CN105374484A - High-coercivity samarium-cobalt permanent magnet material and preparation method thereof - Google Patents
High-coercivity samarium-cobalt permanent magnet material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-coercivity samarium-cobalt permanent magnet material and a preparation method thereof. The high-coercivity samarium-cobalt permanent magnet material comprises a main alloy and an auxiliary alloy, wherein a chemical formula of the main alloy is Sm<x>Co<y>Fe<z>Cu<w>Zr<bal>; x is smaller than or equal to 27% and greater than or equal to 24%; y is smaller than or equal to 55% and greater than or equal to 45%; z is smaller than or equal to 20% and greater than or equal to 15%; w is smaller than or equal to 10% and greater than or equal to 4%; the chemical formula of the auxiliary alloy is N<a>M<b>Fe<c>; N represents one or a mixture of light rare earth elements Sm, Pr and Nd; M is one or the mixture of heavy rare earth elements Dy and Tb; a is smaller than or equal to 25% and greater than or equal to 20%; b is smaller than or equal to 65% and greater than or equal to 60%; c is smaller than or equal to 20% and greater than or equal to 15%; and meanwhile, Dy<2>O<3> powder which is equivalent to 0.1%-0.5% of the weight of the main alloy is added. According to the high-coercivity samarium-cobalt permanent magnet material, growth of crystal particles in a sintering process can be prevented; the crystal particles of a samarium-cobalt alloy are refined; and improvement of the coercivity is facilitated; and continuously adjustable coercivity can be achieved by proportioning the main alloy and the auxiliary alloy with different ratios.
Description
Technical field
The present invention relates to a kind of samarium-cobalt permanent-magnetic material and preparation method thereof, particularly relate to a kind of high-coercive force samarium-cobalt permanent-magnetic material and preparation method thereof.
Background technology
Sintered samarium cobalt permanent magnetic material, because of the magnetic property that it is excellent, particularly has higher coercive force and low-temperature coefficient, good resistance to elevated temperatures and corrosion resistance, in a lot of fields, is particularly used widely in high temperature environments.Traditional Sm
2co
17the main component of type samarium-cobalt permanent-magnetic material is samarium, cobalt, iron, copper, zirconium, and general serviceability temperature is no more than 400-450 DEG C, if improve serviceability temperature again, can bring the sharply reduction of coercive force and magnetic energy product.In order to improve the serviceability temperature of samarium cobalt permanent magnet further, need the coercive force and the reduction coercive force temperature coefficient that improve samarium cobalt permanent magnet further.
In existing patent, if application number is the Chinese patent application etc. of 201010176900.3,201110030314.2, adopt single alloyage to add heavy rare earth element and improve coercive force, reduce temperature coefficient, but this method can not regulate and control coercive force.In ZL201210576210.6, by adopting the first samarium-cobalt alloy and the second samarium-cobalt alloy ingot casting containing heavy rare earth, mixing and ball milling powder process after coarse crushing; Be in the Chinese patent application of 201310196922.X at application number, mention the mixed-powder adopting the low-melting alloy powder be mixed with containing heavy rare earth.What both adopted above is all that common melting casting ingot method prepares alloy.
Application number is the Chinese patent application of 201410532244.4, adopts solwution method to obtain SmCo powder, but this method complex process, industrialization cost is higher.
Summary of the invention
Technical problem to be solved by this invention overcomes the deficiencies in the prior art, provides a kind of high-coercive force samarium-cobalt permanent-magnetic material and preparation method thereof.
The technical solution adopted for the present invention to solve the technical problems is:
The high-coercive force samarium-cobalt permanent-magnetic material of the present invention, comprises master alloying and secondary alloy, and master alloying and secondary alloy mass ratio are 100: 1-5; Master alloying chemical formula is Sm
xco
yfe
zcu
wzr
bal, x, y, z in formula, w, bal be the mass percent of respective element in expression respectively, 24%≤x≤27%, 45%≤y≤55%, 15%≤z≤20%, 4%≤w≤10%, wherein x+y+z+w+bal=100%; Secondary alloy formula is N
am
bfe
c, N represents one in light rare earth element Sm, Pr, Nd or complex element, and M is a kind of in heavy rare earth element Dy, Tb or complex element, in formula, a, b, c represent the mass percent of respective element, 20%≤a≤25%, 60%≤b≤65%, 15%≤c≤20%, wherein a+b+c=100%; Add the Dy being equivalent to master alloying powder quality 0.1-0.5% simultaneously
2o
3powder.
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present invention, coordinates prior powder metallurgy technique to prepare samarium cobalt permanent magnet by two alloyage, prepares master alloying and secondary alloy, specifically comprise the following steps:
The preparation that step (1), (2), (3) are master alloying powder:
(1) prepare burden: master alloying is Sm by chemical formula
xco
yfe
zcu
wzr
balmass percent batching, x, y, z in formula, w, bal be the mass percent of respective element in expression respectively, 24%≤x≤27%, 45%≤y≤55%, 15%≤z≤20%, 4%≤w≤10%, wherein x+y+z+w+bal=100%;
Raw material preferably adopts the metal of purity >=99.9%;
(2) melting: master alloying raw material step (1) prepared drops in vacuum induction melting furnace crucible, is evacuated to 3 ~ 6Pa, is preheated to 600-700 DEG C, applying argon gas to 9 × 10
5~ 9.01 × 10
5pa, improves power and carries out melting to 50-60kw, and after alloy melts completely, insulation 8 ~ 10min, is then poured in water cooled copper mould by aluminium alloy, makes alloy cast ingot;
(3) powder process: the particle first alloy cast ingot of step (2) being become 0.1-0.3mm size by coarse crushing; Again the alloying pellet of coarse crushing is made the fine powder of 3.0-5.0 micron by planetary ball mill or rolling ball milling, winner's alloy powder;
The preparation that step (4), (5), (6) are secondary alloyed powder:
(4) prepare burden: secondary alloy is N by chemical formula
am
bfe
c, N represents one in light rare earth element Sm, Pr, Nd or complex element, and M is a kind of in heavy rare earth element Dy, Tb or complex element, in formula, a, b, c represent the mass percent of respective element, 20%≤a≤25%, 60%≤b≤65%, 15%≤c≤20%, wherein a+b+c=100%;
Raw material preferably adopts the metal of purity >=99.9%;
(5) melting: secondary alloy raw material step (4) prepared drops into vacuum induction and gets rid of in band smelting furnace crucible, is evacuated to 3 ~ 6Pa, is preheated to 600-700 DEG C, applying argon gas to 9 × 10
5~ 9.01 × 10
5pa, improve power carry out melting to 50-60kw, after alloy melts completely, be incubated 8 ~ 10min, then aluminium alloy is poured on water-cooled copper roller, make average thickness be 0.2 ~ 0.5mm get rid of strap;
(6) powder process: secondary for step (5) gained alloy is got rid of the broken method of strap hydrogen and carry out hydrogen and break, make the meal that average grain diameter is 100 ~ 200 microns, 2 ~ 5mL antioxidant and 2 ~ 5mL gasoline is added by every kilogram of meal, then airflow milling is passed through, obtained particle mean size is the (N of 3 ~ 5 microns, M, Fe)-H
xrare earth hydride magnetic, i.e. secondary alloy powder;
At least one in the preferred benzinum of described antioxidant, cyclohexane, dichlorodifluoromethan;
(7) batch mixing: by step (3) gained master alloying powder and the secondary alloy powder batching of (6) gained, the mass ratio of master alloying powder and secondary alloy powder is 100:1-5, adds the Dy being equivalent to master alloying powder quality 0.1-0.5% simultaneously
2o
3powder, then mixes 0.5-1.5h on batch mixer, the mixing magnetic of obtained granularity and uniform composition;
(8) shaping: to be oriented moulding in the magnetic field of 1.5-2.0T in magnetic field intensity by step (7) gained mixing magnetic, then isostatic pressed, stripping oil is carried out, blank product with inner membrance is transported in sintering furnace glove box and peels inner membrance off, obtain pressed compact (preparing sintering);
(9) sinter: step (8) gained pressed compact is transported to sintering furnace burner hearth high temperature sintering, suction to 2.5 × 10
-2-5 × 10
-2pa, calcined temperature 1175-1185 DEG C, insulation 0.5-1.5h; Sintering temperature is 1190-1210 DEG C, insulation 1-2h; Solid solubility temperature 1175-1185 DEG C, insulation 0.5-2h; Solid solution terminates rear air-cooled to 60 ~ 80 DEG C;
(10) tempering: the product after step (9) sintering is carried out one-level Ageing Treatment and secondary time effect process, wherein one-level aging temp 800 ~ 850 DEG C, is incubated 10 ~ 20 hours, secondary time effect temperature 400 ~ 450 DEG C, is incubated 10 ~ 15 hours.
Further, in step (5), during secondary alloy melting, the rotating speed of described water-cooled copper roller is 3 ~ 4m/s.
Further, in step (6), described jet mill sorting wheel rotating speed is 2500 ~ 3500r/min.
Compared with prior art, the present invention has the following advantages:
1, by the different ratio of master alloying and secondary alloy two kinds of alloys, the heavy rare earth elements such as Dy or Tb are introduced from composition, form the Hard Magnetic outer shell containing heavy rare earth Dy or Tb, enhance the local magnetocrystalline anisotropy in main phase grain boundary layer, degaussing coupling between effectively playing neighboring die, improves coercive force.Add rare earth hydride when batch mixing, due to the high activity after hydride dehydrogenation, can reduce the oxidation of samarium-cobalt alloy, rare earth hydride can dilute the content of heavy rare earth in crystal boundary, effectively improves coercive force, and realizes the efficiency utilization of Dy.Small amounts thing Dy
2o
3add growing up of crystal grain when can stop sintering, the crystal grain of refinement samarium-cobalt alloy, be conducive to improving coercive force.
2, the major-minor alloy proportion of different proportion, can realize coercitive continuously adjustabe, according to requirements prepares the samarium-cobalt alloy of heterogeneity, thus meets different performance requirement.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
In each embodiment, the raw material selected by batching is the metal of purity 99.9%.
Embodiment 1
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, comprises master alloying and secondary alloy, and master alloying and secondary alloy mass ratio are 100: 1; Master alloying chemical formula is Sm
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%, secondary alloy is Sm by chemical formula
20%dy
60%fe
20%.
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, coordinates prior powder metallurgy technique to prepare samarium cobalt permanent magnet by two alloyage, prepares master alloying and secondary alloy, specifically comprise the following steps:
The preparation that step (1), (2), (3) are master alloying powder:
(1) prepare burden: chemical formula Sm pressed by master alloying
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%mass percent batching;
(2) melting: master alloying raw material step (1) prepared drops in vacuum induction melting furnace crucible, is evacuated to 5Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improves power and carries out melting to 50kw, and after alloy melts completely, insulation 8min, is then poured in water cooled copper mould by aluminium alloy, makes alloy cast ingot;
(3) powder process: the particle first alloy cast ingot of step (2) being become particle diameter 0.15mm-0.25mm size by coarse crushing; Again the alloying pellet of coarse crushing is made the fine powder of 3.5-4.0 μm by planetary ball mill or rolling ball milling, winner's alloy powder;
The preparation that step (4), (5), (6) are secondary alloyed powder:
(4) prepare burden: chemical formula Sm pressed by secondary alloy
20%dy
60%fe
20%mass percent batching;
(5) melting: secondary alloy raw material step (4) prepared drops into vacuum induction and gets rid of in band smelting furnace crucible, is evacuated to 3.5Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improve power carry out melting to 50kw, after alloy melts completely, be incubated 10min, be then poured into by aluminium alloy on water-cooled copper roller, the rotating speed of water-cooled copper roller is 3.5m/s, make average thickness be 0.35mm get rid of strap;
(6) powder process: secondary for step (5) gained alloy is got rid of the broken method of strap hydrogen and carry out hydrogen and break, make the meal that particle mean size is 180 μm, every kilogram of meal adds 3mL cyclohexane and 5mL gasoline, then airflow milling is passed through, jet mill sorting wheel rotating speed is 3300r/min, obtained particle mean size is (Sm, Dy, Fe)-H of 3.3 μm
xmagnetic, i.e. secondary alloy powder;
(7) step (3) gained master alloying powder and the secondary alloy powder of (6) gained are prepared burden according to mass ratio 100:1, then on batch mixer, mix 1h, the mixing magnetic of obtained granularity and uniform composition;
(8) shaping: to be oriented moulding in the magnetic field of 1.8T in magnetic field intensity by step (7) gained mixing magnetic, then carry out isostatic pressed, stripping oil, the blank product with inner membrance is transported in sintering furnace glove box and peels inner membrance off, obtain pressed compact (preparing sintering);
(9) sinter: the pressed compact of step (8) is transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10
-2pa, calcined temperature 1185 DEG C, insulation 1h, sintering temperature is 1200 DEG C, insulation 1.5h, solid solubility temperature 1185 DEG C, insulation 1h, and solid solution terminates rear air-cooled to 70 DEG C;
(10) tempering: the product after step (9) sintering is carried out one-level timeliness and secondary time effect process, wherein one-level aging temp 850 DEG C, is incubated 10 hours, secondary time effect temperature 400 DEG C, is incubated 10 hours.
Embodiment 2
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, comprises master alloying and secondary alloy, and master alloying and secondary alloy mass ratio are 100: 1; Master alloying chemical formula is Sm
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%, secondary alloy is Sm by chemical formula
20%dy
60%fe
20%.
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, coordinates prior powder metallurgy technique to prepare samarium cobalt permanent magnet by two alloyage, prepares master alloying and secondary alloy, specifically comprise the following steps:
The preparation that step (1), (2), (3) are master alloying powder:
(1) prepare burden: chemical formula Sm pressed by master alloying
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%mass percent batching;
(2) master alloying raw material step (1) prepared drops in vacuum induction melting furnace crucible, is evacuated to 5Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improves power and carries out melting to 60kw, and after alloy melts completely, insulation 8min, is then poured in water cooled copper mould by aluminium alloy, makes alloy cast ingot;
(3) first the alloy cast ingot of step (2) is become the particle of average grain diameter 0.15mm size by coarse crushing; Again the alloying pellet of coarse crushing is made the fine powder of average grain diameter 3.5 μm by planetary ball mill, winner's alloy powder;
The preparation that step (4), (5), (6) are secondary alloyed powder:
(4) chemical formula Sm pressed by secondary alloy
20%dy
60%fe
20%mass percent batching;
(5) the secondary alloy raw material vacuum induction that step (4) prepares is got rid of in band smelting furnace crucible, be evacuated to 3.5Pa, be preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improve power carry out melting to 60kw, after alloy melts completely, be incubated 10min, be then poured into by aluminium alloy on water-cooled copper roller, the rotating speed of water-cooled copper roller is 3.5m/s, make average thickness be 0.35mm get rid of strap;
(6) secondary for step (5) gained alloy is got rid of the broken method of strap hydrogen to carry out hydrogen and break, make the meal that particle mean size is 180 μm, every kilogram of meal adds 3mL antioxidant cyclohexane and 5mL gasoline, then airflow milling is passed through, jet mill sorting wheel rotating speed is 3300r/min, obtained particle mean size is (Sm, Dy, Fe)-H of 3.3 μm
xmagnetic, i.e. secondary alloy powder;
(7) by step (3) gained master alloying powder and the secondary alloy powder batching of (6) gained, master alloying powder and secondary alloy powder, according to 100:1 ratio batching, add the Dy being equivalent to master alloying quality 0.1%
2o
3powder, then mixes 1h on batch mixer, the mixing magnetic of obtained granularity and uniform composition;
(8) by step (7) gained mixing magnetic in magnetic field intensity be 1.8T magnetic field in oriented moulding, then carry out isostatic pressed, stripping oil, the blank product with inner membrance be transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact (prepare sintering);
(9) pressed compact of step (8) is transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10
-2pa, calcined temperature 1185 DEG C, insulation 1h, sintering temperature is 1200 DEG C, insulation 1.5h, solid solubility temperature 1185 DEG C, insulation 1h, and solid solution terminates rear air-cooled to 70 DEG C;
(10) tempering: the product after step (9) being sintered carries out one-level timeliness and secondary time effect process, wherein one-level aging temp 850 DEG C, is incubated 10 hours, secondary time effect temperature 400 DEG C, is incubated 10 hours.
Embodiment 3
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, comprises master alloying and secondary alloy, and master alloying and secondary alloy mass ratio are 100: 3; Master alloying chemical formula is Sm
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%, secondary alloy is Sm by chemical formula
20%dy
60%fe
20%.
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, coordinates prior powder metallurgy technique to prepare samarium cobalt permanent magnet by two alloyage, prepares master alloying and secondary alloy, specifically comprise the following steps:
The preparation that step (1), (2), (3) are master alloying powder:
(1) chemical formula Sm pressed by master alloying
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%mass percent batching;
(2) master alloying raw material step (1) prepared drops in vacuum induction melting furnace crucible, is evacuated to 5Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improves power and carries out melting to 60kw, and after alloy melts completely, insulation 8min, is then poured in water cooled copper mould by aluminium alloy, makes on copper roller, make alloy cast ingot;
(3) first the alloy cast ingot of step (2) is become the particle of average grain diameter 0.15mm size by coarse crushing; Again the alloying pellet of coarse crushing is made the fine powder of average grain diameter 3.5 μm by rolling ball milling, winner's alloy powder;
The preparation that step (4), (5), (6) are secondary alloyed powder:
(4) chemical formula Sm pressed by secondary alloy
20%dy
60%fe
20%mass percent batching;
(5) secondary alloy raw material step (4) prepared drops into vacuum induction and gets rid of in band smelting furnace crucible, is evacuated to 3.5Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improve power carry out melting, after alloy melts completely, insulation 10min, be then poured into by aluminium alloy on water-cooled copper roller, the rotating speed of water-cooled copper roller is 3.5m/s, make average thickness be 0.35mm get rid of strap;
(6) secondary for step (5) gained alloy is got rid of the broken method of strap hydrogen to carry out hydrogen and break, make the meal that particle mean size is 180 μm, every kilogram of meal adds 3mL antioxidant cyclohexane and 5mL gasoline, then airflow milling is passed through, jet mill sorting wheel rotating speed is 3300r/min, obtained particle mean size is (Sm, Dy, Fe)-H of 3.3 μm
xmagnetic, i.e. secondary alloy powder;
(7) by step (3) gained master alloying powder and the secondary alloy powder batching of (6) gained, master alloying powder and secondary alloy powder are prepared burden according to mass ratio 100:3, add and are equivalent to master alloying quality 0.2%Dy
2o
3powder, then mixes 1h on batch mixer, the mixing magnetic of obtained granularity and uniform composition;
(8) by step (7) gained mixing magnetic in magnetic field intensity be 1.8T magnetic field in oriented moulding, then carry out isostatic pressed, stripping oil, the blank product with inner membrance be transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact (prepare sintering);
(9) pressed compact of step (8) is transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10
-2pa, calcined temperature 1185 DEG C, insulation 1h, sintering temperature is 1200 DEG C, insulation 1.5h, solid solubility temperature 1185 DEG C, insulation 1h, and solid solution terminates rear air-cooled to 70 DEG C;
(10) tempering: the product after step (9) sintering is carried out one-level timeliness and secondary time effect process, wherein one-level aging temp 850 DEG C, is incubated 10 hours, secondary time effect temperature 400 DEG C, is incubated 10 hours.
Embodiment 4
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, comprises master alloying and secondary alloy, and master alloying and secondary alloy mass ratio are 100: 5; Master alloying chemical formula is Sm
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%, secondary alloy formula is Sm
20%dy
60%fe
20%.
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, coordinates prior powder metallurgy technique to prepare samarium cobalt permanent magnet by two alloyage, prepares master alloying and secondary alloy, specifically comprise the following steps:
The preparation that step (1), (2), (3) are master alloying powder:
(1) chemical formula Sm pressed by master alloying
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%mass percent batching;
(2) master alloying raw material step (1) prepared drops in vacuum induction melting furnace crucible, is evacuated to 5Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improves power and carries out melting to 60kw, and after alloy melts completely, insulation 8min, is then poured in water cooled copper mould by aluminium alloy, makes alloy cast ingot;
(3) first the alloy cast ingot of step (2) is become the particle of average grain diameter 0.15mm size by coarse crushing; Again the alloying pellet of coarse crushing is made by rolling ball milling the fine powder that average grain diameter is 3.5 μm, winner's alloy powder;
The preparation that step (4), (5), (6) are secondary alloyed powder:
(4) chemical formula Sm pressed by secondary alloy
20%dy
60%fe
20%mass percent batching;
(5) secondary alloy raw material step (4) prepared drops into vacuum induction and gets rid of in band smelting furnace crucible, is evacuated to 3.5Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improve power carry out melting to 60kw, after alloy melts completely, be incubated 10min, be then poured into by aluminium alloy on water-cooled copper roller, the rotating speed of water-cooled copper roller is 3.5m/s, make average thickness be 0.35mm get rid of strap;
(6) secondary for step (5) gained alloy is got rid of the broken method of strap hydrogen to carry out hydrogen and break, make the meal that particle mean size is 180 μm, every kilogram of meal adds 3mL antioxidant cyclohexane and 5mL gasoline, then airflow milling is passed through, jet mill sorting wheel rotating speed is 3300r/min, obtained particle mean size is (Sm, Dy, Fe)-H of 3.3 μm
xmagnetic, i.e. secondary alloy powder;
(7) step (3) gained master alloying powder and the secondary alloy powder of (6) gained are prepared burden according to 100:5 mass ratio, add and be equivalent to master alloying powder quality 0.3%Dy
2o
3powder, then mixes 1h on batch mixer, the mixing magnetic of obtained granularity and uniform composition;
(8) by step (7) gained mixing magnetic in magnetic field intensity be 1.8T magnetic field in oriented moulding, then carry out isostatic pressed, stripping oil, the blank product with inner membrance be transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact (prepare sintering);
(9) pressed compact of step (8) is transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10
-2pa, calcined temperature 1185 DEG C, insulation 1h, sintering temperature is 1200 DEG C, insulation 1.5h, solid solubility temperature 1185 DEG C, insulation 1h, and solid solution terminates rear air-cooled to 70 DEG C;
(10) tempering: the product after step (9) being sintered carries out one-level timeliness and secondary time effect process, wherein one-level aging temp 850 DEG C, is incubated 10 hours, secondary time effect temperature 400 DEG C, is incubated 10 hours.
Embodiment 5
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, comprises master alloying and secondary alloy, and master alloying and secondary alloy mass ratio are 100: 1; Master alloying chemical formula is Sm
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%, secondary alloy is Sm by chemical formula
20%tb
60%fe
20%.
The concrete steps of its preparation method are:
The preparation that step (1), (2), (3) are master alloying powder:
(1) chemical formula Sm pressed by master alloying
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%mass percent batching;
(2) master alloying raw material step (1) prepared drops in vacuum induction melting furnace crucible, is evacuated to 3Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improves power and carries out melting to 60kw, and after alloy melts completely, insulation 10min, is then poured in water cooled copper mould by aluminium alloy, makes alloy cast ingot;
(3) first the alloy cast ingot of step (2) is become the particle of average grain diameter 0.1mm size by coarse crushing; Again the alloying pellet of coarse crushing is made the fine powder of average grain diameter 3.3 μm by planetary ball mill;
The preparation that step (4), (5), (6) are secondary alloyed powder:
(4) by chemical formula Sm
20%tb
60%fe
20%mass percent batching;
(5) secondary alloy raw material step (4) prepared drops into vacuum induction and gets rid of in band smelting furnace crucible, is evacuated to 3Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improve power carry out melting to 60kw, after alloy melts completely, be incubated 8min, be then poured into by aluminium alloy on water-cooled copper roller, the rotating speed of water-cooled copper roller is 3.5m/s, make average thickness be 0.35mm get rid of strap;
(6) secondary for step (5) gained alloy is got rid of the broken method of strap hydrogen to carry out hydrogen and break, make the meal that particle mean size is 150 μm, every kilogram of meal adds 3mL antioxidant cyclohexane and 5mL gasoline, then airflow milling is passed through, jet mill sorting wheel rotating speed is 3300r/min, obtained particle mean size is (Sm, Tb, Fe)-H of 3.5 μm
xmagnetic, i.e. secondary alloy powder;
(7) step (3) gained master alloying powder and the secondary alloy powder of (6) gained are prepared burden according to mass ratio 100:1 ratio, add the Dy being equivalent to master alloying powder quality 0.1%
2o
3powder, then mixes 1.5h on batch mixer, the mixing magnetic of obtained granularity and uniform composition;
(8) by step (7) gained mixing magnetic in magnetic field intensity be 1.6T magnetic field in oriented moulding, then carry out isostatic pressed, stripping oil, the blank product with inner membrance be transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact (prepare sintering);
(9) pressed compact of step (8) is transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10
-2pa, calcined temperature 1175 DEG C, insulation 1h, sintering temperature is 1205 DEG C, insulation 1h, solid solubility temperature 1175 DEG C, insulation 1h, and solid solution terminates rear air-cooled to 70 DEG C;
(10) tempering: the product after step (9) being sintered carries out one-level timeliness and secondary time effect process, wherein one-level aging temp 800 DEG C, is incubated 20 hours, secondary time effect temperature 420 DEG C, is incubated 10 hours.
Embodiment 6
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, comprises master alloying and secondary alloy, and master alloying and secondary alloy mass ratio are 100: 3; Master alloying chemical formula is Sm
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%, secondary alloy formula is Sm
20%tb
60%fe
20%.
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, coordinates prior powder metallurgy technique to prepare samarium cobalt permanent magnet by two alloyage, prepares master alloying and secondary alloy, specifically comprise the following steps:
The preparation that step (1), (2), (3) are master alloying powder:
(1) chemical formula Sm pressed by master alloying
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%mass percent batching;
(2) master alloying raw material step (1) prepared drops in vacuum induction melting furnace crucible, is evacuated to 3Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improves power and carries out melting to 60kw, and after alloy melts completely, insulation 10min, is then poured in water cooled copper mould by aluminium alloy, makes alloy cast ingot;
(3) first the alloy cast ingot of step (2) is become the particle of average grain diameter 0.1mm size by coarse crushing; Again the alloying pellet of coarse crushing is made the fine powder of average grain diameter 3.3 μm by planetary ball mill;
The preparation that step (4), (5), (6) are secondary alloyed powder:
(4) chemical formula Sm pressed by secondary alloy
20%tb
60%fe
20%mass percent batching;
(5) secondary alloy raw material step (4) prepared drops into vacuum induction and gets rid of in band smelting furnace crucible, is evacuated to 3Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improve power carry out melting to 60kw, after alloy melts completely, be incubated 8min, be then poured into by aluminium alloy on water-cooled copper roller, the rotating speed of water-cooled copper roller is 3.5m/s, make average thickness be 0.35mm get rid of strap;
(6) secondary for step (5) gained alloy is got rid of the broken method of strap hydrogen to carry out hydrogen and break, make the meal that particle mean size is 150 μm, every kilogram of meal adds 3mL antioxidant cyclohexane and 5mL gasoline, then airflow milling is passed through, jet mill sorting wheel rotating speed is 3300r/min, obtained particle mean size is (Sm, Tb, Fe)-H of 3.5 μm
xmagnetic, i.e. secondary alloy powder;
(7) step (3) gained master alloying powder and the secondary alloy powder of (6) gained are prepared burden according to mass ratio 100:3, add and be equivalent to master alloying powder quality 0.2%Dy
2o
3powder, then mixes 1.5h on batch mixer, the mixing magnetic of obtained granularity and uniform composition;
(8) by step (7) gained mixing magnetic in magnetic field intensity be 1.6T magnetic field in oriented moulding, then carry out isostatic pressed, stripping oil, the blank product with inner membrance be transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact (prepare sintering);
(9) pressed compact of step (8) is transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10
-2pa, calcined temperature 1175 DEG C, insulation 1h, sintering temperature is 1205 DEG C, insulation 1h, solid solubility temperature 1175 DEG C, insulation 1h, and solid solution terminates rear air-cooled to 70 DEG C;
(10) tempering: the product after step (9) being sintered carries out one-level timeliness and secondary time effect process, wherein one-level aging temp 800 DEG C, is incubated 20 hours, secondary time effect temperature 420 DEG C, is incubated 10 hours.
Embodiment 7
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, comprises master alloying and secondary alloy, and master alloying and secondary alloy mass ratio are 100: 5; Master alloying chemical formula is Sm
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%, secondary alloy is Sm by chemical formula
20%tb
60%fe
20%.
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, coordinates prior powder metallurgy technique to prepare samarium cobalt permanent magnet by two alloyage, prepares master alloying and secondary alloy, specifically comprise the following steps:
The preparation that step (1), (2), (3) are master alloying powder:
(1) by chemical formula Sm
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%mass percent batching;
(2) master alloying raw material step (1) prepared drops in vacuum induction melting furnace crucible, is evacuated to 3Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improves power and carries out melting to 60kw, and after alloy melts completely, insulation 10min, is then poured in water cooled copper mould by aluminium alloy, makes alloy cast ingot;
(3) first the alloy cast ingot of step (2) is become the particle of average grain diameter 0.1mm size by coarse crushing; Again the alloying pellet of coarse crushing is made the fine powder of average grain diameter 3.3 μm by rolling ball milling, winner's alloy powder;
The preparation that step (4), (5), (6) are secondary alloyed powder:
(4) chemical formula Sm pressed by secondary alloy
20%tb
60%fe
20%mass percent batching;
(5) secondary alloy raw material step (4) prepared drops into vacuum induction and gets rid of in band smelting furnace crucible, is evacuated to 3Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improve power carry out melting to 60kw, after alloy melts completely, be incubated 8min, be then poured into by aluminium alloy on water-cooled copper roller, the rotating speed of water-cooled copper roller is 3.5m/s, make average thickness be 0.35mm get rid of strap;
(6) secondary for step (5) gained alloy is got rid of the broken method of strap hydrogen to carry out hydrogen and break, make the meal that particle mean size is 150 μm, every kilogram of meal adds 3mL antioxidant cyclohexane and 5mL gasoline, then airflow milling is passed through, jet mill sorting wheel rotating speed is 3300r/min, obtained particle mean size is (Sm, Tb, Fe)-H of 3.5 μm
xmagnetic, i.e. secondary alloy powder;
(7) step (3) gained master alloying powder and the secondary alloy powder of (6) gained are prepared burden according to mass ratio 100:5, add and be equivalent to master alloying powder quality 0.3%Dy
2o
3powder, then mixes 1.5h on batch mixer, the mixing magnetic of obtained granularity and uniform composition;
(8) by step (7) gained mixing magnetic in magnetic field intensity be 1.6T magnetic field in oriented moulding, then carry out isostatic pressed, stripping oil, the blank product with inner membrance be transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact (prepare sintering);
(9) pressed compact of step (8) is transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10
-2pa, calcined temperature 1175 DEG C, insulation 1h, sintering temperature is 1205 DEG C, insulation 1h, solid solubility temperature 1175 DEG C, insulation 1h, and solid solution terminates rear air-cooled to 70 DEG C;
(10) tempering: the product after step (9) being sintered carries out one-level timeliness and secondary time effect process, wherein one-level aging temp 800 DEG C, is incubated 20 hours, secondary time effect temperature 420 DEG C, is incubated 10 hours.
Embodiment 8
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, comprises master alloying and secondary alloy, and master alloying and secondary alloy mass ratio are 100: 3; Master alloying chemical formula is Sm
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%, secondary alloy formula is Pr
20%dy
60%fe
20%.
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, coordinates prior powder metallurgy technique to prepare samarium cobalt permanent magnet by two alloyage, prepares master alloying and secondary alloy, specifically comprise the following steps:
The preparation that step (1), (2), (3) are master alloying powder:
(1) by chemical formula Sm
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%mass percent batching;
(2) master alloying raw material step (1) prepared drops in vacuum induction melting furnace crucible, is evacuated to 3Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improves power and carries out melting to 60kw, and after alloy melts completely, insulation 10min, is then poured in water cooled copper mould by aluminium alloy, makes alloy cast ingot;
(3) first the alloy cast ingot of step (2) is become the particle of average grain diameter 0.1mm size by coarse crushing; Again the alloying pellet of coarse crushing is made the fine powder of average grain diameter 3.3 μm by rolling ball milling, winner's alloy powder;
The preparation that step (4), (5), (6) are secondary alloyed powder:
(4) chemical formula Pr pressed by secondary alloy
20%dy
60%fe
20%mass percent batching;
(5) secondary alloy raw material step (4) prepared drops into vacuum induction and gets rid of in band smelting furnace crucible, is evacuated to 3Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improve power carry out melting to 60kw, after alloy melts completely, be incubated 8min, be then poured into by aluminium alloy on water-cooled copper roller, the rotating speed of water-cooled copper roller is 3.5m/s, make average thickness be 0.35mm get rid of strap;
(6) secondary for step (5) gained alloy is got rid of the broken method of strap hydrogen to carry out hydrogen and break, make the meal that particle mean size is 150 μm, every kilogram of meal adds 3mL antioxidant cyclohexane and 5mL gasoline, then airflow milling is passed through, jet mill sorting wheel rotating speed is 3300r/min, obtained particle mean size is (Pr, Dy, Fe)-H of 3.5 μm
xmagnetic, i.e. secondary alloy powder;
(7) step (3) gained master alloying powder and the secondary alloy powder of (6) gained are prepared burden according to mass ratio 100:3, add the Dy being equivalent to master alloying powder quality 0.2%
2o
3powder, then mixes 1.5h on batch mixer, the mixing magnetic of obtained granularity and uniform composition;
(8) by step (7) gained mixing magnetic in magnetic field intensity be 1.6T magnetic field in oriented moulding, then carry out isostatic pressed, stripping oil, the blank product with inner membrance be transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact (prepare sintering);
(9) pressed compact of step (8) is transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10
-2pa, calcined temperature 1175 DEG C, insulation 1h, sintering temperature is 1205 DEG C, insulation 1h, solid solubility temperature 1175 DEG C, insulation 1h, and solid solution terminates rear air-cooled to 70 DEG C;
(10) tempering: the product after step (9) being sintered carries out one-level timeliness and secondary time effect process, wherein one-level aging temp 800 DEG C, is incubated 20 hours, secondary time effect temperature 420 DEG C, is incubated 10 hours.
Embodiment 9
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, comprises master alloying and secondary alloy, and master alloying and secondary alloy mass ratio are 100: 3; Master alloying chemical formula is Sm
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%, secondary alloy is Nd by chemical formula
20%dy
60%fe
20%.
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, coordinates prior powder metallurgy technique to prepare samarium cobalt permanent magnet by two alloyage, prepares master alloying and secondary alloy, specifically comprise the following steps:
The preparation that step (1), (2), (3) are master alloying powder:
(1) by chemical formula Sm
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%mass percent batching;
(2) master alloying raw material step (1) prepared drops in vacuum induction melting furnace crucible, is evacuated to 3Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improves power and carries out melting to 60kw, and after alloy melts completely, insulation 10min, is then poured in water cooled copper mould by aluminium alloy, makes alloy cast ingot;
(3) first the alloy cast ingot of step (2) is become the particle of average grain diameter 0.1mm size by coarse crushing; Again the alloying pellet of coarse crushing is made the fine powder of average grain diameter 3.3 μm by rolling ball milling, winner's alloy powder;
The preparation that step (4), (5), (6) are secondary alloyed powder:
(4) chemical formula Nd pressed by secondary alloy
20%dy
60%fe
20%mass percent batching;
(5) secondary alloy raw material step (4) prepared drops into vacuum induction and gets rid of in band smelting furnace crucible, is evacuated to 3Pa, preheat temperature 650 DEG C, applying argon gas to 9.01 × 10
5pa, improve power carry out melting to 60kw, after alloy melts completely, be incubated 8min, be then poured into by aluminium alloy on water-cooled copper roller, the rotating speed of water-cooled copper roller is 3.5m/s, make average thickness be 0.35mm get rid of strap;
(6) secondary for step (5) gained alloy is got rid of the broken method of strap hydrogen to carry out hydrogen and break, make the meal that particle mean size is 150 μm, every kilogram of meal adds 3mL antioxidant cyclohexane and 5mL gasoline, then airflow milling is passed through, jet mill sorting wheel rotating speed is 3300r/min, obtained particle mean size is (Nd, Dy, Fe)-H of 3.5 μm
xmagnetic, i.e. secondary alloy powder;
(7) step (3) gained master alloying powder and the secondary alloy powder of (6) gained are prepared burden according to mass ratio 100:3, add and be equivalent to master alloying powder quality 0.2%Dy
2o
3powder, then mixes 1.5h on batch mixer, the mixing magnetic of obtained granularity and uniform composition;
(8) by step (7) gained mixing magnetic in magnetic field intensity be 1.6T magnetic field in oriented moulding, then carry out isostatic pressed, stripping oil, the blank product with inner membrance be transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact (prepare sintering);
(9) pressed compact of step (8) is transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10
-2pa, calcined temperature 1175 DEG C, insulation 1h, sintering temperature is 1205 DEG C, insulation 1h, solid solubility temperature 1175 DEG C, insulation 1h, and solid solution terminates rear air-cooled to 70 DEG C;
(10) tempering: the product after step (9) being sintered carries out one-level timeliness and secondary time effect process, wherein one-level aging temp 800 DEG C, is incubated 20 hours, secondary time effect temperature 420 DEG C, is incubated 10 hours.
Comparative example 1
The present embodiment only prepares master alloying, and master alloying chemical formula is Sm
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%, the concrete steps of its preparation method are:
(1) by chemical formula Sm
24.5%co
49.5%fe
16.2%cu
6.1%zr
3.7%mass percent batching;
(2) master alloying raw material step (1) prepared drops in vacuum induction melting furnace crucible, is evacuated to 5Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 10
5pa, improves power and carries out melting to 60kw, and after alloy melts completely, insulation 8min, is then poured in water cooled copper mould by aluminium alloy, makes alloy cast ingot;
(3) first the alloy cast ingot of step (2) is become the particle of average grain diameter 0.15mm size by coarse crushing; Again the alloying pellet of coarse crushing is made the fine powder of average grain diameter 3.5 μm by planetary ball mill;
(4) batch mixing: master alloying powder prepared by step (3) is mixed 1h on batch mixer, the mixed-powder of obtained granularity and uniform composition;
(5) shaping: to be oriented moulding in the magnetic field of 1.8T in magnetic field intensity by step (4) gained mixing magnetic, then carry out isostatic pressed, stripping oil, the blank product with inner membrance is transported in sintering furnace glove box and peels inner membrance off, obtain pressed compact (preparing sintering);
(6) step (5) gained pressed compact is transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10
-2pa, calcined temperature 1185 DEG C, insulation 1h, sintering temperature is 1200 DEG C, insulation 1.5h, solid solubility temperature 1185 DEG C, insulation 1h, and solid solution terminates rear air-cooled to 70 DEG C;
(7) tempering: the product after step (6) being sintered carries out one-level Ageing Treatment and secondary time effect process, wherein one-level aging temp 850 DEG C, is incubated 10 hours, secondary time effect temperature 400 DEG C, is incubated 10 hours.
Test the performance of embodiment 1-9 and comparative example 1 gained samarium cobalt permanent magnet body, examination criteria is according to " XB/T507-20092:17 type samarium-cobalt permanent-magnetic material ", and test result is in table 1.
Visible, by mixing the secondary alloy of different proportion, in samarium cobalt permanent magnet, introduce heavy rare earth Dy and Tb, and add a small amount of Dy
2o
3powder, not quite, coercive force improves 0.6-2.5KOe, and effect clearly for remanent magnetism and magnetic energy product change.And by the coercive force regulating the ratio of major-minor alloy to regulate gained permanent magnetic material, can meet the requirement of industrial application better.
Specific embodiment described in the invention is only to the present invention's explanation for example, is not construed as limiting the invention.The technical staff in field of the present invention can do described specific embodiment variously to supplement or improve, but allly supplements or improve the scope not departing from claims.
Claims (8)
1. a high-coercive force samarium-cobalt permanent-magnetic material, is characterized in that, comprises master alloying and secondary alloy, and master alloying and secondary alloy mass ratio are 100: 1-5; Master alloying chemical formula is Sm
xco
yfe
zcu
wzr
bal, x, y, z in formula, w, bal be the mass percent of respective element in expression respectively, 24%≤x≤27%, 45%≤y≤55%, 15%≤z≤20%, 4%≤w≤10%, wherein x+y+z+w+bal=100%; Secondary alloy formula is N
am
bfe
c, N represents one in light rare earth element Sm, Pr, Nd or complex element, and M is a kind of in heavy rare earth element Dy, Tb or complex element, in formula, a, b, c represent the mass percent of respective element, 20%≤a≤25%, 60%≤b≤65%, 15%≤c≤20%, wherein a+b+c=100%; Add the Dy being equivalent to master alloying powder quality 0.1-0.5% simultaneously
2o
3powder.
2. a preparation method for high-coercive force samarium-cobalt permanent-magnetic material as claimed in claim 1, is characterized in that, comprise the following steps:
The preparation that step (1), (2), (3) are master alloying powder:
(1) prepare burden: master alloying is Sm by chemical formula
xco
yfe
zcu
wzr
balmass percent batching, x, y, z in formula, w, bal be the mass percent of respective element in expression respectively, 24%≤x≤27%, 45%≤y≤55%, 15%≤z≤20%, 4%≤w≤10%, wherein x+y+z+w+bal=100%;
(2) melting: master alloying raw material step (1) prepared drops in vacuum induction melting furnace crucible, is evacuated to 3 ~ 6Pa, is preheated to 600-700 DEG C, applying argon gas to 9 × 10
5~ 9.01 × 10
5pa, improves power and carries out melting to 50-60kw, and after alloy melts completely, insulation 8 ~ 10min, is then poured in water cooled copper mould by aluminium alloy, makes alloy cast ingot;
(3) powder process: the particle first alloy cast ingot of step (2) being become 0.1-0.3mm size by coarse crushing; Again the alloying pellet of coarse crushing is made the fine powder of 3.0-5.0 micron by planetary ball mill or rolling ball milling, winner's alloy powder;
The preparation that step (4), (5), (6) are secondary alloyed powder:
(4) prepare burden: secondary alloy is N by chemical formula
am
bfe
c, N represents one in light rare earth element Sm, Pr, Nd or complex element, and M is a kind of in heavy rare earth element Dy, Tb or complex element, in formula, a, b, c represent the mass percent of respective element, 20%≤a≤25%, 60%≤b≤65%, 15%≤c≤20%, wherein a+b+c=100%;
(5) melting: secondary alloy raw material step (4) prepared drops into vacuum induction and gets rid of in band smelting furnace crucible, is evacuated to 3 ~ 6Pa, is preheated to 600-700 DEG C, applying argon gas to 9 × 10
5~ 9.01 × 10
5pa, improve power carry out melting to 50-60kw, after alloy melts completely, be incubated 8 ~ 10min, then aluminium alloy is poured on water-cooled copper roller, make average thickness be 0.2 ~ 0.5mm get rid of strap;
(6) powder process: secondary for step (5) gained alloy is got rid of the broken method of strap hydrogen and carry out hydrogen and break, make the meal that average grain diameter is 100 ~ 200 microns, 2 ~ 5mL antioxidant and 2 ~ 5mL gasoline is added by every kilogram of meal, then airflow milling is passed through, obtained particle mean size is the (N of 3 ~ 5 microns, M, Fe)-H
xrare earth hydride magnetic, i.e. secondary alloy powder;
(7) batch mixing: by step (3) gained master alloying powder and the secondary alloy powder batching of (6) gained, the mass ratio of master alloying powder and secondary alloy powder is 100:1-5, adds the Dy being equivalent to master alloying powder quality 0.1-0.5% simultaneously
2o
3powder, then mixes 0.5-1.5h on batch mixer, the mixing magnetic of obtained granularity and uniform composition;
(8) shaping: to be oriented moulding in the magnetic field of 1.5-2.0T in magnetic field intensity by step (7) gained mixing magnetic, then carry out isostatic pressed, stripping oil, the blank product with inner membrance is transported in sintering furnace glove box and peels inner membrance off, obtain pressed compact;
(9) sinter: step (8) gained pressed compact is transported to sintering furnace burner hearth high temperature sintering, suction to 2.5 × 10
-2-5 × 10
-2pa, calcined temperature 1175-1185 DEG C, insulation 0.5-1.5h; Sintering temperature is 1190-1210 DEG C, insulation 1-2h; Solid solubility temperature 1175-1185 DEG C, insulation 0.5-2h; Solid solution terminates rear air-cooled to 60 ~ 80 DEG C;
(10) tempering: the product after step (9) sintering is carried out one-level Ageing Treatment and secondary time effect process, wherein one-level aging temp 800 ~ 850 DEG C, is incubated 10 ~ 20 hours, secondary time effect temperature 400 ~ 450 DEG C, is incubated 10 ~ 15 hours.
3. the preparation method of high-coercive force samarium-cobalt permanent-magnetic material according to claim 2, is characterized in that, in step (5), during secondary alloy melting, the rotating speed of described water-cooled copper roller is 3 ~ 4m/s.
4. the preparation method of the high-coercive force samarium-cobalt permanent-magnetic material according to Claims 2 or 3, is characterized in that, in step (6), described jet mill sorting wheel rotating speed is 2500 ~ 3500r/min.
5. the preparation method of the high-coercive force samarium-cobalt permanent-magnetic material according to Claims 2 or 3, is characterized in that, in step (6), described antioxidant is at least one in benzinum, cyclohexane, dichlorodifluoromethan.
6. the preparation method of high-coercive force samarium-cobalt permanent-magnetic material according to claim 4, is characterized in that, in step (6), described antioxidant is at least one in benzinum, cyclohexane, dichlorodifluoromethan.
7. the preparation method of the high-coercive force samarium-cobalt permanent-magnetic material according to Claims 2 or 3, is characterized in that, in step (1), described raw material adopts the metal of purity >=99.9%.
8. the preparation method of the high-coercive force samarium-cobalt permanent-magnetic material according to Claims 2 or 3, is characterized in that, in step (4), described raw material adopts the metal of purity >=99.9%.
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| CN108899191A (en) * | 2018-06-30 | 2018-11-27 | 苏州诺弘添恒材料科技有限公司 | A kind of preparation method of the samarium cobalt permanent magnet body with ceramic layer |
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| CN109872855A (en) * | 2017-12-04 | 2019-06-11 | 中国科学院宁波材料技术与工程研究所 | A kind of high-coercive force rare earth cobalt-based permanent-magnet material and preparation method thereof |
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| CN108899191A (en) * | 2018-06-30 | 2018-11-27 | 苏州诺弘添恒材料科技有限公司 | A kind of preparation method of the samarium cobalt permanent magnet body with ceramic layer |
| CN109273241A (en) * | 2018-11-08 | 2019-01-25 | 浙江嘉兴南湖电子器材集团有限公司 | A kind of high mechanical strength permanent magnet sintering process |
| CN112712986A (en) * | 2019-12-24 | 2021-04-27 | 中国计量大学 | Low-temperature coefficient Sm2Co17Molded sintered magnet and method for producing same |
| CN112712986B (en) * | 2019-12-24 | 2022-04-15 | 中国计量大学 | Low-temperature coefficient Sm2Co17Molded sintered magnet and method for producing same |
| CN112103068A (en) * | 2020-08-28 | 2020-12-18 | 杭州永磁集团有限公司 | Preparation method of high-magnetic-performance 1:5 pure samarium cobalt permanent magnet |
| CN113744987A (en) * | 2021-08-25 | 2021-12-03 | 北京航空航天大学 | Method for preparing high-performance samarium-cobalt magnet through grain boundary structure reconstruction |
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