CN102568729B - Method for preparing bulk composite nanocrystalline rare earth permanent magnetic material - Google Patents
Method for preparing bulk composite nanocrystalline rare earth permanent magnetic material Download PDFInfo
- Publication number
- CN102568729B CN102568729B CN201210005073.0A CN201210005073A CN102568729B CN 102568729 B CN102568729 B CN 102568729B CN 201210005073 A CN201210005073 A CN 201210005073A CN 102568729 B CN102568729 B CN 102568729B
- Authority
- CN
- China
- Prior art keywords
- rare earth
- pulse
- magnetic field
- earth permanent
- alloy
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The invention discloses a method for preparing bulk composite nanocrystalline rare earth permanent magnetic material. The method comprises the steps of: firstly, preparing an alloy ingot by vacuum smelting method; secondly, melting the alloy ingot and applying an external pulsed electric field in the molten alloy ingot to carry out electric pulse modification treatment; thirdly, preparing the bulk composite nanocrystalline rare earth permanent magnetic material by rapid solidification method in a copper mold under the action of an external pulsed magnetic field; finally, subjecting the material to proper thermal treatment according to the concrete condition. The method provided by the invention is simple and has short production period, and the prepared bulk composite nanocrystalline rare earth permanent magnetic material has fine grains, uniform texture, high density, and good comprehensive permanent magnetic performance.
Description
Technical field
The invention belongs to field of magnetic material preparation, be specifically related to a kind of method preparing bulk composite nanocrystalline rare earth permanent magnetic material.
Background technology
Nanocomposite rare earth permanent-magnetic material by nanocrystalline hard magnetic phase (as Nd
2fe
14b, Sm
2fe
17n
3) and soft magnetism phase (as α-Fe, Fe
3b) form, hard magnetic has high HCJ mutually, and soft magnetism has high saturation magnetization mutually, and two-phase interface place exists magnetic exchange coupling effect, make material have the high saturation and magnetic intensity of soft magnetism phase and the high-coercive force of hard magnetic phase simultaneously, thus there is high energy product.The magnetic energy product theoretical value of nanocrystalline composite magnets can reach 1000kJ/m
3, higher nearly 1 times than the theoretical magnetic energy product of Sintered NdFeB magnet.And the content of rare earth of nanocrystalline composite permanent-magnet material is few, low price, has wide development prospect, causes the attention of domestic and international investigation of materials personnel.
At present, the preparation method of such material mainly contains melt-quenching method and mechanical alloying method, and the product obtained is strip and powder mainly, drop into actual use and must be made into block.Adopt conventional powder sintering process to prepare fully dense block materials and can cause nanograin growth, thus significantly reduce magnetic property.Therefore Magnaglo and binding agent mix by people, make bonded permanent magnet, but add due to non-magnetic binder and auxiliary agent the magnetic property diluting magnetic, are unfavorable for the raising of magnet magnetic property.Simultaneously owing to there is the problem such as mobility of the uniformity consistency of magnetic, the kind of binding agent and addition, magnetic, often cause the density of bonded permanent magnet relatively low, mechanical strength is poor, in use easily produces distortion or breaks.Also some researchers are had to adopt discharge plasma sintering technique (Spark Plasma Sintering, be called for short SPS technology, Chinese Patent Application No.: 200510087114.5 and 2006910089122.8), superelevation hot pressing and sintering technique (Chinese Patent Application No.: 200810063723.0), electric field activation pressure assisted sintering technology (Chinese Patent Application No.: 200510021982.3) prepare bulk composite nanocrystalline rare earth permanent magnetic material.These methods can obtain the higher nanocomposite block permanent-magnetic material of density, but still the complex process of foundry alloy melting-broken powder process-magnetic compacting-sinter molding-machining can not be avoided, technique is loaded down with trivial details, production cycle is long, magnetic easily produces oxidation and pollutes, and to agglomerating plant and process control needs high, otherwise easily there is excessively growing up of nanocrystal, cause magnetism of material to worsen.Also have some researchers to adopt copper mold technology to prepare amorphous block material, then prepare nanocrystalline composite permanent-magnet material by crystallization and thermal treatment.But the cooling capacity of copper mold is limited, the amorphous formation ability of the RE permanent magnetic alloy such as Nd-Fe-B and Sm-Co is all more weak, have to carry heavy alloyed amorphous formation ability by the mode improving Boron contents or a large amount of interpolation nonmagnetic elements, thus sacrifice the magnetic property of magnet.On the other hand, the crystallization temperature difference of soft magnetism phase and Hard Magnetic phase two kinds of Magnetic Phases is larger, and there will be metastable phase in Amorphous Crystallization process and affect magnetic property (see IEEE Transactions On Magnetics 31 (1995) 3596-3601), therefore during crystallization, very high requirement is proposed to equipment for Heating Processing and process parameter control, otherwise easy generation crystallization is incomplete or the phenomenon of abnormal grain growth, causes magnet magnetic property to decline.
In order to overcome above-mentioned deficiency, the present invention adopts impulse electric field alloy melt to carry out inoculation, then rapid solidification under pulsed magnetic field action, can obtain the bulk composite nanocrystalline rare earth permanent magnetic material that crystal grain is tiny, even tissue, density are high, magnetic property is good.
Summary of the invention
The object of the present invention is to provide a kind of method preparing bulk composite nanocrystalline rare earth permanent magnetic material.The inventive method technique is simple, and with short production cycle, obtained bulk nano-crystalline permanent magnetic material crystal grain is tiny, even tissue, density are high, has good comprehensive permanent magnetism performance.
For achieving the above object, the present invention adopts following technical scheme:
A kind of concrete steps preparing the method for bulk nano-crystalline rare earth permanent-magnetic material are:
1) first prepared composition is R
xtM
100-x-ym
yalloy cast ingot, in formula, R is rare earth element, and wherein the content of Nd or Pr is no less than the 70at% of R total amount; TM is transition metal, IIIA race metal or IVA race metal, and wherein the content of Fe is no less than the 60at% of TM total amount; M is metalloid, and wherein B content is no less than the 80at% of M total amount; X is 3.5 ~ 11.6at%, y is 5 ~ 30at%; Ingot casting melting in arc furnace, induction furnace or magnetic levitation melting stove, melting is carried out under vacuum or high-purity argon gas protection.
2) ingot casting is put into bottom and open the quartz glass tube of aperture, and be placed in the vacuum spray to cast stove with impulse electric field and pulsed magnetic field apparatus, place water cooled copper mould in the lower end of quartz ampoule.Ingot casting induction melting under high-purity argon gas protection becomes liquid, then inserts in melt by electrode, applies impulse electric field, carry out Electric Pulse.During alloy melt Electric Pulse, the impulse electric field parameter of employing is: pulse frequency 50 ~ 2500Hz, pulse current peak density 10 ~ 5000A/cm
2, pulse duration 5 ~ 500 μ s, processing time 5 ~ 120s.With after-applied pulsed magnetic field, the magnetic line of force, through copper mold cavity, then opens the air valve be connected with quartz ampoule, and melt injects copper mold cavity fast by the aperture bottom quartz ampoule under the effect of spraying air pressure, the foundry goods of obtained designed shape.When alloy melt injects water cooled copper mould, the pulsed magnetic field parameter of employing is: pulse frequency 20 ~ 500Hz, pulsed magnetic field peak strength 0.3 ~ 5T, pulse duration 10 ~ 600 μ s, and the processing time is until alloy cool to room temperature from spray to cast.The cooling rate of alloy melt in water cooled copper mould is 100 ~ 5000 DEG C/sec.
3) carry out appropriate heat treatment to above-mentioned foundry goods as the case may be, heat treatment is carried out under vacuum or high-purity argon gas protection, and heat treatment temperature is 300 ~ 800 DEG C, and temperature retention time 0 ~ 10 minute, is then chilled to room temperature soon.
Remarkable advantage of the present invention is:
1) the present invention owing to have employed impulse electric field inoculation in alloy melt, and under pulsed magnetic field action, melt spray to cast is entered water cooled copper mould, the block rare earth permanent-magnetic material of preparation has tiny, uniform nanometer crystal microstructure structure, thus the exchange-coupling interaction enhanced between soft magnetism phase and hard magnetic phase nanocrystal, and magnet density is high, good comprehensive permanent magnetism performance and mechanical strength can be obtained.
2) the bulk nano-crystalline rare earth permanent-magnetic material prepared of the inventive method, required ree content is less, with low cost, and by changing shape and the size of copper mold cavity, can prepare the magnet of various shape, meeting the needs of engineer applied.
3) bulk nano-crystalline rare earth permanent-magnetic material preparation method of the present invention, production equipment is simple, and technological process is simple, and convenient operation, processes expend is few.
Accompanying drawing explanation
Fig. 1 is the demagnetization curve figure of bulk composite nanocrystalline rare earth permanent magnetic material in embodiment 1.
Fig. 2 is the X ray diffracting spectrum of bulk composite nanocrystalline rare earth permanent magnetic material in embodiment 1.
Fig. 3 is micro-organization chart's (transmission electron microscope photo) of bulk composite nanocrystalline rare earth permanent magnetic material in embodiment 1.
Embodiment
Elaborate below in conjunction with embodiment.
Adopting purity to be greater than Nd, Pr, Tb, Dy, Fe, Co, Zr, Ti, Ga, B, C etc. of 99.7wt% as raw material, is R according to composition
xtM
100-x-ym
ythe proportioning of (R is rare earth element, and TM is transition metal, IIIA race metal or IVA race metal, and M is metalloid) prepares, and in formula, x is 3.5 ~ 11.6at%, y is 5 ~ 30at%, puts into induction furnace, arc furnace or magnetic levitation melting stove, is evacuated down to 10
-5pa or more, then passes into 0.5 × 10
5~ 1.3 × 10
5the high-purity argon gas of Pa, under argon shield, melt back 4 ~ 8 times is to ensure the ingot casting obtaining uniform composition; Then, ingot casting is put into bottom and open the quartz glass tube of aperture, and be placed in the vacuum spray to cast stove with impulse electric field and pulsed magnetic field apparatus, place water cooled copper mould in the lower end of quartz ampoule, be evacuated down to 10
-5pa or more, then passes into 0.5 × 10
5~ 1.3 × 10
5the high-purity argon gas of Pa, ingot casting induction melting under argon shield becomes liquid, then inserts in melt by electrode, applies impulse electric field, carries out Electric Pulse.During alloy melt Electric Pulse, the impulse electric field parameter of employing is: pulse frequency 50 ~ 2500Hz, pulse current peak density 10 ~ 5000A/cm
2, pulse duration is 5 ~ 500 μ s, and the processing time is 5 ~ 120s.With after-applied pulsed magnetic field, the magnetic line of force, through copper mold cavity, then opens the air valve be connected with quartz ampoule, and melt injects copper mold cavity fast by the aperture bottom quartz ampoule under the effect of spraying air pressure, the foundry goods of obtained designed shape.When alloy melt injects water cooled copper mould, the pulsed magnetic field parameter of employing is: pulse frequency 20 ~ 500Hz, pulsed magnetic field peak strength 0.3 ~ 5T, pulse duration 10 ~ 600 μ s, and the processing time is until alloy cool to room temperature from spray to cast.Finally, as the case may be gained foundry goods is put into heat-treatment furnace, be evacuated to 10
-5pa or more, passes into 1.0 × 10
5~ 1.5 × 10
5the high-purity argon gas of Pa, is heated to 300 ~ 800 DEG C, and temperature retention time 0 ~ 10 minute, is then chilled to room temperature soon, obtains finished product.
Embodiment 1
Adopt purity be Nd, Fe, Co, Zr, Nb, Cr, Mo and B of 99.9wt% as raw material, according to Nd
10.5fe
56co
12zr
1nb
2cr
1mo
0.5b
17proportioning, put into magnetic levitation melting stove, be evacuated down to 10
-5pa, then passes into 1.1 × 10
5the high-purity argon gas of Pa, melt back 6 times under argon shield, to ensure the ingot casting obtaining uniform composition, for ensureing that the composition of ingot casting meets design mix substantially, must pay close attention to the waste of alloying element in fusion process.Then, alloy cast ingot is put into bottom with the quartz glass tube of aperture (aperture is 0.7mm), and be placed in the vacuum spray to cast stove with impulse electric field and pulsed magnetic field apparatus, water cooled copper mould is placed in quartz ampoule lower end, copper mold cavity internal diameter is 2mm, and length is 50mm.The vacuum degree be evacuated in spray to cast furnace cavity is 10
-5pa, then passes into 0.7 × 10
5the high-purity argon gas of Pa, ingot casting induction melting under high-purity argon gas protection becomes liquid, then inserts in melt by electrode; apply impulse electric field; carry out Electric Pulse, the impulse electric field parameter of employing is: pulse frequency 1200Hz, pulse current peak density 3000A/cm
2, pulse duration 100 μ s, the processing time is 60s.With after-applied pulsed magnetic field, its magnetic line of force flows uniformly across copper mold cavity, and perpendicular to the axis direction of copper mold cavity, the pulsed magnetic field parameter adopted is: pulse frequency 300Hz, pulsed magnetic field peak strength 2T, pulse duration 50 μ s, the processing time is until alloy cool to room temperature from spray to cast.Then open the air valve be connected with quartz ampoule, melt under the effect of spraying air pressure by the micropore jet bottom quartz ampoule in water cooled copper mould, obtaining diameter is 2mm, and length is the bar-shaped alloy of 50mm.With vibrating specimen magnetometer, the magnetic property result measuring magnet is as follows: B
r=0.76T,
ih
c=605kA/m, (BH)
max=102kJ/m
3, Fig. 1 is the demagnetization curve figure of this sample.With the phase constituent of X-ray diffractometer working sample, test result is shown in Fig. 2, and this sample known is by Nd
2fe
14b phase and α-Fe phase composition.By this sample microscopic structure of transmission electron microscope observation, as shown in Figure 3, can find out, microscopic structure is fine and close, and crystallite dimension is all less than 100nm.
The alloy cast ingot of identical component in the present embodiment, adopt traditional conventional copper mold rapid solidification method (no pulse electric field and pulse magnetic field treatment), obtained diameter is 2mm, and length is the bar-shaped alloy of 50mm.With vibrating specimen magnetometer, the magnetic property result measuring magnet is as follows: B
r=0.63T,
ih
c=457kA/m, (BH)
max=55kJ/m
3.Can find out, than conventional copper mold rapid solidification method, the remanent magnetism of nanocomposite rare earth permanent-magnetic material prepared by the present invention, HCJ and maximum magnetic energy product are all significantly improved.
Embodiment 2
Adopt purity be Nd, Dy, Fe, Y, Co, Nb, Zr, Ti, Si and B of 99.9wt% as raw material, according to Nd
9dy
0.5fe
59y
2co
9nb
1zr
1ti
1.5si
1b
16proportioning, put into magnetic levitation melting stove, be evacuated down to 10
-5pa, then passes into 1.1 × 10
5the high-purity argon gas of Pa, melt back 6 times under argon shield, to ensure the ingot casting obtaining uniform composition, for ensureing that the composition of ingot casting meets design mix substantially, must pay close attention to the waste of alloying element in fusion process.Then, alloy cast ingot is put into bottom with the quartz glass tube of aperture (aperture is 0.7mm), and be placed in the vacuum spray to cast stove with impulse electric field and pulsed magnetic field apparatus, water cooled copper mould is placed in quartz ampoule lower end, copper mold cavity internal diameter is 1.5mm, and length is 50mm.The vacuum degree be evacuated in spray to cast furnace cavity is 10
-5pa, then passes into 0.7 × 10
5the high-purity argon gas of Pa, ingot casting induction melting under high-purity argon gas protection becomes liquid, then inserts in melt by electrode; apply impulse electric field; carry out Electric Pulse, the impulse electric field parameter of employing is: pulse frequency 1500Hz, pulse current peak density 2500A/cm
2, pulse duration 50 μ s, the processing time is 90s.With after-applied pulsed magnetic field, its magnetic line of force flows uniformly across copper mold cavity, and perpendicular to the axis direction of copper mold cavity, the pulsed magnetic field parameter adopted is: pulse frequency 200Hz, pulsed magnetic field peak strength 3T, pulse duration 100 μ s, the processing time is until alloy cool to room temperature from spray to cast.Then open the air valve be connected with quartz ampoule, melt under the effect of spraying air pressure by the micropore jet bottom quartz ampoule in water cooled copper mould, obtaining diameter is 1.5mm, and length is the bar-shaped alloy of 50mm.The bar-shaped alloy of gained is loaded in vacuum heat treatment furnace, is evacuated to 10
-5pa, passes into 1.2 × 10
5the high-purity argon gas of Pa, is heated to 600 DEG C under high-purity argon gas protection, and insulation 30s, is chilled to room temperature soon.With vibrating specimen magnetometer, the magnetic property result measuring magnet is as follows: B
r=0.81T,
ih
c=623kA/m, (BH)
max=115kJ/m
3.
The alloy cast ingot of identical component in the present embodiment, adopt traditional conventional copper mold rapid solidification method (no pulse electric field and pulse magnetic field treatment), obtained diameter is 1.5mm, and length is the bar-shaped alloy of 50mm, and through identical Technology for Heating Processing.With vibrating specimen magnetometer, the magnetic property result measuring magnet is as follows: B
r=0.67T,
ih
c=503kA/m, (BH)
max=63kJ/m
3.Can find out, than conventional copper mold rapid solidification method, the remanent magnetism of nanocomposite rare earth permanent-magnetic material prepared by the present invention, HCJ and maximum magnetic energy product are all significantly improved.
Embodiment 3
Adopt purity be Nd, La, In, Fe, Co, Zr, Ti, Nb, Mo and B of 99.9wt% as raw material, according to (Nd
0.
95la
0.05)
4.5in
0.5fe
53.5co
10zr
2ti
1nb
1mo
1.5b
26proportioning, put into magnetic levitation melting stove, be evacuated down to 10
-5pa, then passes into 1.1 × 10
5the high-purity argon gas of Pa, melt back 6 times under argon shield, to ensure the ingot casting obtaining uniform composition, for ensureing that the composition of ingot casting meets design mix substantially, must pay close attention to the waste of alloying element in fusion process.Then, alloy cast ingot is put into bottom with the quartz glass tube of aperture (aperture is 0.7mm), and be placed in the vacuum spray to cast stove with impulse electric field and pulsed magnetic field apparatus, water cooled copper mould is placed in quartz ampoule lower end, copper mold cavity internal diameter is 5mm, and length is 50mm.The vacuum degree be evacuated in spray to cast furnace cavity is 10
-5pa, then passes into 0.7 × 10
5the high-purity argon gas of Pa, ingot casting induction melting under high-purity argon gas protection becomes liquid, then inserts in melt by electrode; apply impulse electric field; carry out Electric Pulse, the impulse electric field parameter of employing is: pulse frequency 50Hz, pulse current peak density 5000A/cm
2, pulse duration 500 μ s, the processing time is 7s.With after-applied pulsed magnetic field, its magnetic line of force flows uniformly across copper mold cavity, and perpendicular to the axis direction of copper mold cavity, the pulsed magnetic field parameter adopted is: pulse frequency 20Hz, pulsed magnetic field peak strength 5T, pulse duration 600 μ s, the processing time is until alloy cool to room temperature from spray to cast.Then open the air valve be connected with quartz ampoule, melt under the effect of spraying air pressure by the micropore jet bottom quartz ampoule in water cooled copper mould, obtaining diameter is 5mm, and length is the bar-shaped alloy of 50mm.The bar-shaped alloy of gained is loaded in vacuum heat treatment furnace, is evacuated to 10
-5pa, passes into 1.2 × 10
5the high-purity argon gas of Pa, is heated to 350 DEG C under high-purity argon gas protection, and insulation 10min, is chilled to room temperature soon.With vibrating specimen magnetometer, the magnetic property result measuring magnet is as follows: B
r=0.91T,
ih
c=315kA/m, (BH)
max=67kJ/m
3.
The alloy cast ingot of identical component in the present embodiment, adopt traditional conventional copper mold rapid solidification method (no pulse electric field and pulse magnetic field treatment), obtained diameter is 5mm, and length is the bar-shaped alloy of 50mm, and through identical Technology for Heating Processing.With vibrating specimen magnetometer, the magnetic property result measuring magnet is as follows: B
r=0.65T,
ih
c=227kA/m, (BH)
max=30kJ/m
3.Can find out, than conventional copper mold rapid solidification method, the remanent magnetism of nanocomposite rare earth permanent-magnetic material prepared by the present invention, HCJ and maximum magnetic energy product are all significantly improved.
Embodiment 4
Adopt purity be Nd, Pr, Tb, Fe, Co, Ga, Zr, Ti, Nb, V and B of 99.9wt% as raw material, according to Nd
7pr
2tb
0.
5fe
59.5co
6ga
1zr
1ti
2nb
1v
1b
19proportioning, put into magnetic levitation melting stove, be evacuated down to 10
-5pa, then passes into 1.1 × 10
5the high-purity argon gas of Pa, melt back 6 times under argon shield, to ensure the ingot casting obtaining uniform composition, for ensureing that the composition of ingot casting meets design mix substantially, must pay close attention to the waste of alloying element in fusion process.Then, alloy cast ingot is put into bottom with the quartz glass tube of aperture (aperture is 0.7mm), and be placed in the vacuum spray to cast stove with impulse electric field and pulsed magnetic field apparatus, water cooled copper mould is placed in quartz ampoule lower end, copper mold cavity internal diameter is 3mm, and length is 50mm.The vacuum degree be evacuated in spray to cast furnace cavity is 10
-5pa, then passes into 0.7 × 10
5the high-purity argon gas of Pa, ingot casting induction melting under high-purity argon gas protection becomes liquid, then inserts in melt by electrode; apply impulse electric field; carry out Electric Pulse, the impulse electric field parameter of employing is: pulse frequency 2500Hz, pulse current peak density 10A/cm
2, pulse duration 8 μ s, the processing time is 120s.With after-applied pulsed magnetic field, its magnetic line of force flows uniformly across copper mold cavity, and perpendicular to the axis direction of copper mold cavity, the pulsed magnetic field parameter adopted is: pulse frequency 500Hz, pulsed magnetic field peak strength 0.3T, pulse duration 10 μ s, the processing time is until alloy cool to room temperature from spray to cast.Then open the air valve be connected with quartz ampoule, melt under the effect of spraying air pressure by the micropore jet bottom quartz ampoule in water cooled copper mould, obtaining diameter is 3mm, and length is the bar-shaped alloy of 50mm.With vibrating specimen magnetometer, the magnetic property result measuring magnet is as follows: B
r=0.83T,
ih
c=557kA/m, (BH)
max=108kJ/m
3.
The alloy cast ingot of identical component in the present embodiment, adopt traditional conventional copper mold rapid solidification method (no pulse electric field and pulse magnetic field treatment), obtained diameter is 3mm, and length is the bar-shaped alloy of 50mm.With vibrating specimen magnetometer, the magnetic property result measuring magnet is as follows: B
r=0.62T,
ih
c=405kA/m, (BH)
max=52kJ/m
3.Can find out, than conventional copper mold rapid solidification method, the remanent magnetism of nanocomposite rare earth permanent-magnetic material prepared by the present invention, HCJ and maximum magnetic energy product are all significantly improved.
Embodiment 5
Adopt purity be Nd, Pr, Fe, Co, Y, Zr, Ti, Nb, Cr and B of 99.9wt% as raw material, according to Nd
3pr
1fe
71.5co
8y
1.5zr
1ti
2nb
1cr
1b
10proportioning, put into magnetic levitation melting stove, be evacuated down to 10
-5pa, then passes into 1.1 × 10
5the high-purity argon gas of Pa, melt back 6 times under argon shield, to ensure the ingot casting obtaining uniform composition, for ensureing that the composition of ingot casting meets design mix substantially, must pay close attention to the waste of alloying element in fusion process.Then, alloy cast ingot is put into bottom with the quartz glass tube of aperture (aperture is 0.7mm), and be placed in the vacuum spray to cast stove with impulse electric field and pulsed magnetic field apparatus, water cooled copper mould is placed in quartz ampoule lower end, copper mold cavity internal diameter is 2.5mm, and length is 50mm.The vacuum degree be evacuated in spray to cast furnace cavity is 10
-5pa, then passes into 0.7 × 10
5the high-purity argon gas of Pa, ingot casting induction melting under high-purity argon gas protection becomes liquid, then inserts in melt by electrode; apply impulse electric field; carry out Electric Pulse, the impulse electric field parameter of employing is: pulse frequency 300Hz, pulse current peak density 500A/cm
2, pulse duration 250 μ s, the processing time is 25s.With after-applied pulsed magnetic field, its magnetic line of force flows uniformly across copper mold cavity, and perpendicular to the axis direction of copper mold cavity, the pulsed magnetic field parameter adopted is: pulse frequency 70Hz, pulsed magnetic field peak strength 1T, pulse duration 300 μ s, the processing time is until alloy cool to room temperature from spray to cast.Then open the air valve be connected with quartz ampoule, melt under the effect of spraying air pressure by the micropore jet bottom quartz ampoule in water cooled copper mould, obtaining diameter is 2.5mm, and length is the bar-shaped alloy of 50mm.The bar-shaped alloy of gained is loaded in vacuum heat treatment furnace, is evacuated to 10
-5pa, passes into 1.2 × 10
5the high-purity argon gas of Pa, is heated to 750 DEG C under high-purity argon gas protection, and insulation 2min, is chilled to room temperature soon.With vibrating specimen magnetometer, the magnetic property result measuring magnet is as follows: B
r=0.94T,
ih
c=338kA/m, (BH)
max=75kJ/m
3.
The alloy cast ingot of identical component in the present embodiment, adopt traditional conventional copper mold rapid solidification method (no pulse electric field and pulse magnetic field treatment), obtained diameter is 2.5mm, and length is the bar-shaped alloy of 50mm, and through identical Technology for Heating Processing.With vibrating specimen magnetometer, the magnetic property result measuring magnet is as follows: B
r=0.68T,
ih
c=213kA/m, (BH)
max=32kJ/m
3.Can find out, than conventional copper mold rapid solidification method, the remanent magnetism of nanocomposite rare earth permanent-magnetic material prepared by the present invention, HCJ and maximum magnetic energy product are all significantly improved.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (1)
1. prepare a method for bulk composite nanocrystalline rare earth permanent magnetic material, it is characterized in that: concrete steps are:
1) first prepared composition is R
xtM
100-x-ym
yalloy cast ingot, in formula, R is rare earth element, and wherein the content of Nd or Pr is no less than the 70at% of R total amount; TM is transition metal, IIIA race metal or IVA race metal, and wherein the content of Fe is no less than the 60at% of TM total amount; M is metalloid, and wherein B content is no less than the 80at% of M total amount; X is 3.5 ~ 11.6at%, y is 5 ~ 30at%; Ingot casting melting in arc furnace, induction furnace or magnetic levitation melting stove, melting is carried out under vacuum or high-purity argon gas protection;
2) ingot casting is put into bottom and open the quartz glass tube of aperture, and be placed in the vacuum spray to cast stove with impulse electric field and pulsed magnetic field apparatus, place water cooled copper mould in the lower end of quartz ampoule; Ingot casting induction melting under high-purity argon gas protection becomes liquid, then inserts in melt by electrode, applies impulse electric field, carry out Electric Pulse; With after-applied pulsed magnetic field, the magnetic line of force, through copper mold cavity, then opens the air valve be connected with quartz ampoule, and melt injects copper mold cavity fast by the aperture bottom quartz ampoule under the effect of spraying air pressure, the foundry goods of obtained designed shape;
3) as the case may be appropriate heat treatment is carried out to above-mentioned foundry goods: heat treatment is carried out under vacuum or high-purity argon gas protection, and heat treatment temperature is 300 ~ 800 DEG C, and temperature retention time is 0 ~ 10 minute, is then chilled to room temperature soon;
During alloy melt Electric Pulse, the impulse electric field parameter of employing is pulse frequency 50 ~ 2500Hz, pulse current peak density 10 ~ 5000A/cm
2, pulse duration 5 ~ 500 μ s, processing time 5 ~ 120s;
When alloy melt injects water cooled copper mould, the pulsed magnetic field parameter of employing is pulse frequency 20 ~ 500Hz, pulsed magnetic field peak strength 0.3 ~ 5T, pulse duration 10 ~ 600 μ s, and the processing time is until alloy cool to room temperature from spray to cast;
The cooling rate of alloy melt in water cooled copper mould is 100 ~ 5000 DEG C/sec.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210005073.0A CN102568729B (en) | 2012-01-10 | 2012-01-10 | Method for preparing bulk composite nanocrystalline rare earth permanent magnetic material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210005073.0A CN102568729B (en) | 2012-01-10 | 2012-01-10 | Method for preparing bulk composite nanocrystalline rare earth permanent magnetic material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102568729A CN102568729A (en) | 2012-07-11 |
| CN102568729B true CN102568729B (en) | 2015-04-15 |
Family
ID=46413914
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210005073.0A Expired - Fee Related CN102568729B (en) | 2012-01-10 | 2012-01-10 | Method for preparing bulk composite nanocrystalline rare earth permanent magnetic material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102568729B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103794355B (en) * | 2014-02-25 | 2016-05-18 | 浙江爱特新能源汽车有限公司 | A kind of preparation method of the neodymium iron boron magnetic body with high-Curie-point |
| CN103794320B (en) * | 2014-03-04 | 2017-01-18 | 南京信息工程大学 | Neodymium iron nitrogen permanent magnet material and preparation method |
| CN103894587B (en) * | 2014-03-20 | 2016-10-05 | 华南理工大学 | A kind of Nd-Fe-B permanent magnet material and preparation method assist direct casting device with magnetic field |
| CN104588622B (en) * | 2014-12-24 | 2017-06-06 | 北方民族大学 | Metal bath bulk nanostructured material preparation system |
| CN106057461A (en) * | 2016-05-20 | 2016-10-26 | 中国计量大学 | Anisotropic blocky nanocomposite permanent magnet and preparation method therefor |
| CN107790650B (en) * | 2016-09-06 | 2019-03-26 | 鞍钢股份有限公司 | A kind of micro alloyed steel directly fills the control method for rolling plate crackle |
| CN112201429B (en) * | 2020-10-14 | 2021-12-21 | 燕山大学 | Permanent magnet with nanoscale gradient structure and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002038245A (en) * | 2000-07-27 | 2002-02-06 | Hitachi Metals Ltd | Rare earth alloy powder for rermanent magnet and method for manufacturing rare earth permanent magnet |
| CN100465323C (en) * | 2007-07-13 | 2009-03-04 | 上海大学 | Nano crystal composite permanent-magnet alloy and its preparation method |
| CN102108452B (en) * | 2011-02-15 | 2013-01-23 | 江苏大学 | Method for synthesizing particle reinforced composite material under pulsed electric field and electromagnetic field |
-
2012
- 2012-01-10 CN CN201210005073.0A patent/CN102568729B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN102568729A (en) | 2012-07-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102568729B (en) | Method for preparing bulk composite nanocrystalline rare earth permanent magnetic material | |
| CN102737801B (en) | Method for preparing Sm-Fe-N anisotropic magnetic powder | |
| CN108039258A (en) | A kind of high temperature high-coercive force samarium-cobalt permanent-magnetic material and preparation method | |
| CN101620906B (en) | Block-shaped nanocrystalline magnetically soft alloy material and preparation method thereof | |
| CN106935350A (en) | A kind of anisotropy SmCo5Type rare earth permanent-magnetic material and preparation method | |
| CN102543341B (en) | Method for preparing anisotropic nanocrystalline rare-earth permanent magnet block material | |
| WO2016201944A1 (en) | Preparation method of ndfeb magnet having low melting point light rare-earth-copper alloy at grain boundary | |
| CN104576028A (en) | Methods for manufacturing cerium-rich anisotropy nano-crystalline rare-earth permanent magnets | |
| CN102140598B (en) | Preparation method of super high coercivity and low-Co type Sm-Co nanocrystalline alloy | |
| CN106448986A (en) | Anisotropic nanocrystalline rare earth permanent magnet and preparation method therefor | |
| CN108063045A (en) | A kind of no heavy rare earth Nd-Fe-B permanent magnet material and preparation method thereof | |
| CN106384637A (en) | Method for improving boundary structure to prepare high-performance neodymium iron boron magnet | |
| CN104851545A (en) | Production method of permanent magnet material with grain boundary diffusion layer | |
| CN107564644B (en) | A kind of compound samarium ferromagnetic alloy of nanoporous two-phase and preparation method thereof | |
| CN107564651A (en) | A kind of high remanent magnetism material and preparation method thereof | |
| CN101265529A (en) | Method for preparing block-shaped nano-crystal SmCo series permanent magnetic material | |
| CN103280288B (en) | A kind of preparation method of high-coercive force SmCo based permanent magnetic material | |
| CN110534279A (en) | A kind of pure high abundance Rare-Earth Ce, La, the nanocrystalline permanent-magnet alloy of the Quito Y member and preparation | |
| CN101673605B (en) | Anisotropic nano/amorphous complex phase block permanent-magnetic material and preparation method thereof | |
| Li et al. | Bulk amorphous powder cores with low core loss by spark-plasma sintering Fe76Si9. 6B8. 4P6 amorphous powder with small amounts of SiO2 | |
| CN103632835A (en) | Rapid forming method of high-performance Nd-Fe-B magnetic body | |
| CN104846255B (en) | A kind of preparation method of yttrium iron based permanent magnetic material | |
| CN110079749A (en) | A kind of iron based nano crystal-amorphous soft magnet magnetically soft alloy and the preparation method and application thereof | |
| CN105280319B (en) | Rare-earth iron-boron material prepared by technical pure mischmetal and its preparation method and application | |
| CN103258609B (en) | The preparation method of anisotropism nanometer rare earth permanent magnetic material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150415 Termination date: 20180110 |