CN102737801A - Method for preparing Sm-Fe-N anisotropic magnetic powder - Google Patents
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Abstract
The invention discloses a method for preparing Sm-Fe-N anisotropic magnetic powder, which belongs to the field of magnetic materials. The technological process is as follows: preparing an alloy melt; controlling parameters of a rapid solidification process and the thicknesses of casting pieces; obtaining fast-setting casting pieces with nearly-consistent oriented small Sm2Fe17 cylindrical crystals; carrying out crystallization processing on the fast-setting casting pieces; carrying out coarse crushing; nitriding the fast-setting casting pieces; carrying out fine grinding; and obtaining the anisotropic Sm-Fe-N magnetic powder. The method is mainly characterized in that: through controlling the rotating speed of a cooling copper roller, the gas pressure of melt injection, the size of a nozzle, the temperature of the melt and the compositions of the melt, the cooling rate and crystallization process of the melt are controlled, so that fast-setting casting pieces with consistent oriented small Sm2Fe17 cylindrical crystals are obtained, thereby laying a foundation for the preparation of anisotropic magnetic powder and bonded permanent magnets with consistent oriented magneto-crystallines. By using the method for preparing Sm-Fe-N anisotropic magnetic powder, a normally required operation of carrying out long-time high-temperature homogenizing annealing on Sm-Fe alloy ingots is avoided.
Description
Technical field
The invention belongs to field of magnetic material, relate to a kind of preparation method of Sm-Fe-N anisotropic magnet powder.
Background technology
Sm2Fe
17N
xHave excellent intrinsic magnetic properties ability, be described as the later permanent magnetic material of new generation of the Nd-Fe-B that continues.With Nd
2Fe
14B compares, and it has higher Curie temperature (exceeding nearly 160 ° of C), extra high magnetocrystalline anisotropy, H
A=11.2MA/m (140KOe) is only second to SmCo
5, be Nd
2Fe
142 times of B, theoretical magnetic energy product is 472KJ/m
3(59.2MGOe), with Nd
2Fe
14B (509KJ/m
3) about the same.Because Sm
2Fe
17N
xAt high temperature can decompose, thus can not sintering, can only make bonded magnet.With regard to intrinsic magnetic characteristic, Sm
2Fe
17N
xSaturated pole intensity a little less than Nd
2Fe
14B, but its Curie temperature and magnetocrystalline anisotropy field are all far above the latter.See Sm in addition from the angle of practicability
2Fe
17N
xThermal stability, non-oxidizability and corrosion resistance all be superior to Nd
2Fe
14B.The outstanding advantage of it another is to process anisotropy bonded magnetic powder and bonded magnet.
Prepare Sm at present
2Fe
17N
xMethod mainly contain: mechanical alloying method (MA), hydrogen crush method (HDDR), reduction-diffusion process (R/D), quick quenching technique (RQ), powder metallurgic method (PM).The preparation Sm of the whole bag of tricks
2Fe
17Powder and Sm thereof
2Fe
17N
xTechnological process, the characteristics of magnetic are following:
Mechanical alloying method (MA): pure constituent element powder → high-energy ball milling → formation laminate granular → diffusion annealing forms nanocrystal → nitrogenize → Sm
2Fe
17N
xMagnetic.Mechanical alloying method prepares Sm
2Fe
17Need long high-energy ball milling, powder activity is high, particle is thin, the increase that in nitrogenize and preparation bonded magnet process, brings oxygen content easily; Because powder particle is too little, is difficult to prepare highdensity bonded permanent magnet; Though powder particle is very little, be not necessarily the monocrystalline single domain particle, mainly be suitable for preparing the isotropism magnetic.
Reduction-diffusion process (R/D): the Sm of certain proportioning
2O
3, raw material → batch mixing → briquetting → reduction diffusion reaction → product separation → nitrogenize → fine grinding → Sm such as Ca, Fe
2Fe
17N
xMagnetic.This method mainly is suitable for preparing the isotropism magnetic, and the difficult point of this method mainly is the anti-oxidation problem powder metallurgic method (PM) of Sm-Fe alloy powder in separation and the separation process of product: the alloy raw material → melting → homogenizing processing → coarse crushing → ball milling powder process → nitrogenize → fine grinding → Sm of certain proportioning
2Fe
17N
xMagnetic.
Powder metallurgic method (PM): the alloy raw material → melting → homogenizing processing → coarse crushing → ball milling powder process → nitrogenize → fine grinding → Sm of certain proportioning
2Fe
17N
xMagnetic.Powder metallurgic method can produce high-performance anisotropic Sm
2Fe
17N
xMagnetic is because the remanent magnetism of anisotropic magnet powder, magnetic energy product far above the isotropism magnetic, have the better application prospect.This method shortcoming need be carried out long high temperature homogenizing annealing to the alloy of melting, because the cooling rate of induction melting water cooled copper mould casting process is slower, solidified superalloy is organized thick, and the ingot structure component distributing is inhomogeneous; Because L+Fe → Sm
2Fe
17The characteristics of peritectic reaction, reaction not exclusively exist more α-Fe and rich Sm mutually in the alloy.For obtaining more Sm
2Fe
17Phase constitution changes the incomplete alloy structure of peritectic reaction into Sm
2Fe
17Phase must be handled through the long-time homogenizing of high temperature (about 1020 ° of C), generally reaches about 20 hours and just can reach effect preferably.In addition, alloy is not necessarily along intercrystalline cracking in pulverizing process, and the part Sm-Fe-N powder particle of acquisition possibly be made up of polycrystalline, because grain orientation is different, this part powder particle does not possess anisotropy yet.
Hydrogen crush method (HDDR): the hydrogen treat → nitrogenize → Sm of foundry alloy melting → homogenizing annealing → coarse crushing → HDDR process
2Fe
17N
xMagnetic.The HDDR method be with the foundry alloy of handling through homogenizing through hydrogenation, disproportionation decompose, dehydrogenation chemical combination process again, with refinement Sm
2Fe
17Crystal grain, via nitride make the isotropism magnetic of high-coercive force.
Quick quenching technique (RQ): foundry alloy melting → fast quenching becomes strip (amorphous state) → crystallization to handle (nanocrystal) → fragmentation, ball milling powdered.Be utilized in and add a spot of Co, Zr, B in the Sm-Fe alloy respectively to improve Sm
2Fe
17N
xCurie temperature, refinement Sm
2Fe
17Crystal grain and fast quenching thin strap are decrystallized, improve Sm through tiny α in the fast quenching thin strap-Fe phase exchange-coupling interaction
2Fe
17N
xThe remanent magnetism of magnetic has obtained the isotropism magnetic that remanent magnetism, magnetic energy product all are superior to other methods such as HDDR method so far.
Powder metallurgic method can be made the high-performance anisotropic magnetic, but because ingot casting needs long homogenizing annealing to handle, has hindered powder metallurgic method applying on suitability for industrialized production, and restricting this method development key is Sm
2Fe
17The alloy fabrication portion.Compare with other method, quick quenching technique has been showed good development prospect, and at present report is used quick quenching technique and made isotropism Sm-Fe-N magnetic, if can make anisotropic magnet powder, and will be for further improving remanent magnetism from now on and magnetic energy product creates favorable conditions.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing fast melt-quenching to prepare the Sm-Fe-N anisotropic magnet powder; Through copper roller rotating speed, melt jet gas pressure, jet size, melt temperature, bath composition in the control rapid solidification; With the cooling rate of control melt and the thickness of rapid hardening casting sheet, reach acquisition rapid hardening strip Sm
2Fe
17Principal phase is the target that tiny column crystal is arranged; Column crystal is consistent basically to be orientated, perpendicular to rapid hardening casting sheet surface; Through further crystallization processing, fragmentation, nitrogenize, fine grinding, obtain consistent anisotropy Sm-Fe-N magnetic and the anisotropic bonded magnet that is orientated of magnetocrystalline direction of easy axis in the powder particle again.
The technological process that the present invention prepares the Sm-Fe-N magnetic is: raw material select and proportioning → vacuum induction melting (alloy melt preparation) → fast quenching (control of rapid solidification parameter control, casting sheet thickness) → alloy structure analysis → tiny Sm
2Fe
17Column crystal near consistent be orientated rapid hardening cast sheet → coarse crushing → heat treatment (Sm
2Fe
17Further crystallization) → fragmentation → nitrogenize → fine grinding → anisotropy Sm-Fe-N magnetic → detection powder magnetic property.The Sm-Fe-N magnetic that makes has tangible anisotropic character, compares with the isotropism sample, and remanent magnetism improves more than 20% after orientation.
Technical process of the present invention:
(1) with Sm, Fe batching, can add a spot of Co, V, Zr, B, press Sm
2(Fe
1-xM
x)
17Molecular formula batching, M is one or more among Co, V, Zr, the B, every kind of atomic percent that replaces Fe is not more than 5%, because Sm volatilizees easily, it is certain excessive to have, and generally adds amount of calculation 18% ~ 35%.Application of high temperatures induction melting alloy; Melted alloy flows to and is rapidly solidificated into strip on the copper roller rotating; Rotating speed through control copper roller (4 ~ 15m/s), jet size (wide by 0.2 ~ 0.65mm), melt jet gas pressure gas pressure (0.5 ~ 1.5atm), melt temperature (1520-1570 ° of C), obtain Sm
2Fe
17The strip tissue that is the nearly parallel distribution of tiny column crystal mutually, strip thickness 0.1 ~ 0.4mm.
(2) the applying electronic microscope carries out observation analysis to the strip cross section and determines whether to have formed columanar structure; The applying X-ray diffraction analysis confirms whether the main phase constitution of rapid hardening strip is Sm
2Fe
17Phase.
(3) qualified rapid hardening casting sheet carry out coarse crushing to 1 ~ 5mm, further crystallization and thermal treatment under 700 ~ 800 ° of C high-purity argon gas protective atmospheres promotes atom diffusion, so that Sm
2Fe
17Phase degree of crystallinity is more complete.
(4) fragmentation: use under benzinum media protection or the high-purity argon gas protective medium, the Sm-Fe alloy powder be crushed to below 320 orders so that in the nitridation process N atom to diffusion inside.
(5) nitrogen treatment: the Sm-Fe alloyed powder is at high purity nitrogen or NH
3And H
2Mixed atmosphere in carry out nitriding, nitriding gas pressure is at 0.1 ~ 1.0MPa, 400 ~ 500 ° of C of nitriding temperature, nitridation time 3 ~ 5 hours.
(6) fine grinding: with the benzinum is ball-milling medium, and ratio of grinding media to material is 4:1 ~ 30:1, ball milling 3 ~ 20 hours.
(7) drying and sample preparation.After ball milling was good, the vacuumize of discharging normal temperature obtained anisotropy Sm-Fe-N magnetic.To dust sampling; As binding agent, orientation cured and prepared measuring samples size
is used vibrating specimen magnetometer (VSM) and is measured the powder magnetic property under 2T magnetic field with AB glue.
The invention has the advantages that: the Sm-Fe alloy rapid hardening casting sheet even tissue of acquisition does not need long high temperature homogenizing annealing to handle; Because tiny Sm
2Fe
17Column crystal as raw material, can prepare anisotropy Sm-Fe-N magnetic perpendicular to nearly consistent orientation the in rapid hardening casting sheet surface.
Description of drawings
Fig. 1. perpendicular to columanar structure's structure (not corroding) of copper roller, the main Sm of light gray form and aspect among the figure
2Fe
17Column crystal, the white that intergranular distributes is rich Sm phase mutually
Fig. 2. the XRD analysis of rapid hardening casting sheet, visible by the X-diffraction, mainly formed Sm
2Fe
17Phase also has rich Sm phase---SmFe in addition
3
Embodiment
Embodiment 1
Using purity is that 99.9% pure iron, rare-earth Sm are raw material, and the Fe rod is cleaned out, and presses Sm
2Fe
17Batching because Sm volatilizees easily, adds 22% on the basis of amount of calculation., the Sm for preparing, Fe raw material are put into the magnesia crucible of vacuum induction melting furnace, close stove evacuation, when vacuum degree reaches 0.01Pa; Begin heating, be heated to about 700 ° of C, charge into 0.05MPa high-purity argon gas (purity is 99.999%); Along with the rising of temperature, Sm melts earlier fully, continue heating after 3 minutes Fe melt fully; At the about 1540 ° of C of temperature, the insulation refining poured in the water cooled copper mould after 3 minutes, and cooling was taken out ingot casting more than 30 minutes in stove.Then in the quartz ampoule of rapid hardening casting sheet preparation facilities under the vacuum condition induction heating melt again; Be poured under the effect of 0.8 atmospheric pressure expulsion pressure on the copper roller of roll surface speed at the 5m/s high speed rotating; Form about 0.24mm thickness band; The strip interface taken a sample to observe down in electron microscope has formed column crystal, has mainly formed Sm with the XRD analysis proof
2Fe
17Phase.The strip of this rapid hardening is broken into the sheet of 1 ~ 5mm, and the magazine of packing into is put into quartz ampoule, earlier with being evacuated to 4 * 10
-3Pa charges into high-purity argon gas (purity is 99.9995%), and quartz ampoule is put into stove, after 1 hour, takes out boiler tube 730 ° of C insulations, takes out alloy sheet behind the cool to room temperature.Under the high-purity argon gas protective medium, cross 500 mesh sieves with the fragmentation of steel alloy mortar; With the magazine of packing into of the powder after sieving, put into quartz ampoule, pumping high vacuum to 4 * 10
-3Pa closes extraction valve, charges into high pure nitrogen, and nitrogen pressure reaches 0.5MPa, puts into the stove nitriding, and nitriding temperature is 480 ° of C, is incubated after 5 hours, takes out boiler tube, takes out powder behind the cool to room temperature; With the ratio of grinding media to material is that 30:1, benzinum are ball-milling medium, and charging ball milling, ball milling be the discharging deposition after 9 hours, unnecessary benzinum is reclaimed, with the vacuumize of slip normal temperature; As binding agent, measure through VSM and to obtain the powder magnetic property by orientation cured and prepared vibrating specimen magnetometer (VSM) measuring samples under 2T magnetic field with AB glue for powder with drying after good.Orientation characteristic is: H
Ci2113Oe, Br0.89T; Magnetic field orientating (same sex sample) performance is not: H
Ci2230Oe, Br0.7T.
Embodiment 2
Using purity is that 99.9% pure iron, rare-earth Sm, Co, V are raw material, and the Fe rod is cleaned out, and presses Sm
2(Fe
0.94Co
0.02V
0.04)
17Batching because Sm volatilizees easily, adds 25% on the basis of amount of calculation.Preparation process and embodiment 1 are similar, with vacuum induction melting, water cooled copper mould cooling, obtain alloy cast ingot earlier.Then in the quartz ampoule of rapid hardening casting sheet preparation facilities under the vacuum condition induction heating melt again; Be poured under the effect of 0.8 atmospheric pressure expulsion pressure on the copper roller of roll surface speed at the 7m/s high speed rotating; Form about 0.16mm thickness band; The strip interface taken a sample to observe down in electron microscope has formed column crystal, has mainly formed Sm with the XRD analysis proof
2Fe
17Phase.The strip of this rapid hardening is broken into the sheet of 1 ~ 5mm, and the following 780 ° of C insulation of high-purity argon gas atmosphere is 0.5 hour then, with further crystallization treatment S m
2Fe
17Phase.Alloy sheet is carried out nitrogen treatment being broken into the steel alloy mortar under the high-purity argon gas protective medium below 500 orders; Nitrogen treatment uses high pure nitrogen pressure 0.2MPa, and nitriding temperature is 490 ° of C, is incubated 5 hours; Ball milling, drying, sample preparation obtain the powder magnetic property with embodiment 1, and orientation characteristic is: H
Ci4980Oe, Br0.83T; The magnetic field orientating performance is not: H
Ci5260Oe, Br0.66T.
Embodiment 3
Using purity is that 99.9% pure iron, rare-earth Sm, V are raw material, and the Fe rod is cleaned out, and presses Sm
2(Fe
0.95V
0.05)
17Batching because Sm volatilizees easily, adds 23% on the basis of amount of calculation.Preparation process and embodiment 1 are similar, with vacuum induction melting, water cooled copper mould cooling, obtain alloy cast ingot earlier.Then in the quartz ampoule of rapid hardening casting sheet preparation facilities under the vacuum condition induction heating melt again; Be poured under the effect of 0.8 atmospheric pressure expulsion pressure on the copper roller of roll surface speed at the 6m/s high speed rotating; Form about 0.19mm thickness band; The strip interface taken a sample to observe down in electron microscope has formed column crystal, has mainly formed Sm with the XRD analysis proof
2Fe
17Phase.The strip of this rapid hardening is broken into the sheet of 1 ~ 5mm, and the following 780 ° of C insulation of high-purity argon gas atmosphere is 0.5 hour then, with further crystallization treatment S m
2Fe
17Phase.Alloy sheet is carried out nitrogen treatment being broken into the steel alloy mortar under the high-purity argon gas protective medium below 320 orders; Use NH
3And H
2The mist of (volume ratio 3:7) carries out nitriding, and gas pressure is 0.12MPa, and nitriding temperature is 450 ° of C, is incubated 3.5 hours; Ball milling, drying, sample preparation obtain the powder magnetic property with embodiment 1, and orientation characteristic is: H
Ci3920Oe, Br0.85T; The magnetic field orientating performance is not: H
Ci4130Oe, Br0.68T.
Embodiment 4
Using purity is that 99.9% pure iron, rare-earth Sm, Co, V are raw material, and the Fe rod is cleaned out, and presses Sm
2(Fe
0.94Co
0.02V
0.03)
17Batching because Sm volatilizees easily, adds 25% on the basis of amount of calculation.Save vacuum induction melting; Directly in rapid hardening casting sheet preparation facilities induction heating melting alloy and spray to the copper roller of roll surface speed at the 15m/s high speed rotating; Pouring nozzle width 0.65mm, spray high-purity argon gas pressure 1atm forms about 0.3mm thickness band; Detect the microscopic structure and the phase composition of rapid hardening casting sheet, to obtain tiny Sm
2Fe
17The microscopic structure that column crystal is arranged.The strip of this rapid hardening is broken into the sheet of 1 ~ 5mm, and the following 750 ° of C insulation of high-purity argon gas atmosphere is 1 hour then, with further crystallization treatment S m
2Fe
17Phase.With alloy sheet is that medium, ratio of grinding media to material are 8:1 with the benzinum, charging ball milling 1 hour, and discharging then, deposition with the slime vacuum air drying, obtain alloy powder; At NH
3And H
2Carry out nitrogen treatment in the mist of (volume ratio 3:7), gas pressure is 0.12MPa, and nitriding temperature is 450 ° of C, is incubated 3.5 hours; The powder ball-milling technology is that ratio of grinding media to material is 8:1, ball milling time 12 hours after the nitrogenize, and discharging then, deposition with the slime vacuum air drying, are measured the powder magnetic property with embodiment 1 sample preparation, and the result is: orientation characteristic is: H
Ci4580Oe, Br0.84T; The magnetic field orientating performance is not: H
Ci4720Oe, Br0.67T.
Claims (4)
1. the preparation method of a Sm-Fe-N anisotropic magnet powder, it is characterized in that: technological process is: the control → tiny Sm of alloy melt preparation → rapid solidification parameter control, casting sheet thickness
2Fe
17Column crystal near consistent be orientated rapid hardening cast sheet → crystallization processing → coarse crushing → nitrogenize → fine grinding → anisotropy Sm-Fe-N magnetic, specifically preparation process is following:
(1) with Sm, Fe batching; Application of high temperatures induction melting alloy; Melted alloy flows to and is rapidly solidificated into strip on the copper roller rotating; The wide 0.2 ~ 0.65mm of rotating speed 4 ~ 15m/s, jet size, melt jet gas pressure gas pressure 0.5 ~ 1.5atm, melt temperature 1520-1570 ° C through control copper roller obtain Sm
2Fe
17The strip tissue that is the nearly parallel distribution of tiny column crystal mutually, strip thickness 0.1 ~ 0.4mm;
(2) the applying electronic microscope carries out observation analysis to the strip cross section and determines whether to have formed columanar structure; The applying X-ray diffraction analysis confirms whether the main phase constitution of rapid hardening strip is Sm
2Fe
17Phase;
(3) qualified rapid hardening casting sheet carry out coarse crushing to 1 ~ 5mm, further crystallization and thermal treatment under 700 ~ 800 ° of C high-purity argon gas protective atmospheres promotes atom diffusion, so that Sm
2Fe
17Phase degree of crystallinity is more complete;
(4) fragmentation: use under benzinum media protection or the high-purity argon gas protective medium, the Sm-Fe alloy powder be crushed to below 320 orders so that in the nitridation process N atom to diffusion inside;
(5) nitrogen treatment: the Sm-Fe alloyed powder is at high purity nitrogen or NH
3And H
2Mixed atmosphere in carry out nitriding, nitriding gas pressure is at 0.1 ~ 1.0Mpa, 400 ~ 500 ° of C of nitriding temperature, nitridation time 3 ~ 5 hours;
(6) fine grinding: with the benzinum is ball-milling medium, and ratio of grinding media to material is 4:1 ~ 30:1, ball milling 3 ~ 20 hours;
(7) drying and sample preparation: after ball milling was good, the vacuumize of discharging normal temperature obtained anisotropy Sm-Fe-N magnetic.
2. the preparation method of a kind of Sm-Fe-N anisotropic magnet powder according to claim 1 is characterized in that: Sm is total excessive in 18% ~ 35% during batching.
3. the preparation method of a kind of Sm-Fe-N anisotropic magnet powder according to claim 1 is characterized in that: cooling copper roll surface speed is at 4 ~ 15m/s when preparation rapid hardening strip.
4. the preparation method of a kind of Sm-Fe-N anisotropic magnet powder according to claim 1 is characterized in that: add a spot of Co, V, Zr, B, press Sm
2(Fe
1-xM
x)
17The molecular formula batching, M is one or more among Co, V, Zr, the B, every kind of atomic percent that replaces Fe is not more than 5%.
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