CN104399994B - Preparation method for Sm2Fe17Nx rare earth permanent magnet powder - Google Patents
Preparation method for Sm2Fe17Nx rare earth permanent magnet powder Download PDFInfo
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Abstract
The invention belongs to the technical field of rare earth permanent magnet materials and discloses a preparation method for Sm2Fe17Nx rare earth permanent magnet powder. According to the preparation method for the Sm2Fe17Nx rare earth permanent magnet powder, the Sm2Fe17Nx rare earth permanent magnet powder is prepared by mechanical alloying, iron powder or ferric oxide powder serves as raw materials, high-pure nitrogen, ammonia gas or decomposed ammonia serves as a nitrogen source, and the atmosphere pressure is from 0.01 to 0.1MPa; microwaves are served as heat sources, the frequency is 2.45GHz, the power is from 1 to 5KW, the resultant temperature is from 500 to 800 DEG C, the heat preservation time is from 2 to 5h, iron nitride powder is synthesized, and the nitrogen content is from 3 wt.% to 8 wt.%. The preparation method for the Sm2Fe17Nx rare earth permanent magnet powder comprises the following steps of mixing pure samarium powder and the prepared iron nitride powder according to a Sm and Fe molar ratio of 2 to 17, and putting the pure samarium powder, the prepared iron nitride powder and aluminum oxide or zirconia ceramic balls into a high-energy ball milling pot after primary mixing, wherein a ratio of grinding media to material is from 10 to 1 to 20 to 1, the ball milling time is from 5 to 10h, and the ball milling medium is high-pure nitrogen; preparing powder in a vacuum glove box. thus obtaining the Sm2Fe17Nx rare earth permanent magnet powder. The preparation method for the Sm2Fe17Nx rare earth permanent magnet powder is simple in technology, low in cost and easy for industrialization, and high-performance Sm2Fe17Nx rare earth permanent magnet powder with different nitrogen contents can be efficiently synthesized according to requirements.
Description
Technical field
The invention belongs to powder metallurgy process and prepare rare-earth permanent-magnet material technical field, in particular, provide a kind of profit
The preparation method of samarium ferrum nitrogen rare earth permanent-magnet powder is prepared with mechanical alloying.
Technical background
Nineteen ninety, Coey etc. utilizes gas-solid phase reaction to synthesize interstitial atom intermetallic compound R2Fe17Nx,
Cause the extensive concern of magnetics circle.Wherein Sm2Fe17NxCompound has the interior natural endowment magnetic property of excellence, it
Saturation magnetization reach 1.54T, this can compare favourably with the 1.6T of NdFeB, Curie temperature 470 DEG C, each
Anisotropy field 14T (NdFeB is 8T) all values than NdFeB are much higher, and its corrosion resistance, heat
Stability, non-oxidizability are better than NdFeB permanent magnet material.Therefore, Sm2Fe17NxIt it is gap nitride rare earth
Permanent magnet material has the very high potential becoming a new generation's rare earth permanent-magnetic material.Simultaneously as NdFeB in recent years
Rare earth permanent-magnetic material quickly grows, and neodium resource is on the verge of exhaustion, and price constantly rises；On the other hand, samarium resource phase
To surplus, the mine tailing rich in samarium is piled up in a large number, and have the most directly discharges, and causes serious environmental pollution.
Therefore, Sm is greatly developed2Fe17NxMagnet Industry, effectively utilizes the samarium resource of domestic surplus to become scientific and technological circle
The focus paid close attention to industrial circle, is also a highly important content in " 12 planning ".
At present, Sm2Fe17NxIt is that the preparation method of rare earth permanent-magnet powder mainly has fast melt-quenching (RS) method, machine
Tool alloying (MA) method, hydrogenation-disproportionation-dehydrogenation-recombination (HDDR) method, powder metallurgy (PM) method
Deng 4 kinds of main method.Also obtain it addition, vat blue RS (RD) method produces at Japan's magnetic material industry
Application.Above method is generally divided into two steps: first prepare single-phase Sm2Fe17Compound, then to Sm2Fe17
Compound carries out nitrogen treatment.But there is following problem in existing samarium ferrum nitrogen rare earth permanent-magnetic material preparation technology:
(1) it is difficult to obtain the Sm that composition is uniform, phase composition is single2Fe17Phase alloy；(2)Sm2Fe17Alloy nitride
Kinetics is very poor；(3)Sm2Fe17NxPyrolytic problem the most unresolved.Chinese invention patent " one
The method of samarium ferrum nitrogen permanent magnet material is prepared in kind mechanical alloying " (patent No. ZL 03150162.1) although improve
Nitridation process, prepares high nitrogen content SmFeN permanent magnet material, but still is to rely in nitrogenous media environment
The diffusion of nitrogen nitrogenizes, and efficiency of nitridation is relatively low, and nitriding result is poor.
Summary of the invention
It is an object of the invention to overcome prior art to prepare samarium ferrum nitrogen rare earth permanent-magnet powder complex process, nitridation effect
The low problem with weak effect of rate, it is provided that a kind of " nitrided iron-samarium ferrum nitrogen " two steps prepare samarium ferrum nitrogen rare earth permanent magnet powder
The preparation method at end, the method can effectively control nitrogen content and nitrogen distribution in samarium ferrum nitrogen rare earth permanent-magnet powder, real
Now prepare high-performance samarium ferrum nitrogen rare earth permanent-magnet powder.
The preparation method of a kind of samarium ferrum nitrogen rare earth permanent-magnet powder, initially with microwave nitriding process preparation nitridation iron powder
End, then by mixed for samarium powder, prepare Sm through high-energy ball milling2Fe17NxRare earth permanent-magnet powder.Concrete grammar bag
Include herein below:
1, iron nitride powder is prepared in microwave nitridation
(1) iron powder or brown iron oxide are laid in microwave oven boat, are evacuated to vacuum and reach 10Pa
Hereinafter, be passed through purity be more than 99.9% containing nitrogen medium atmosphere, atmosphere pressures is maintained at 0.01～0.1MPa；
(2) starting microwave heating, frequency is 2.45GHz, and power controls 1～5KW, synthesis temperature control
System is at 500～800 DEG C, and temperature retention time controls 2～5h；
(3) being cooled to room temperature come out of the stove, synthetic product is iron nitride powder, and nitrogen content is at 3wt.%～8wt.%.
2, high-energy ball milling prepares samarium ferrum nitrogen rare earth permanent-magnet powder
(1) iron nitride powder of pure samarium powder Yu above-mentioned preparation is pressed Sm Yu Fe mol ratio 2:17 dispensing, tentatively
Mixing；
(2) compound is inserted in high-energy ball milling tank, load aluminium oxide or zirconia ceramics ball, ratio of grinding media to material
10:1～20:1, Ball-milling Time 5～10h, ball-milling medium is high pure nitrogen；
(3) ball grinder outer wall has water collar, prevents in mechanical milling process temperature in tank too high；At vacuum glove box
Middle powder delivery.
(4) in mechanical milling process, Sm powder and Fe-N powder can realize alloying, form supersaturated solid solution, i.e.
Sm can be prepared2Fe17NxRare earth permanent-magnet powder.
Iron powder described in step 1 is any one or a few in atomized iron powder, reduced iron powder or carbonyl iron dust.
Containing nitrogen medium atmosphere described in step 1 is high pure nitrogen, ammonia or cracked ammonium, and wherein iron powder correspondence is wherein
Any one or a few, one or both in brown iron oxide correspondence ammonia or cracked ammonium.
Microwave oven described in step 1 is microwave rotary furnace or microwave pushes away boat stove.
Compared with prior art, the present invention is advantageous in that:
(1) " nitrided iron-samarium ferrum nitrogen " two-step method is used to prepare samarium ferrum nitrogen rare earth permanent-magnet powder, by Fe-N solid-state
Nitrogen source is applied in ma process, compared with the diffusion in Sm-Fe of the nitrogen in gaseous nitrogen source, greatly
Shorten nitridation process, improve Sm2Fe17NxRare earth permanent-magnet powder transformation efficiency.
(2) can efficiently prepare, due to microwave treatment, the iron nitride powder that nitrogen content is controlled, can according to actual needs,
High-performance Sm of Fast back-projection algorithm different nitrogen contents2Fe17NxRare earth permanent-magnet powder.
(3) present invention process is simple, with low cost, be prone to industrialization.
Detailed description of the invention
Embodiment 1
(1) iron powder (-200 mesh) that makes water fogging is laid in microwave rotary furnace, is evacuated to vacuum and reaches 10
Below Pa, is passed through the high pure nitrogen that purity is more than 99.9%, and atmosphere pressures is maintained at 0.1MPa.Start micro-
Wave heating, frequency is 2.45GHz, and power is 1KW, and synthesis temperature is 800 DEG C, is incubated 2h.It is cooled to
Room temperature is come out of the stove, and synthetic product is iron nitride powder, and nitrogen content is 3wt.%.
(2) iron nitride powder of pure samarium powder Yu above-mentioned preparation is pressed Sm Yu Fe mol ratio 2:17 dispensing, tentatively
Mixing, loads ball grinder, ratio of grinding media to material 10:1, Ball-milling Time 5h, ball-milling medium by compound with alumina balls
For high pure nitrogen.After ball milling completes, powder delivery in vacuum glove box, can be prepared by Sm2Fe17NxRare earth permanent magnet
Powder, magnetic property is Br=0.8T,iHc=1950KA/m, (BH)m=156kJ/m3。
Embodiment 2
(1) ultra-fine reduced iron powder (5 μm) is laid in microwave to push away in boat furnace-boat ware, is evacuated to vacuum
Reaching below 10Pa, be passed through the cracked ammonium gas that purity is more than 99.9%, atmosphere pressures is maintained at 0.05MPa.
Starting microwave heating, frequency is 2.45GHz, and power is 3KW, and synthesis temperature is 600 DEG C, is incubated 3h.
Being cooled to room temperature come out of the stove, synthetic product is iron nitride powder, and nitrogen content is 4.8wt.%.
(2) iron nitride powder of pure samarium powder Yu above-mentioned preparation is pressed Sm Yu Fe mol ratio 2:17 dispensing, tentatively
Mixing, loads ball grinder, ratio of grinding media to material 15:1, Ball-milling Time 8h, ball-milling medium by compound with alumina balls
For high pure nitrogen.After ball milling completes, powder delivery in vacuum glove box, can be prepared by Sm2Fe17NxRare earth permanent magnet
Powder, magnetic property is Br=0.9T,iHc=2278KA/m, (BH)m=182kJ/m3。
Embodiment 3
(1) carbonyl iron dust (3 μm) is laid in microwave rotary furnace, is evacuated to vacuum and reaches 10Pa
Hereinafter, being passed through high-purity ammonia that purity is more than 99.9%, atmosphere pressures is maintained at 0.01MPa.Start microwave
Heating, frequency is 2.45GHz, and power is 5KW, and synthesis temperature is 500 DEG C, is incubated 5h.It is cooled to room
Temperature is come out of the stove, and synthetic product is iron nitride powder, and nitrogen content is 6.2wt.%.
(2) iron nitride powder of pure samarium powder Yu above-mentioned preparation is pressed Sm Yu Fe mol ratio 2:17 dispensing, tentatively
Mixing, loads ball grinder, ratio of grinding media to material 20:1, Ball-milling Time 10h, ball-milling medium by compound with alumina balls
For high pure nitrogen.After ball milling completes, powder delivery in vacuum glove box, can be prepared by Sm2Fe17NxRare earth permanent magnet
Powder, magnetic property is Br=0.9T,iHc=2306KA/m, (BH)m=197kJ/m3。
Embodiment 4
(1) brown iron oxide (-325 mesh) is laid in microwave rotary furnace, is evacuated to vacuum and reaches 10Pa
Hereinafter, being passed through high-purity ammonia that purity is more than 99.9%, atmosphere pressures is maintained at 0.08MPa.Start microwave
Heating, frequency is 2.45GHz, and power is 2KW, and synthesis temperature is 700 DEG C, is incubated 4h.It is cooled to room
Temperature is come out of the stove, and synthetic product is iron nitride powder, and nitrogen content is 8wt.%.
(2) iron nitride powder of pure samarium powder Yu above-mentioned preparation is pressed Sm Yu Fe mol ratio 2:17 dispensing, tentatively
Mixing, loads ball grinder, ratio of grinding media to material 15:1, Ball-milling Time 6h, ball-milling medium by compound with alumina balls
For high pure nitrogen.After ball milling completes, powder delivery in vacuum glove box, can be prepared by Sm2Fe17NxRare earth permanent magnet
Powder, magnetic property is Br=1.1T,iHc=2380KA/m, (BH)m=248kJ/m3。
Embodiment 5
(1) brown iron oxide (20 μm) is laid in microwave to push away in boat furnace-boat ware, is evacuated to vacuum and reaches
Below 10Pa, is passed through the cracked ammonium gas that purity is more than 99.9%, and atmosphere pressures is maintained at 0.03MPa.
Starting microwave heating, frequency is 2.45GHz, and power is 4KW, and synthesis temperature is 600 DEG C, is incubated 3h.
Being cooled to room temperature come out of the stove, synthetic product is iron nitride powder, and nitrogen content is 7.3wt.%.
(2) iron nitride powder of pure samarium powder Yu above-mentioned preparation is pressed Sm Yu Fe mol ratio 2:17 dispensing, tentatively
Mixing, loads ball grinder, ratio of grinding media to material 10:1, Ball-milling Time 4h, ball-milling medium by compound with alumina balls
For high pure nitrogen.After ball milling completes, powder delivery in vacuum glove box, can be prepared by Sm2Fe17NxRare earth permanent magnet
Powder, magnetic property is Br=1.0T,iHc=2630KA/m, (BH)m=260kJ/m3。
Claims (1)
1. the preparation method of a samarium ferrum nitrogen rare earth permanent-magnet powder, it is characterised in that preparation process bag
Include:
Iron nitride powder is prepared in a, microwave nitridation
(1) iron powder or brown iron oxide are laid in microwave oven boat, are evacuated to vacuum and reach 10
Below Pa, be passed through purity be more than 99.9% containing nitrogen medium atmosphere, atmosphere pressures is maintained at
0.01～0.1MPa；
(2) starting microwave heating, frequency is 2.45GHz, and power controls 1～5KW, synthesis temperature
Degree controls at 500～800 DEG C, and temperature retention time controls 2～5h；
(3) being cooled to room temperature come out of the stove, synthetic product is iron nitride powder, nitrogen content at 3wt.%～
8wt.%；
B, high-energy ball milling prepare samarium ferrum nitrogen rare earth permanent-magnet powder
(1) iron nitride powder of pure samarium powder Yu above-mentioned preparation is pressed Sm Yu Fe mol ratio 2:17 dispensing,
Preliminary mixing；
(2) compound is inserted in high-energy ball milling tank, load aluminium oxide or zirconia ceramics ball, ball material
Ratio 10:1～20:1, Ball-milling Time 5～10h, ball-milling medium is high pure nitrogen；
(3) ball grinder outer wall is provided with water collar, prevents in mechanical milling process temperature in tank too high；In vacuum
Powder delivery in glove box；
(4) in mechanical milling process, Sm powder can realize alloying with nitridation iron powder, forms super saturated solid solution
Body, can be prepared by Sm2Fe17NxRare earth permanent-magnet powder；
Iron powder described in step a (1) is any one in atomized iron powder, reduced iron powder or carbonyl iron dust
Or it is several；
Containing nitrogen medium atmosphere described in step a (1) is high pure nitrogen, ammonia or cracked ammonium, wherein iron powder
Corresponding any of which or several, the one or two in brown iron oxide correspondence ammonia or cracked ammonium
Kind；
Microwave oven described in step a (1) is microwave rotary furnace or microwave pushes away boat stove.
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| CN1125351A (en) * | 1994-08-29 | 1996-06-26 | 陶圣臣 | Method for making samarium-ferronitrogen permanent magnet |
| CN1202537C (en) * | 2003-07-21 | 2005-05-18 | 北京科技大学 | Method of preparing samarium iron nitrogen permanent amgnet material using mechanical alloying |
| CN100441341C (en) * | 2006-10-10 | 2008-12-10 | 河北工业大学 | Samarium-iron-nitrogen and iron-platinum double phase nano magnetic material and its preparing method |
| JP2008283141A (en) * | 2007-05-14 | 2008-11-20 | Seiko Instruments Inc | Method of manufacturing rare earth magnet powder, and method of manufacturing rare earth bond magnet |
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