CN105374484B - 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
- Publication number
- CN105374484B CN105374484B CN201510916433.6A CN201510916433A CN105374484B CN 105374484 B CN105374484 B CN 105374484B CN 201510916433 A CN201510916433 A CN 201510916433A CN 105374484 B CN105374484 B CN 105374484B
- Authority
- CN
- China
- Prior art keywords
- powder
- alloy
- incubated
- preparation
- master alloying
- 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.)
- Active
Links
Landscapes
- Hard Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
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, more particularly to a kind of high-coercive force samarium cobalt permanent magnet material
Material and preparation method thereof.
Background technology
Sintered samarium cobalt permanent magnet material, because of its excellent magnetic property, particularly with higher coercivity and low-temperature coefficient,
Good resistance to elevated temperatures and corrosion resistance, in many fields, are particularly used widely in high temperature environments.Traditional
Sm2Co17The main component of type samarium-cobalt permanent-magnetic material is samarium, cobalt, ferrum, copper, zirconium, generally uses temperature less than 400-450 DEG C, if
Operation at high temperature is carried again, can bring drastically reducing for coercivity and magnetic energy product.It is warm in order to further improve using for samarium cobalt permanent magnet
Degree, needs further to improve the coercivity of samarium cobalt permanent magnet and reduces coercive force temperature coefficient.
In existing patent, such as the Chinese patent application of Application No. 201010176900.3,201110030314.2
Deng, add heavy rare earth element to improve coercivity using single alloyage, reduce temperature coefficient, but this method can not regulate and control coercive
Power.In ZL201210576210.6, by the second samarium-cobalt alloy ingot casting using the first samarium-cobalt alloy and containing heavy rare earth, slightly
Mixing and ball milling powder after broken；In the Chinese patent application of Application No. 201310196922.X, mentioning
There is the mixed-powder of the low-melting alloy powder of heavy rare earth.What both of the above was adopted is all that common melting casting ingot method prepares conjunction
Gold.
The Chinese patent application of Application No. 201410532244.4, is obtained SmCo powder, but this side using solwution method
Method complex process, industrialization are relatively costly.
The content of the invention
The technical problem to be solved is to overcome the deficiencies in the prior art, there is provided a kind of high-coercive force SmCo is forever
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, including master alloying and secondary alloy, master alloying and secondary alloy mass ratio
For 100: 1-5；Master alloying chemical formula is SmxCoyFezCuwZrbal, respective element in x, y, z, w, bal difference expression in formula
Mass percent, 24%≤x≤27%, 45%≤y≤55%, 15%≤z≤20%, 4%≤w≤10%, wherein x+y+z+w+bal=
100%；Secondary alloy formula is NaMbFec, N represents one kind or complex element in LREE Sm, Pr, Nd, and M is heavy rare earth
A kind of or complex element in element Dy, Tb, in formula, a, b, c represent the mass percent of respective element, 20%≤a≤25%, 60%≤
B≤65%, wherein 15%≤c≤20%, a+b+c=100%；The Dy equivalent to master alloying powder quality 0.1-0.5% is added simultaneously2O3
Powder.
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present invention, coordinates prior powder metallurgy work by dual alloy method
Skill prepares samarium cobalt permanent magnet, prepares master alloying and secondary alloy, specifically includes following steps：
Step（1）、（2）、（3）Based on alloyed powder preparation：
（1）Dispensing：Master alloying presses chemical formula for SmxCoyFezCuwZrbalMass percent dispensing, x, y, z in formula, w,
The mass percent of respective element, 24%≤x≤27%, 45%≤y≤55%, 15%≤z≤20%, 4%≤w in bal difference expressions
≤ 10%, wherein x+y+z+w+bal=100%；
Raw material is preferably using the metal of purity >=99.9%；
（2）Melting：By step（1）In the master alloying raw material input vacuum induction melting furnace crucible for preparing, 3 are evacuated to～
6Pa, is preheated to 600-700 DEG C, applying argon gas to 9 × 105～9.01 × 105Pa, improving power carries out melting to 50-60kw, waits to close
After gold is completely melt, 8～10min is incubated, then aluminium alloy is poured in water cooled copper mould, alloy cast ingot is made；
（3）Powder processed：First by step（2）Alloy cast ingot by coarse crushing into 0.1-0.3mm sizes granule；Slightly will break again
Broken alloying pellet makes the fine powder of 3.0-5.0 microns, winner's alloy powder by planetary ball mill or rolling ball milling；
Step（4）、（5）、（6）For the preparation of secondary alloyed powder：
（4）Dispensing：Secondary alloy presses chemical formula for NaMbFec, N represents the one kind in LREE Sm, Pr, Nd or mixing
Element, M are a kind of or complex element in heavy rare earth element Dy, Tb, and in formula, a, b, c represent the mass percent of respective element, 20%
≤ a≤25%, 60%≤b≤65%, wherein 15%≤c≤20%, a+b+c=100%；
Raw material is preferably using the metal of purity >=99.9%；
（5）Melting：By step（4）The secondary alloy raw material input vacuum induction for preparing is got rid of in band smelting furnace crucible, evacuation
To 3～6Pa, 600-700 DEG C is preheated to, applying argon gas to 9 × 105～9.01 × 105Pa, improves power and is melted to 50-60kw
Refining, after alloy is completely melt, is incubated 8～10min, then aluminium alloy is poured in water-cooled copper roller, and making average thickness is
0.2～0.5mm's gets rid of strap；
（6）Powder processed：By step（5）The secondary alloy of gained gets rid of the broken method of strap hydrogen to carry out hydrogen and breaks, make mean diameter for 100～
200 microns of coarse powder, adds 2～5mL antioxidants and 2～5mL gasoline by every kilogram of coarse powder, then by airflow milling, is obtained
Particle mean size is 3～5 microns (N, M, Fe)-HxRare earth hydride magnetic powder, i.e., secondary alloy powder；
At least one in the preferred petroleum ether of the antioxidant, cyclohexane, dichlorodifluoromethan；
（7）Batch mixing：By step（3）Gained master alloying powder and（6）The secondary alloy powder dispensing of gained, master alloying powder and pair
The mass ratio of alloy powder is 100:1-5, while adding the Dy equivalent to master alloying powder quality 0.1-0.5%2O3Powder, then
Mix 0.5-1.5h on batch mixer, granularity is obtained and composition uniformly mixes magnetic powder；
（8）Molding：By step（7）Gained mixing magnetic powder oriented moulding in magnetic field of the magnetic field intensity for 1.5-2.0T, so
After carry out isostatic pressed, stripping oil, the blank product with inner membrance is transported in sintering furnace glove box and peels inner membrance off, pressed compact is obtained（It is accurate
Standby sintering）；
（9）Sintering：By step（8）Gained pressed compact is transported to sintering furnace burner hearth high temperature sintering, suction to 2.5 × 10-2-5
×10-2Pa, 1175-1185 DEG C of calcined temperature are incubated 0.5-1.5h；Sintering temperature is 1190-1210 DEG C, is incubated 1-2h；Solid solution
Temperature 1175-1185 DEG C, is incubated 0.5-2h；Solid solution is air-cooled to 60～80 DEG C after terminating；
（10）Tempering：By Jing steps（9）Product after sintering carries out one-level Ageing Treatment and secondary time effect is processed, wherein one
800～850 DEG C of aging temp of level, is incubated 10～20 hours, and 400～450 DEG C of secondary time effect temperature is incubated 10～15 hours, i.e.,
Into.
Further, step（5）In, during secondary alloy melting, the rotating speed of the water-cooled copper roller is 3～4m/s.
Further, step（6）In, the jet mill sorting wheel rotating speed is 2500～3500r/min.
Compared with prior art, the present invention has advantages below：
1st, by the different ratio of two kinds of alloys of master alloying and secondary alloy, the heavy rare earth such as Dy or Tb unit is introduced from composition
Element, forms the Hard Magnetic outer shell of Dy containing heavy rare earth or Tb, enhances the local magnetocrystalline anisotropy of main phase grain boundary region, have
Playing the magnetic coupling interaction that goes between neighboring die for effect, improves coercivity.Rare earth hydride is added in batch mixing, due to hydrogenation
High activity after thing dehydrogenation, can reduce the oxidation of samarium-cobalt alloy, and rare earth hydride can dilute the content of heavy rare earth in crystal boundary, effectively
Raising coercivity, and realize the efficient utilization of Dy.Small amounts thing Dy2O3Addition can prevent sinter when crystal grain length
Greatly, the crystal grain of samarium-cobalt alloy is refined, is conducive to improving coercivity.
2nd, the major-minor alloy proportion of different proportion, can realize coercitive continuously adjustabe, prepare according to requirements difference
The samarium-cobalt alloy of composition, so as to meet different performance requirement.
Specific embodiment
With reference to embodiment, the invention will be further described.
In each embodiment, metal of the raw material selected by dispensing for purity 99.9%.
Embodiment 1
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, including master alloying and secondary alloy, master alloying and secondary alloy mass
Than for 100: 1；Master alloying chemical formula is Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%, it is Sm that secondary alloy presses chemical formula20%Dy60%
Fe20%。
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, coordinates prior powder metallurgy by dual alloy method
Technique prepares samarium cobalt permanent magnet, prepares master alloying and secondary alloy, specifically includes following steps：
Step（1）、（2）、（3）Based on alloyed powder preparation：
（1）Dispensing：Master alloying presses chemical formula Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%Mass percent dispensing；
（2）Melting：By step（1）In the master alloying raw material input vacuum induction melting furnace crucible for preparing, it is evacuated to
5Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 50kw, after alloy is completely melt,
Insulation 8min, is then poured into aluminium alloy in water cooled copper mould, makes alloy cast ingot；
（3）Powder processed：First by step（2）Alloy cast ingot by coarse crushing into particle diameter 0.15mm-0.25mm sizes granule；
The alloying pellet of coarse crushing is made 3.5-4.0 μm of fine powder, winner's alloy powder again by planetary ball mill or rolling ball milling；
Step（4）、（5）、（6）For the preparation of secondary alloyed powder：
（4）Dispensing：Secondary alloy presses chemical formula Sm20%Dy60%Fe20%Mass percent dispensing；
（5）Melting：By step（4）The secondary alloy raw material input vacuum induction for preparing is got rid of in band smelting furnace crucible, evacuation
To 3.5Pa, 650 DEG C are preheated to, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 50kw, treats that alloy is completely melt
Afterwards, 10min is incubated, then aluminium alloy is poured in water-cooled copper roller, the rotating speed of water-cooled copper roller is 3.5m/s, makes average thickness
Strap is got rid of for 0.35mm；
（6）Powder processed：By step（5）The secondary alloy of gained gets rid of the broken method of strap hydrogen to carry out hydrogen and breaks, and makes particle mean size for 180 μm
Coarse powder, every kilogram of coarse powder adds 3mL cyclohexanes and 5mL gasoline, and then by airflow milling, jet mill sorting wheel rotating speed is
3300r/min, prepared particle mean size are 3.3 μm (Sm, Dy, Fe)-HxMagnetic powder, i.e., secondary alloy powder；
（7）By step（3）Gained master alloying powder and（6）The secondary alloy powder of gained is according to mass ratio 100:1 dispensing, then
Mix 1h on batch mixer, granularity is obtained and composition uniformly mixes magnetic powder；
（8）Molding：By step（7）Gained mixing magnetic powder oriented moulding, Ran Houjin in magnetic field of the magnetic field intensity for 1.8T
Row isostatic pressed, stripping oil, the blank product with inner membrance are transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact（Prepare to burn
Knot）；
（9）Sintering：By step（8）Pressed compact be transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10-2Pa, in advance
1185 DEG C of temperature is burnt, 1h is incubated, sintering temperature is 1200 DEG C, be incubated 1.5h, 1185 DEG C of solid solubility temperature is incubated 1h, and solid solution terminates
It is air-cooled to 70 DEG C afterwards；
（10）Tempering：By Jing steps（9）When product after sintering carries out one-level timeliness and secondary time effect process, wherein one-level
850 DEG C of temperature of effect, is incubated 10 hours, and 400 DEG C of secondary time effect temperature is incubated 10 hours,.
Embodiment 2
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, including master alloying and secondary alloy, master alloying and secondary alloy mass
Than for 100: 1；Master alloying chemical formula is Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%, it is Sm that secondary alloy presses chemical formula20%Dy60%
Fe20%。
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, coordinates prior powder metallurgy by dual alloy method
Technique prepares samarium cobalt permanent magnet, prepares master alloying and secondary alloy, specifically includes following steps：
Step（1）、（2）、（3）Based on alloyed powder preparation：
（1）Dispensing：Master alloying presses chemical formula Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%Mass percent dispensing；
(2) by step（1）In the master alloying raw material input vacuum induction melting furnace crucible for preparing, 5Pa is evacuated to, is preheated
To 650 DEG C, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 60kw, after alloy is completely melt, is incubated 8min,
Then aluminium alloy is poured in water cooled copper mould, makes alloy cast ingot；
（3）First by step（2）Alloy cast ingot by coarse crushing into mean diameter 0.15mm size granule；Slightly will break again
Broken alloying pellet makes the fine powder of 3.5 μm of mean diameter, winner's alloy powder by planetary ball mill；
Step（4）、（5）、（6）For the preparation of secondary alloyed powder：
（4）Secondary alloy presses chemical formula Sm20%Dy60%Fe20%Mass percent dispensing；
（5）By step（4）The secondary alloy raw material vacuum induction for preparing is got rid of in band smelting furnace crucible, is evacuated to 3.5Pa, in advance
Hot to 650 DEG C, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 60kw, after alloy is completely melt, insulation
10min, is then poured into aluminium alloy in water-cooled copper roller, and the rotating speed of water-cooled copper roller is 3.5m/s, and making average thickness is
0.35mm's gets rid of strap；
（6）By step（5）The secondary alloy of gained gets rid of the broken method of strap hydrogen to carry out hydrogen and breaks, and it is 180 μm thick to make particle mean size
Powder, every kilogram of coarse powder add 3mL antioxidants cyclohexane and 5mL gasoline, and then by airflow milling, jet mill sorting wheel rotating speed is
3300r/min, prepared particle mean size are 3.3 μm (Sm, Dy, Fe)-HxMagnetic powder, i.e., secondary alloy powder；
（7）By step（3）Gained master alloying powder and（6）The secondary alloy powder dispensing of gained, master alloying powder and secondary alloy
Powder is according to 100:1 ratio dispensing, adds the Dy equivalent to master alloying quality 0.1%2O3Powder, then mixes on batch mixer
1h, is obtained granularity and composition uniformly mixes magnetic powder；
（8）By step（7）Gained mixing magnetic powder oriented moulding in magnetic field of the magnetic field intensity for 1.8T, is then carried out etc. quiet
Pressure, stripping oil, the blank product with inner membrance are transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact（Prepare sintering）；
（9）By step（8）Pressed compact be transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10-2Pa, pre-burning temperature
1185 DEG C of degree, is incubated 1h, and sintering temperature is 1200 DEG C, is incubated 1.5h, and 1185 DEG C of solid solubility temperature is incubated 1h, and solid solution terminates rear wind
It is cooled to 70 DEG C；
（10）Tempering：By step（9）Product after sintering carries out one-level timeliness and secondary time effect is processed, wherein one-level timeliness
850 DEG C of temperature, is incubated 10 hours, and 400 DEG C of secondary time effect temperature is incubated 10 hours,.
Embodiment 3
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, including master alloying and secondary alloy, master alloying and secondary alloy mass
Than for 100: 3；Master alloying chemical formula is Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%, it is Sm that secondary alloy presses chemical formula20%Dy60%
Fe20%。
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, coordinates prior powder metallurgy by dual alloy method
Technique prepares samarium cobalt permanent magnet, prepares master alloying and secondary alloy, specifically includes following steps：
Step（1）、（2）、（3）Based on alloyed powder preparation：
（1）Master alloying presses chemical formula Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%Mass percent dispensing；
(2) by step（1）In the master alloying raw material input vacuum induction melting furnace crucible for preparing, 5Pa is evacuated to, is preheated
To 650 DEG C, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 60kw, after alloy is completely melt, is incubated 8min,
Then aluminium alloy is poured in water cooled copper mould, makes on copper roller, make alloy cast ingot；
（3）First by step（2）Alloy cast ingot by coarse crushing into mean diameter 0.15mm size granule；Slightly will break again
Broken alloying pellet makes the fine powder of 3.5 μm of mean diameter, winner's alloy powder by rolling ball milling；
Step（4）、（5）、（6）For the preparation of secondary alloyed powder：
（4）Secondary alloy presses chemical formula Sm20%Dy60%Fe20%Mass percent dispensing；
（5）By step（4）The secondary alloy raw material input vacuum induction for preparing is got rid of in band smelting furnace crucible, is evacuated to
3.5Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 105Pa, improving power carries out melting, after alloy is completely melt, insulation
10min, is then poured into aluminium alloy in water-cooled copper roller, and the rotating speed of water-cooled copper roller is 3.5m/s, and making average thickness is
0.35mm's gets rid of strap；
（6）By step（5）The secondary alloy of gained gets rid of the broken method of strap hydrogen to carry out hydrogen and breaks, and it is 180 μm thick to make particle mean size
Powder, every kilogram of coarse powder add 3mL antioxidants cyclohexane and 5mL gasoline, and then by airflow milling, jet mill sorting wheel rotating speed is
3300r/min, prepared particle mean size are 3.3 μm (Sm, Dy, Fe)-HxMagnetic powder, i.e., secondary alloy powder；
（7）By step（3）Gained master alloying powder and（6）The secondary alloy powder dispensing of gained, master alloying powder and secondary alloy
Powder is according to mass ratio 100:3 dispensings, add equivalent to 0.2% Dy of master alloying quality2O3Powder, then mixes on batch mixer
1h, is obtained granularity and composition uniformly mixes magnetic powder；
（8）By step（7）Gained mixing magnetic powder oriented moulding in magnetic field of the magnetic field intensity for 1.8T, is then carried out etc. quiet
Pressure, stripping oil, the blank product with inner membrance are transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact（Prepare sintering）；
（9）By step（8）Pressed compact be transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10-2Pa, pre-burning temperature
1185 DEG C of degree, is incubated 1h, and sintering temperature is 1200 DEG C, is incubated 1.5h, and 1185 DEG C of solid solubility temperature is incubated 1h, and solid solution terminates rear wind
It is cooled to 70 DEG C；
（10）Tempering：By Jing steps（9）When product after sintering carries out one-level timeliness and secondary time effect process, wherein one-level
850 DEG C of temperature of effect, is incubated 10 hours, and 400 DEG C of secondary time effect temperature is incubated 10 hours,.
Embodiment 4
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, including master alloying and secondary alloy, master alloying and secondary alloy mass
Than for 100: 5；Master alloying chemical formula is Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%, secondary alloy formula is Sm20%Dy60%Fe20%。
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, coordinates prior powder metallurgy by dual alloy method
Technique prepares samarium cobalt permanent magnet, prepares master alloying and secondary alloy, specifically includes following steps：
Step（1）、（2）、（3）Based on alloyed powder preparation：
（1）Master alloying presses chemical formula Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%Mass percent dispensing；
(2) by step（1）In the master alloying raw material input vacuum induction melting furnace crucible for preparing, 5Pa is evacuated to, is preheated
To 650 DEG C, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 60kw, after alloy is completely melt, is incubated 8min,
Then aluminium alloy is poured in water cooled copper mould, makes alloy cast ingot；
（3）First by step（2）Alloy cast ingot by coarse crushing into mean diameter 0.15mm size granule；Slightly will break again
Broken alloying pellet makes the fine powder that mean diameter is 3.5 μm, winner's alloy powder by rolling ball milling；
Step（4）、（5）、（6）For the preparation of secondary alloyed powder：
（4）Secondary alloy presses chemical formula Sm20%Dy60%Fe20%Mass percent dispensing；
（5）By step（4）The secondary alloy raw material input vacuum induction for preparing is got rid of in band smelting furnace crucible, is evacuated to
3.5Pa, is preheated to 650 DEG C, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 60kw, treats that alloy is completely melt
Afterwards, 10min is incubated, then aluminium alloy is poured in water-cooled copper roller, the rotating speed of water-cooled copper roller is 3.5m/s, makes average thickness
Strap is got rid of for 0.35mm；
（6）By step（5）The secondary alloy of gained gets rid of the broken method of strap hydrogen to carry out hydrogen and breaks, and it is 180 μm thick to make particle mean size
Powder, every kilogram of coarse powder add 3mL antioxidants cyclohexane and 5mL gasoline, and then by airflow milling, jet mill sorting wheel rotating speed is
3300r/min, prepared particle mean size are 3.3 μm (Sm, Dy, Fe)-HxMagnetic powder, i.e., secondary alloy powder；
（7）By step（3）Gained master alloying powder and（6）The secondary alloy powder of gained is according to 100:5 mass are added than dispensing
Equivalent to 0.3% Dy of master alloying powder quality2O3Powder, then mixes 1h on batch mixer, granularity is obtained and composition is uniformly mixed
Close magnetic powder；
（8）By step（7）Gained mixing magnetic powder oriented moulding in magnetic field of the magnetic field intensity for 1.8T, is then carried out etc. quiet
Pressure, stripping oil, the blank product with inner membrance are transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact（Prepare sintering）；
（9）By step（8）Pressed compact be transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10-2Pa, pre-burning temperature
1185 DEG C of degree, is incubated 1h, and sintering temperature is 1200 DEG C, is incubated 1.5h, and 1185 DEG C of solid solubility temperature is incubated 1h, and solid solution terminates rear wind
It is cooled to 70 DEG C；
（10）Tempering：By step（9）Product after sintering carries out one-level timeliness and secondary time effect is processed, wherein one-level timeliness
850 DEG C of temperature, is incubated 10 hours, and 400 DEG C of secondary time effect temperature is incubated 10 hours,.
Embodiment 5
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, including master alloying and secondary alloy, master alloying and secondary alloy mass
Than for 100: 1；Master alloying chemical formula is Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%, it is Sm that secondary alloy presses chemical formula20%Tb60%
Fe20%。
Its preparation method is concretely comprised the following steps：
Step（1）、（2）、（3）Based on alloyed powder preparation：
（1）Master alloying presses chemical formula Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%Mass percent dispensing；
(2) by step（1）In the master alloying raw material input vacuum induction melting furnace crucible for preparing, 3Pa is evacuated to, is preheated
To 650 DEG C, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 60kw, after alloy is completely melt, insulation
10min, is then poured into aluminium alloy in water cooled copper mould, makes alloy cast ingot；
（3）First by step（2）Alloy cast ingot by coarse crushing into mean diameter 0.1mm size granule；Slightly will break again
Broken alloying pellet makes the fine powder of 3.3 μm of mean diameter by planetary ball mill；
Step（4）、（5）、（6）For the preparation of secondary alloyed powder：
（4）By chemical formula Sm20%Tb60%Fe20%Mass percent dispensing；
（5）By step（4）The secondary alloy raw material input vacuum induction for preparing is got rid of in band smelting furnace crucible, is evacuated to 3Pa,
650 DEG C are preheated to, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 60kw, after alloy is completely melt, insulation 8
Min, is then poured into aluminium alloy in water-cooled copper roller, and the rotating speed of water-cooled copper roller is 3.5m/s, makes average thickness for 0.35mm
Get rid of strap；
（6）By step（5）The secondary alloy of gained gets rid of the broken method of strap hydrogen to carry out hydrogen and breaks, and it is 150 μm thick to make particle mean size
Powder, every kilogram of coarse powder add 3mL antioxidants cyclohexane and 5mL gasoline, and then by airflow milling, jet mill sorting wheel rotating speed is
3300r/min, prepared particle mean size are 3.5 μm (Sm, Tb, Fe)-HxMagnetic powder, i.e., secondary alloy powder；
（7）By step（3）Gained master alloying powder and（6）The secondary alloy powder of gained is according to mass ratio 100:1 ratio dispensing,
Add the Dy equivalent to master alloying powder quality 0.1%2O3Powder, then on batch mixer mixes 1.5h, granularity and composition is obtained
Uniform mixing magnetic powder；
（8）By step（7）Gained mixing magnetic powder oriented moulding in magnetic field of the magnetic field intensity for 1.6T, is then carried out etc. quiet
Pressure, stripping oil, the blank product with inner membrance are transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact（Prepare sintering）；
（9）By step（8）Pressed compact be transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10-2Pa, pre-burning temperature
1175 DEG C of degree, is incubated 1h, and sintering temperature is 1205 DEG C, is incubated 1h, and 1175 DEG C of solid solubility temperature is incubated 1h, and solid solution is air-cooled after terminating
To 70 DEG C；
（10）Tempering：By step（9）Product after sintering carries out one-level timeliness and secondary time effect is processed, wherein one-level timeliness
800 DEG C of temperature, is incubated 20 hours, and 420 DEG C of secondary time effect temperature is incubated 10 hours,.
Embodiment 6
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, including master alloying and secondary alloy, master alloying and secondary alloy mass
Than for 100: 3；Master alloying chemical formula is Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%, secondary alloy formula is Sm20%Tb60%Fe20%。
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, coordinates prior powder metallurgy by dual alloy method
Technique prepares samarium cobalt permanent magnet, prepares master alloying and secondary alloy, specifically includes following steps：
Step（1）、（2）、（3）Based on alloyed powder preparation：
（1）Master alloying presses chemical formula Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%Mass percent dispensing；
(2) by step（1）In the master alloying raw material input vacuum induction melting furnace crucible for preparing, 3Pa is evacuated to, is preheated
To 650 DEG C, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 60kw, after alloy is completely melt, insulation
10min, is then poured into aluminium alloy in water cooled copper mould, makes alloy cast ingot；
（3）First by step（2）Alloy cast ingot by coarse crushing into mean diameter 0.1mm size granule；Slightly will break again
Broken alloying pellet makes the fine powder of 3.3 μm of mean diameter by planetary ball mill；
Step（4）、（5）、（6）For the preparation of secondary alloyed powder：
（4）Secondary alloy presses chemical formula Sm20%Tb60%Fe20%Mass percent dispensing；
（5）By step（4）The secondary alloy raw material input vacuum induction for preparing is got rid of in band smelting furnace crucible, is evacuated to 3Pa,
650 DEG C are preheated to, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 60kw, after alloy is completely melt, insulation 8
Min, is then poured into aluminium alloy in water-cooled copper roller, and the rotating speed of water-cooled copper roller is 3.5m/s, makes average thickness for 0.35mm
Get rid of strap；
（6）By step（5）The secondary alloy of gained gets rid of the broken method of strap hydrogen to carry out hydrogen and breaks, and it is 150 μm thick to make particle mean size
Powder, every kilogram of coarse powder add 3mL antioxidants cyclohexane and 5mL gasoline, and then by airflow milling, jet mill sorting wheel rotating speed is
3300r/min, prepared particle mean size are 3.5 μm (Sm, Tb, Fe)-HxMagnetic powder, i.e., secondary alloy powder；
（7）By step（3）Gained master alloying powder and（6）The secondary alloy powder of gained is according to mass ratio 100:3 dispensings, add
Equivalent to 0.2% Dy of master alloying powder quality2O3Powder, then mixes 1.5h on batch mixer, granularity is obtained and composition is uniform
Mixing magnetic powder；
（8）By step（7）Gained mixing magnetic powder oriented moulding in magnetic field of the magnetic field intensity for 1.6T, is then carried out etc. quiet
Pressure, stripping oil, the blank product with inner membrance are transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact（Prepare sintering）；
（9）By step（8）Pressed compact be transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10-2Pa, pre-burning temperature
1175 DEG C of degree, is incubated 1h, and sintering temperature is 1205 DEG C, is incubated 1h, and 1175 DEG C of solid solubility temperature is incubated 1h, and solid solution is air-cooled after terminating
To 70 DEG C；
（10）Tempering：By step（9）Product after sintering carries out one-level timeliness and secondary time effect is processed, wherein one-level timeliness
800 DEG C of temperature, is incubated 20 hours, and 420 DEG C of secondary time effect temperature is incubated 10 hours,.
Embodiment 7
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, including master alloying and secondary alloy, master alloying and secondary alloy mass
Than for 100: 5；Master alloying chemical formula is Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%, it is Sm that secondary alloy presses chemical formula20%Tb60%
Fe20%。
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, coordinates prior powder metallurgy by dual alloy method
Technique prepares samarium cobalt permanent magnet, prepares master alloying and secondary alloy, specifically includes following steps：
Step（1）、（2）、（3）Based on alloyed powder preparation：
（1）By chemical formula Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%Mass percent dispensing；
(2) by step（1）In the master alloying raw material input vacuum induction melting furnace crucible for preparing, 3Pa is evacuated to, is preheated
To 650 DEG C, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 60kw, after alloy is completely melt, insulation
10min, is then poured into aluminium alloy in water cooled copper mould, makes alloy cast ingot；
（3）First by step（2）Alloy cast ingot by coarse crushing into mean diameter 0.1mm size granule；Slightly will break again
Broken alloying pellet makes the fine powder of 3.3 μm of mean diameter, winner's alloy powder by rolling ball milling；
Step（4）、（5）、（6）For the preparation of secondary alloyed powder：
（4）Secondary alloy presses chemical formula Sm20%Tb60%Fe20%Mass percent dispensing；
（5）By step（4）The secondary alloy raw material input vacuum induction for preparing is got rid of in band smelting furnace crucible, is evacuated to 3Pa,
650 DEG C are preheated to, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 60kw, after alloy is completely melt, insulation 8
Min, is then poured into aluminium alloy in water-cooled copper roller, and the rotating speed of water-cooled copper roller is 3.5m/s, makes average thickness for 0.35mm
Get rid of strap；
（6）By step（5）The secondary alloy of gained gets rid of the broken method of strap hydrogen to carry out hydrogen and breaks, and it is 150 μm thick to make particle mean size
Powder, every kilogram of coarse powder add 3mL antioxidants cyclohexane and 5mL gasoline, and then by airflow milling, jet mill sorting wheel rotating speed is
3300r/min, prepared particle mean size are 3.5 μm (Sm, Tb, Fe)-HxMagnetic powder, i.e., secondary alloy powder；
（7）By step（3）Gained master alloying powder and（6）The secondary alloy powder of gained is according to mass ratio 100:5 dispensings, add
Equivalent to 0.3% Dy of master alloying powder quality2O3Powder, then mixes 1.5h on batch mixer, granularity is obtained and composition is uniform
Mixing magnetic powder；
（8）By step（7）Gained mixing magnetic powder oriented moulding in magnetic field of the magnetic field intensity for 1.6T, is then carried out etc. quiet
Pressure, stripping oil, the blank product with inner membrance are transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact（Prepare sintering）；
（9）By step（8）Pressed compact be transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10-2Pa, pre-burning temperature
1175 DEG C of degree, is incubated 1h, and sintering temperature is 1205 DEG C, is incubated 1h, and 1175 DEG C of solid solubility temperature is incubated 1h, and solid solution is air-cooled after terminating
To 70 DEG C；
（10）Tempering：By step（9）Product after sintering carries out one-level timeliness and secondary time effect is processed, wherein one-level timeliness
800 DEG C of temperature, is incubated 20 hours, and 420 DEG C of secondary time effect temperature is incubated 10 hours,.
Embodiment 8
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, including master alloying and secondary alloy, master alloying and secondary alloy mass
Than for 100: 3；Master alloying chemical formula is Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%, secondary alloy formula is Pr20%Dy60%Fe20%。
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, coordinates prior powder metallurgy by dual alloy method
Technique prepares samarium cobalt permanent magnet, prepares master alloying and secondary alloy, specifically includes following steps：
Step（1）、（2）、（3）Based on alloyed powder preparation：
（1）By chemical formula Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%Mass percent dispensing；
(2) by step（1）In the master alloying raw material input vacuum induction melting furnace crucible for preparing, 3Pa is evacuated to, is preheated
To 650 DEG C, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 60kw, after alloy is completely melt, insulation
10min, is then poured into aluminium alloy in water cooled copper mould, makes alloy cast ingot；
（3）First by step（2）Alloy cast ingot by coarse crushing into mean diameter 0.1mm size granule；Slightly will break again
Broken alloying pellet makes the fine powder of 3.3 μm of mean diameter, winner's alloy powder by rolling ball milling；
Step（4）、（5）、（6）For the preparation of secondary alloyed powder：
（4）Secondary alloy presses chemical formula Pr20%Dy60%Fe20%Mass percent dispensing；
（5）By step（4）The secondary alloy raw material input vacuum induction for preparing is got rid of in band smelting furnace crucible, is evacuated to 3Pa,
650 DEG C are preheated to, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 60kw, after alloy is completely melt, insulation 8
Min, is then poured into aluminium alloy in water-cooled copper roller, and the rotating speed of water-cooled copper roller is 3.5m/s, makes average thickness for 0.35mm
Get rid of strap；
（6）By step（5）The secondary alloy of gained gets rid of the broken method of strap hydrogen to carry out hydrogen and breaks, and it is 150 μm thick to make particle mean size
Powder, every kilogram of coarse powder add 3mL antioxidants cyclohexane and 5mL gasoline, and then by airflow milling, jet mill sorting wheel rotating speed is
3300r/min, prepared particle mean size are 3.5 μm (Pr, Dy, Fe)-HxMagnetic powder, i.e., secondary alloy powder；
（7）By step（3）Gained master alloying powder and（6）The secondary alloy powder of gained is according to mass ratio 100:3 dispensings, add
Equivalent to the Dy of master alloying powder quality 0.2%2O3Powder, then mixes 1.5h on batch mixer, granularity is obtained and composition is uniform
Mixing magnetic powder；
（8）By step（7）Gained mixing magnetic powder oriented moulding in magnetic field of the magnetic field intensity for 1.6T, is then carried out etc. quiet
Pressure, stripping oil, the blank product with inner membrance are transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact（Prepare sintering）；
（9）By step（8）Pressed compact be transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10-2Pa, pre-burning temperature
1175 DEG C of degree, is incubated 1h, and sintering temperature is 1205 DEG C, is incubated 1h, and 1175 DEG C of solid solubility temperature is incubated 1h, and solid solution is air-cooled after terminating
To 70 DEG C；
（10）Tempering：By step（9）Product after sintering carries out one-level timeliness and secondary time effect is processed, wherein one-level timeliness
800 DEG C of temperature, is incubated 20 hours, and 420 DEG C of secondary time effect temperature is incubated 10 hours,.
Embodiment 9
The high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, including master alloying and secondary alloy, master alloying and secondary alloy mass
Than for 100: 3；Master alloying chemical formula is Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%, it is Nd that secondary alloy presses chemical formula20%Dy60%
Fe20%。
The preparation method of the high-coercive force samarium-cobalt permanent-magnetic material of the present embodiment, coordinates prior powder metallurgy by dual alloy method
Technique prepares samarium cobalt permanent magnet, prepares master alloying and secondary alloy, specifically includes following steps：
Step（1）、（2）、（3）Based on alloyed powder preparation：
（1）By chemical formula Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%Mass percent dispensing；
(2) by step（1）In the master alloying raw material input vacuum induction melting furnace crucible for preparing, 3Pa is evacuated to, is preheated
To 650 DEG C, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 60kw, after alloy is completely melt, insulation
10min, is then poured into aluminium alloy in water cooled copper mould, makes alloy cast ingot；
（3）First by step（2）Alloy cast ingot by coarse crushing into mean diameter 0.1mm size granule；Slightly will break again
Broken alloying pellet makes the fine powder of 3.3 μm of mean diameter, winner's alloy powder by rolling ball milling；
Step（4）、（5）、（6）For the preparation of secondary alloyed powder：
（4）Secondary alloy presses chemical formula Nd20%Dy60%Fe20%Mass percent dispensing；
（5）By step（4）The secondary alloy raw material input vacuum induction for preparing is got rid of in band smelting furnace crucible, is evacuated to 3Pa,
650 DEG C of preheating temperature, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 60kw, after alloy is completely melt, protects
8 min of temperature, are then poured into aluminium alloy in water-cooled copper roller, and the rotating speed of water-cooled copper roller is 3.5m/s, and making average thickness is
0.35mm's gets rid of strap；
（6）By step（5）The secondary alloy of gained gets rid of the broken method of strap hydrogen to carry out hydrogen and breaks, and it is 150 μm thick to make particle mean size
Powder, every kilogram of coarse powder add 3mL antioxidants cyclohexane and 5mL gasoline, and then by airflow milling, jet mill sorting wheel rotating speed is
3300r/min, prepared particle mean size are 3.5 μm (Nd, Dy, Fe)-HxMagnetic powder, i.e., secondary alloy powder；
（7）By step（3）Gained master alloying powder and（6）The secondary alloy powder of gained is according to mass ratio 100:3 dispensings, add
Equivalent to 0.2% Dy of master alloying powder quality2O3Powder, then mixes 1.5h on batch mixer, granularity is obtained and composition is uniform
Mixing magnetic powder；
（8）By step（7）Gained mixing magnetic powder oriented moulding in magnetic field of the magnetic field intensity for 1.6T, is then carried out etc. quiet
Pressure, stripping oil, the blank product with inner membrance are transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact（Prepare sintering）；
（9）By step（8）Pressed compact be transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10-2Pa, pre-burning temperature
1175 DEG C of degree, is incubated 1h, and sintering temperature is 1205 DEG C, is incubated 1h, and 1175 DEG C of solid solubility temperature is incubated 1h, and solid solution is air-cooled after terminating
To 70 DEG C；
（10）Tempering：By step（9）Product after sintering carries out one-level timeliness and secondary time effect is processed, wherein one-level timeliness
800 DEG C of temperature, is incubated 20 hours, and 420 DEG C of secondary time effect temperature is incubated 10 hours,.
Comparative example 1
The present embodiment only prepares master alloying, and master alloying chemical formula is Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%, its preparation side
Method is concretely comprised the following steps：
（1）By chemical formula Sm24.5%Co49.5%Fe16.2%Cu6.1%Zr3.7%Mass percent dispensing；
(2) by step（1）In the master alloying raw material input vacuum induction melting furnace crucible for preparing, 5Pa is evacuated to, is preheated
To 650 DEG C, applying argon gas to 9.01 × 105Pa, improving power carries out melting to 60kw, after alloy is completely melt, is incubated 8min,
Then aluminium alloy is poured in water cooled copper mould, makes alloy cast ingot；
（3）First by step（2）Alloy cast ingot by coarse crushing into mean diameter 0.15mm size granule；Slightly will break again
Broken alloying pellet makes the fine powder of 3.5 μm of mean diameter by planetary ball mill；
（4）Batch mixing：By step（3）The master alloying powder of preparation mixes 1h on batch mixer, granularity is obtained and composition is uniform
Mixed-powder；
（5）Molding：By step（4）Gained mixing magnetic powder oriented moulding, Ran Houjin in magnetic field of the magnetic field intensity for 1.8T
Row isostatic pressed, stripping oil, the blank product with inner membrance are transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact（Prepare to burn
Knot）；
（6）By step（5）Gained pressed compact is transported to sintering furnace burner hearth high temperature sintering, suction to 3.5 × 10-2Pa, pre-burning
1185 DEG C of temperature, is incubated 1h, and sintering temperature is 1200 DEG C, is incubated 1.5h, and 1185 DEG C of solid solubility temperature is incubated 1h, after solid solution terminates
It is air-cooled to 70 DEG C；
（7）Tempering：By step（6）Product after sintering carries out one-level Ageing Treatment and secondary time effect is processed, wherein one-level
850 DEG C of aging temp, is incubated 10 hours, and 400 DEG C of secondary time effect temperature is incubated 10 hours,.
The performance of 1 gained samarium cobalt permanent magnet body of embodiment 1-9 and comparative example is tested, examination criteria according to《XB/T
507-2009 2:17 type samarium-cobalt permanent-magnetic materials》, test result is shown in Table 1.
It can be seen that, by the secondary alloy for mixing different proportion, heavy rare earth Dy and Tb are introduced in samarium cobalt permanent magnet, and is added few
The Dy of amount2O3Less, coercivity improves 0.6-2.5KOe, and effect is clearly for powder, remanent magnetism and magnetic energy product change.And can be with
Obtained by being adjusted as the ratio of regulation major-minor alloy, the coercivity of permanent magnet material, can conform better to the requirement of industrial application.
Specific embodiment described in the invention is only, to explanation for example of the invention, not constitute the limit to the present invention
System.The technical staff in field of the present invention can make various supplements or improvement, but all benefits to described specific embodiment
Fill or improve all without departing from scope of the following claims.
Claims (8)
1. a kind of high-coercive force samarium-cobalt permanent-magnetic material, it is characterised in that including master alloying and secondary alloy, master alloying and secondary alloy matter
Amount is than being 100: 1-5；Master alloying chemical formula is SmxCoyFezCuwZrbal, it is corresponding in x, y, z, w, bal difference expression in formula
The mass percent of element, 24%≤x≤27%, 45%≤y≤55%, 15%≤z≤20%, wherein 4%≤w≤10%, x+y+z+w+
bal=100%；Secondary alloy formula is NaMbFec, N represents one kind or complex element in LREE Sm, Pr, Nd, and M attaches most importance to
A kind of or complex element in rare earth element Dy, Tb, in formula, a, b, c represent the mass percent of respective element, 20%≤a≤25%,
60%≤b≤65%, wherein 15%≤c≤20%, a+b+c=100%；Add equivalent to master alloying powder quality 0.1-0.5% simultaneously
Dy2O3Powder.
2. a kind of preparation method of high-coercive force samarium-cobalt permanent-magnetic material as claimed in claim 1, it is characterised in that including following
Step：
Step（1）、（2）、（3）Based on alloyed powder preparation：
（1）Dispensing：Master alloying presses chemical formula for SmxCoyFezCuwZrbalMass percent dispensing, x, y, z in formula, w, bal point
The mass percent of respective element in other expression, 24%≤x≤27%, 45%≤y≤55%, 15%≤z≤20%, 4%≤w≤
10%, wherein x+y+z+w+bal=100%；
（2）Melting：By step（1）In the master alloying raw material input vacuum induction melting furnace crucible for preparing, 3～6Pa is evacuated to,
600-700 DEG C is preheated to, applying argon gas to 9 × 105～9.01 × 105Pa, improving power carries out melting to 50-60kw, treats that alloy is complete
After running down, 8～10min is incubated, then aluminium alloy is poured in water cooled copper mould, alloy cast ingot is made；
（3）Powder processed：First by step（2）Alloy cast ingot by coarse crushing into 0.1-0.3mm sizes granule；Again by coarse crushing
Alloying pellet makes the fine powder of 3.0-5.0 microns, winner's alloy powder by planetary ball mill or rolling ball milling；
Step（4）、（5）、（6）For the preparation of secondary alloyed powder：
（4）Dispensing：Secondary alloy presses chemical formula for NaMbFec, N represents one kind or complex element in LREE Sm, Pr, Nd,
M is a kind of or complex element in heavy rare earth element Dy, Tb, and 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：By step（4）The secondary alloy raw material input vacuum induction for preparing is got rid of in band smelting furnace crucible, it is evacuated to 3～
6Pa, is preheated to 600-700 DEG C, applying argon gas to 9 × 105～9.01 × 105Pa, improving power carries out melting to 50-60kw, waits to close
After gold is completely melt, is incubated 8～10min, then aluminium alloy be poured in water-cooled copper roller, make average thickness for 0.2～
0.5mm's gets rid of strap；
（6）Powder processed：By step（5）The secondary alloy of gained gets rid of the broken method of strap hydrogen to carry out hydrogen and breaks, and makes mean diameter for 100～200
The coarse powder of micron, adds 2～5mL antioxidants and 2～5mL gasoline by every kilogram of coarse powder, then by airflow milling, is obtained average
Granularity is 3～5 microns (N, M, Fe)-HxRare earth hydride magnetic powder, i.e., secondary alloy powder；
（7）Batch mixing：By step（3）Gained master alloying powder and（6）The secondary alloy powder dispensing of gained, master alloying powder and secondary alloy
The mass ratio of powder is 100:1-5, while adding the Dy equivalent to master alloying powder quality 0.1-0.5%2O3Powder, then mixed
Mix 0.5-1.5h on material machine, granularity is obtained and composition uniformly mixes magnetic powder；
（8）Molding：By step（7）Gained mixing magnetic powder oriented moulding, Ran Houjin in magnetic field of the magnetic field intensity for 1.5-2.0T
Row isostatic pressed, stripping oil, the blank product with inner membrance are transported in sintering furnace glove box and peel inner membrance off, obtain pressed compact；
（9）Sintering：By step（8）Gained pressed compact is transported to sintering furnace burner hearth high temperature sintering, suction to 2.5 × 10-2-5×10- 2Pa, 1175-1185 DEG C of calcined temperature are incubated 0.5-1.5h；Sintering temperature is 1190-1210 DEG C, is incubated 1-2h；Solid solubility temperature
1175-1185 DEG C, it is incubated 0.5-2h；Solid solution is air-cooled to 60～80 DEG C after terminating；
（10）Tempering：By Jing steps（9）When product after sintering carries out one-level Ageing Treatment and secondary time effect process, wherein one-level
800～850 DEG C of temperature of effect, is incubated 10～20 hours, and 400～450 DEG C of secondary time effect temperature is incubated 10～15 hours,.
3. the preparation method of high-coercive force samarium-cobalt permanent-magnetic material according to claim 2, it is characterised in that step（5）In,
During secondary alloy melting, the rotating speed of the 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, it is characterised in that step（6）
In, the 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, it is characterised in that step（6）
In, the antioxidant is petroleum ether, cyclohexane, at least one in dichlorodifluoromethan.
6. the preparation method of high-coercive force samarium-cobalt permanent-magnetic material according to claim 4, it is characterised in that step（6）In,
The antioxidant is petroleum ether, cyclohexane, at least one in dichlorodifluoromethan.
7. the preparation method of the high-coercive force samarium-cobalt permanent-magnetic material according to Claims 2 or 3, it is characterised in that step（1）
In, metal of the raw material using purity >=99.9%.
8. the preparation method of the high-coercive force samarium-cobalt permanent-magnetic material according to Claims 2 or 3, it is characterised in that step（4）
In, metal of the raw material using purity >=99.9%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510916433.6A CN105374484B (en) | 2015-12-10 | 2015-12-10 | High-coercivity samarium-cobalt permanent magnet material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510916433.6A CN105374484B (en) | 2015-12-10 | 2015-12-10 | High-coercivity samarium-cobalt permanent magnet material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105374484A CN105374484A (en) | 2016-03-02 |
| CN105374484B true CN105374484B (en) | 2017-04-12 |
Family
ID=55376592
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510916433.6A Active CN105374484B (en) | 2015-12-10 | 2015-12-10 | High-coercivity samarium-cobalt permanent magnet material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105374484B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106328366B (en) * | 2016-08-26 | 2017-12-26 | 宁波宁港永磁材料有限公司 | A kind of preparation method of high-performance samarium-cobalt permanent-magnetic material |
| CN109872855B (en) * | 2017-12-04 | 2021-01-15 | 中国科学院宁波材料技术与工程研究所 | High-coercivity rare earth cobalt-based permanent magnet material and preparation method thereof |
| 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 |
| CN111091943B (en) * | 2019-12-24 | 2021-02-26 | 中国计量大学 | Low-temperature coefficient Sm2Co17Molded sintered magnet and method for producing same |
| CN112103068B (en) * | 2020-08-28 | 2022-01-04 | 杭州永磁集团有限公司 | Preparation method of high-magnetic-performance 1:5 pure samarium cobalt permanent magnet |
| CN113744987B (en) * | 2021-08-25 | 2022-09-30 | 北京航空航天大学 | Method for preparing high-performance samarium-cobalt magnet through grain boundary structure reconstruction |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63118042A (en) * | 1986-11-05 | 1988-05-23 | Hitachi Metals Ltd | Permanent magnet material and its production |
| CN102071339A (en) * | 2011-01-24 | 2011-05-25 | 宁波科星材料科技有限公司 | Samarium-cobalt permanent magnet material and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5107198B2 (en) * | 2008-09-22 | 2012-12-26 | 株式会社東芝 | PERMANENT MAGNET, PERMANENT MAGNET MANUFACTURING METHOD, AND MOTOR USING THE SAME |
| CN104183349B (en) * | 2013-05-22 | 2017-08-25 | 中国科学院宁波材料技术与工程研究所 | A kind of SmCo base permanent magnet, its preparation method and magnetic property regulation and control method |
-
2015
- 2015-12-10 CN CN201510916433.6A patent/CN105374484B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63118042A (en) * | 1986-11-05 | 1988-05-23 | Hitachi Metals Ltd | Permanent magnet material and its production |
| CN102071339A (en) * | 2011-01-24 | 2011-05-25 | 宁波科星材料科技有限公司 | Samarium-cobalt permanent magnet material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105374484A (en) | 2016-03-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105374484B (en) | High-coercivity samarium-cobalt permanent magnet material and preparation method thereof | |
| CN108103381B (en) | High-strength FeCoNiCrMn high-entropy alloy and preparation method thereof | |
| CN102220538B (en) | Sintered neodymium-iron-boron preparation method capable of improving intrinsic coercivity and anticorrosive performance | |
| CN105741995B (en) | A kind of high performance sintered neodymium-iron-boron permanent magnet and preparation method thereof | |
| US10049797B2 (en) | Low-neodymium, non-heavy-rare-earth and high performance magnet | |
| CN105321644B (en) | A kind of high-coercive force sintered state Ce magnets or richness Ce magnets and preparation method thereof | |
| CN102568807B (en) | Method for preparing high-coercivity SmCoFeCuZr (samarium-cobalt-ferrum-copper-zirconium) high-temperature permanent magnet by doping nano-Cu powder | |
| CN104599801A (en) | Rare earth permanent magnetic material and preparation method thereof | |
| CN110364325B (en) | Yttrium-added rare earth permanent magnet material and preparation method thereof | |
| CN107742564B (en) | A kind of method that the auxiliary alloy addition of high dysprosium prepares low-cost neodymium iron boron magnet | |
| EP4020505B1 (en) | Preparation method for a neodymium-iron-boron magnet | |
| CN104064301B (en) | NdFeB magnet and preparation method thereof | |
| CN101748326B (en) | Preparation method of carbonic rare earth-ferrum, cobalt and silicon compound with NaZn1 structure | |
| CN104575901A (en) | Neodymium iron boron magnet added with terbium powder and preparation method thereof | |
| CN110853854A (en) | Method for preparing high-performance double-main-phase sintered mixed rare earth iron boron magnet by two-step diffusion method | |
| CN103426578A (en) | Rare earth permanent magnetic material and method for preparing same | |
| CN104575902A (en) | Neodymium iron boron magnet added with cerium and preparation method thereof | |
| CN107146674A (en) | From the cerium-rich rare earth permanent magnet and its production method of heat treatment | |
| CN110534280A (en) | A kind of preparation method of the performance Nd Fe B sintered magnet based on crystal boundary addition | |
| CN110957090A (en) | A samarium cobalt 1: 5-type permanent magnet material and preparation method thereof | |
| CN110153415B (en) | Preparation method of neodymium iron boron magnet | |
| CN106328331B (en) | Sintered NdFeB magnet assistant alloy slab and preparation method thereof | |
| CN109786097A (en) | A kind of preparation method of driving motor dedicated high performance Nd-Fe-B permanent magnet | |
| CN112582123B (en) | Preparation method of sintered samarium-cobalt magnet with low temperature coefficient and high use temperature | |
| CN102768890A (en) | Preparation method of rare earth anisotropism magnetic powder, magnetic powder and magnetic body |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |