets in special suction hydrogen dehydrogenating technology and low temperature nitrogen or the argon gas, after nitrogen content≤300ppm, the illeffects of nitrogen has been reduced to very little, and the antiseptic property of magnet improves greatly, and the present invention is by realizing to sintering whole process relevant device special control requires according to low nitrogen technology transformation and device parameter adjustment melting.
The sintering Re-Fe-B series magnet that contains trace nitrogen of the present invention has the following advantages:
1, do not need to consume the part rare earth because of nitrogen content exists, reduced total amount of rare earth, particularly (Dy, consumption Tb) can further reduce and arrive identical performance for Ang Gui heavy rare earth dysprosium and terbium.
2, magnet performance is reached:
Hcj+ (BH) max 〉=63 or Hcj+ (BH) max 〉=64 (when hcj greater than 20 the time) or Hcj+ (BH) max 〉=65 (when hcj greater than 25 the time) more than high-quality sintering Re-Fe-B based permanent magnet, can reach identical magnetic circuit effect and reduce the magnet consumption.
3, corrosion resistance improves significantly, the magnet that the present invention program makes 504 hours magnet weightlessness under 0.2Mpa, 100%RH humidity weightless test condition is controlled in the 1.8mg/cm2, lays the first stone with the magnet that the surface does not apply for making wind-driven generator and electric motor of automobile and extraordinary heavy-duty motor.
Contrast to the magnet parameters that contains trace nitrogen of the magnet of common process preparation and the inventive method preparation is as shown in the table:
The increase of hence one can see that magnet nitrogen content causes density, coercive force (jhc), remanent magnetism (Br), magnetic energy product and coercive force sum (jhc+ (BH) max) and maximum magnetic energy product (BH) max all to descend, jhc+ (BH) max is issued to 66.0MGsOe in the condition of the average 201ppm of nitrogen content, and is 62.1MGsOe during the average 702ppm of nitrogen content; Magnet weightlessness differed 7.16mg/cm2 in the time of 144 hours, and magnet weightlessness is respectively 37.28mg/cm2 and 1.53mg/cm2 in 504 hours common solution and the present invention program, reacted the low long-time corrosion-resistant ability of magnet of the present invention program's nitrogen content, every index rapid deterioration when surpassing 876ppm.
Embodiment
Embodiment 1
(1) raw material adopt various simple metal Nd, Pr, and Dy, Al, Ga.Co, Fe and alloy B-Fe, Nb-Fe etc. prepare burden by the component design requirement;
(2) make various raw material form the alloy liquid of fusion by vacuum melting method, the alloy liquid casting cooling with fusion has on the chilling copper roller in the 1m/s linear velocity then, makes molten steel form the thick rapid hardening strip of 0.3mm;
(3) hydrogen is pulverized: the rapid hardening strip is put into rotary hydrogenation stove, being warming up to 100 ℃ of insulations, to charge into dividing potential drop in 30 minutes be that 0.03 ar gas environment is inhaled hydrogen down, the suction hydrogen pressure is 0.1MPa, adopt 480 ℃ of dehydrogenations of vacuum high-temperature during dehydrogenation and in 30 minutes, charge into the dividing potential drop argon gas of 0.01Mpa, final dehydrogenation is to below the vacuum degree 0.5pa, adopt the air-cooled or water-cooled of reactor to make hydrogenation powder cool to room temperature after dehydrogenation is intact, the hydrogen content that makes the hydrogenation powder makes the hydrogenation powder stay a small amount of hydrogen and has reducing atmosphere when sintering to be unlikely to the too high Re-Fe-B of making of hydrogen content again be that powder is inhaled nitrogen during the course in 600ppm;
(4) broken in, make hydrogenation powder further levigate to 20 orders with interior nitrogen protection or argon shield with equipment such as paddle-type mill or taper thread grindings by making recyclegas reach 10 ℃;
(5) the airflow milling micro mist is broken: with pure oxygen or regulate the airflow milling oxygen content through the compressed air of super-dry and make the surface passivation of micro mist fractional inspired oxygen; the oxygen uptake that reduces subsequent process makes the rising of micro mist temperature cause inhaling nitrogen, and the protective gas of airflow milling keeps the nitrogen below 10 ℃ to make the fine powder that 4um is worn in the recyclegas protection with argon gas or system forever.
(6) die mould, mold pressing add isostatic cool pressing or rubber mold pressing and prop up powder compaction is become pressed compact, and the process of die mould is finished under hermetic environment.
(7) sintering with pressed compact 1040-1080 ℃ of sintering temperature in vacuum sintering furnace, filled into the argon gas of 100pa per 5 minutes of 250 ℃ of blank contraction phases, and made product continue to heat up during vacuum degree p in the sintering furnace＜5pa in the time of 600 ℃ again.
(8) timeliness with the pressed compact behind the sintering in vacuum sintering furnace two-stage (900-920) ℃ * (2-4) hour and (440-600) heat-treated in ℃ * (2-4) hour, is improved the distribution of rich rare earth phase in the tissue, improves the Hcj of permanent magnet.
Embodiment 2
The hydrogen of step (3) is pulverized: the rapid hardening strip is put into rotary hydrogenation stove, being warming up to 200 ℃ of insulations, to charge into dividing potential drop in 60 minutes be that 0.05 ar gas environment is inhaled hydrogen down, the suction hydrogen pressure is 0.2MPa, adopt 580 ℃ of dehydrogenations of vacuum high-temperature during dehydrogenation and in 30 minutes, charge into the dividing potential drop argon gas of 0.05Mpa, final dehydrogenation is to below the vacuum degree 0.5pa, adopt the air-cooled or water-cooled of reactor to make hydrogenation powder cool to room temperature after dehydrogenation is intact, the hydrogen content that makes the hydrogenation powder is at 500ppm, makes the hydrogenation powder stay a small amount of hydrogen and has reducing atmosphere when sintering to be unlikely to the too high Re-Fe-B of making of hydrogen content again be that powder is inhaled nitrogen during the course;
Step (7) sintering with pressed compact 1040-1080 ℃ of sintering temperature in vacuum sintering furnace, filled into the argon gas of 500pa per 30 minutes of 600 ℃ of blank contraction phases, and made product continue to heat up during vacuum degree p in the sintering furnace＜5pa in the time of 650 ℃ again.
All the other steps are with embodiment 1.
Embodiment 3
The hydrogen of step (3) is pulverized: the rapid hardening strip is put into rotary hydrogenation stove, being warming up to 150 ℃ of insulations, to charge into dividing potential drop in 45 minutes be that 0.04 ar gas environment is inhaled hydrogen down, the suction hydrogen pressure is 0.15MPa, adopt 500 ℃ of dehydrogenations of vacuum high-temperature during dehydrogenation and in 18 minutes, charge into the dividing potential drop argon gas of 0.04Mpa, final dehydrogenation is to below the vacuum degree 0.3pa, adopt the air-cooled or water-cooled of reactor to make hydrogenation powder cool to room temperature after dehydrogenation is intact, the hydrogen content that makes the hydrogenation powder is at 550ppm, makes the hydrogenation powder stay a small amount of hydrogen and has reducing atmosphere when sintering to be unlikely to the too high Re-Fe-B of making of hydrogen content again be that powder is inhaled nitrogen during the course;
Step (7) sintering with pressed compact 1040-1080 ℃ of sintering temperature in vacuum sintering furnace, filled into the argon gas of 350pa per 18 minutes of 630 ℃ of blank contraction phases, and made product continue to heat up during vacuum degree p in the sintering furnace＜5pa in the time of 620 ℃ again.
All the other steps are with embodiment 1.
Claims (7)
1, the preparation method who contains trace nitrogen Re-Fe-B series permanent magnetic material comprises that step (1) prepares burden raw material by the component design requirement; (2) rapid hardening strip; (3) the rapid hardening strip is put into rotary hydrogenation stove, inhale hydrogen dehydrogenation again, adopt the air-cooled or water-cooled of reactor to make hydrogenation powder cool to room temperature after dehydrogenation is intact; (4) make the hydrogenation powder further levigate to 20 orders with equipment such as paddle-type mill or taper thread grindings; (5) utilize air-flow that powder particle is accelerated to the fine powder that velocity of sound makes it to wear into 2.8-4um; (6) powder compaction is become pressed compact; (7) with pressed compact sintering in vacuum sintering furnace; (8) two-stage in vacuum sintering furnace of the pressed compact behind the sintering is heat-treated, it is characterized in that in the described step (3) the rapid hardening strip being put into rotary hydrogenation stove, being warming up to 100～200 ℃ of insulations, to charge into dividing potential drop in 30～60 minutes be that 0.03～0.05 ar gas environment is inhaled hydrogen down, the suction hydrogen pressure is 0.1～0.2MPa, adopt vacuum during dehydrogenation, temperature is 480 ℃～580 ℃ dehydrogenations and the dividing potential drop argon gas that charged into 0.01Mpa-0.05Mpa in 30 minutes, and final dehydrogenation is to below the vacuum degree 0.5pa.
2, the preparation method who contains trace nitrogen Re-Fe-B series permanent magnetic material according to claim 1 is characterized in that in the described step (4) by recyclegas being less than equal 10 ℃ of nitrogen protections or argon shield makes the hydrogenation powder further levigate with equipment.
3, the preparation method who contains trace nitrogen Re-Fe-B series permanent magnetic material according to claim 1 is characterized in that in the described step (5) that protective gas is with argon gas or keep doing the recyclegas protection less than 10 ℃ nitrogen and utilize air-flow that powder particle is worn into fine powder.
4, the preparation method who contains trace nitrogen Re-Fe-B series permanent magnetic material according to claim 1, it is characterized in that sintering process in the described step (7) charges into the argon gas of 100-500pa 250～600 ℃ of blank contraction phases, and in the time of 600 ℃～650 ℃, continue again to heat up during vacuum degree p in the sintering furnace＜5pa.
5, the preparation method who contains trace nitrogen Re-Fe-B series permanent magnetic material according to claim 1 is characterized in that described step (3) dehydrogenation adopts cooling device to make hydrogenation powder cool to room temperature after intact.
6,, it is characterized in that described step (5) is with pure oxygen or regulate the airflow milling oxygen content through the compressed air of super-dry and make the surface passivation of fine powder fractional inspired oxygen according to claim 1 or the 3 described preparation methods that contain trace nitrogen Re-Fe-B series permanent magnetic material.
7, the preparation method who contains trace nitrogen Re-Fe-B series permanent magnetic material according to claim 4 is characterized in that every interval of blank contraction phase described in the described step (7) charged into argon gas in 5～30 minutes.
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| US5162064A (en) * | 1990-04-10 | 1992-11-10 | Crucible Materials Corporation | Permanent magnet having improved corrosion resistance and method for producing the same |
| US5858123A (en) * | 1995-07-12 | 1999-01-12 | Hitachi Metals, Ltd. | Rare earth permanent magnet and method for producing the same |
| JP3294841B2 (en) * | 2000-09-19 | 2002-06-24 | 住友特殊金属株式会社 | Rare earth magnet and manufacturing method thereof |
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