CN109706338A - A kind of sintered samarium cobalt magnet preparation method - Google Patents
A kind of sintered samarium cobalt magnet preparation method Download PDFInfo
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- CN109706338A CN109706338A CN201910064865.7A CN201910064865A CN109706338A CN 109706338 A CN109706338 A CN 109706338A CN 201910064865 A CN201910064865 A CN 201910064865A CN 109706338 A CN109706338 A CN 109706338A
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Abstract
The invention discloses a kind of sintered samarium cobalt magnet preparation methods, comprising the following steps: (1) is crushed sintered samarium cobalt alloy pig, obtains samarium-cobalt alloy particle；(2) it by samarium-cobalt alloy particle, puts into the airflow milling equipment of nitrogen protection, in the case where stream of nitrogen gas is blown, powder particle mutually collides broken；Broken samarium-cobalt alloy powder, screens removal coarse granule by grading wheel, screens removal fine grained using cyclone separator, obtains samarium-cobalt alloy powder of the average grain diameter at 2 ~ 10 μm；Then (3) samarium-cobalt alloy powder is carried out to be orientated in magnetic field and pre-molding, the static pressure suppressions molding such as, finally in 1170-1199 DEG C of sinter molding, obtains sintered samarium cobalt magnet.It is at low cost that the present invention prepares samarium-cobalt magnet method powder, does not use flammable solvent, and no security risk, samarium-cobalt alloy powder uniformity is good, and sintered magnet is easy to control, and product magnetic property is more stable outstanding, can prepare various high-performance or property requires product.
Description
Technical field
The present invention relates to a kind of magnet material processing technology, in particular to a kind of samarium-cobalt magnet preparation method belongs to magnetism
Field of material technology.
Background technique
Samarium-cobalt magnet includes SmCo5、Sm2Co17Extraordinary rare-earth magnet, be widely used in Aeronautics and Astronautics, Military Electronics,
The fields such as automobile, sensor, petrochemical industry, magnetic drives.Samarium-cobalt magnet has high energy product, high-coercive force, high remanent magnetism, extremely low
Temperature coefficient (- 0.030%/DEG C), very high use the outstanding features such as temperature (maximum operation (service) temperature is 550 DEG C).So that samarium
Temperature stability, the chemical stability of cobalt magnet considerably beyond neodymium iron boron magnetic body, can preferably be applied to various severe rings
Border.
Existing sintering 2:17 type Sm-Co magnet is mainly prepared by powder metallurgy process, and technical process is ingredient, melts
Refine alloy, alloy breaks down powder, powder oriented moulding and heat treatment.Molten alloy, alloy breaks down powder and heat treatment process etc.
It is the key link for influencing samarium-cobalt magnet magnetic property, the samarium-cobalt magnet required for high-quality must ensure that each technique walks simultaneously
Suddenly all it is optimal control.
Specifically, being usually sintered 2:17 type samarium-cobalt magnet molten alloy ingot, being that progress machinery is rough and torn first is broken into alloy
Then particle is put into ball grinder, solvent and mill ball is added, rotates ball grinder after ball grinder sealing, the rolling of mill ball is touched
Hitting crushes alloying pellet, obtains powder particle of the average particle size at 2~10 μm, then carry out oriented moulding in magnetic field, goes forward side by side
Row heat treatment, preparation sintering 2:17 type samarium-cobalt magnet.
Wherein, ball milling flouring technology, there are the following problems:
(1) low efficiency, it is at high cost.Ball milling milling efficiency is low, and most important problem is that in mechanical milling process, each ball
The milling amount for grinding machinery equipment is limited, the processing capacity of usually only several kilograms to more than ten kilograms of single ball milling machine, such as 5kg,
Ball milling processing must be carried out using a large amount of mechanical mills are synchronous, just be able to satisfy production needs.In this way, ball milling flouring technology
Efficiency overall performance is lower, a large amount of equipment investment, either management service or production run bring production cost all compared with
It is high.
(2) flammable solvent need to be used, there are very high security risks.It needs to consume a large amount of ball during ball powder-grinding
Mill solvent, existing production line solvent-oil ratio is big, and solvent average unit cost 5-20 member/L is differed, non-for the cost control of powder processed
Chang Buli.Moreover, solvent is usually all inflammable explosive article, charges, discharging, filters, partial solvent is volatized into drying course
Into air, there is biggish security risk.Grinding line must periodically carry out safety training to operator, and necessity is arranged
Safe goalkeeper, secure supervisor, case of emergency processing assistant director etc. posies.
(3) powder uniformity is poor.The uniformity of the samarium-cobalt magnet powder raw material of ball milling preparation is poor, although may be implemented
Better powder size grade, but samarium-cobalt magnet uniformity is poor.A large amount of ball-grinding machines are primarily due to mutually because each
Secondary charging, all there may be fluctuating changes for the preparation of size abrading-ball etc. of ball milling solvent, ball milling, lead to same batch difference ball
There is larger difference between each other in the samarium-cobalt magnet powder of mill machining preparation.
(4) the special hilllock of special messenger must be prepared.The use of ball-grinding machine needs special technical staff to operate, including ball milling
Canned material, addition ball milling solvent etc., a usual operator needs the time most of the day to complete above-mentioned ball milling preparation.And
And ball milling needs to can be only achieved the grain size category (saving the production time, conveniently make full use of the working time) of requirement overnight,
It also needs operator morning next day successively to pour out the product in ball-grinding machine, filter, drying, the powder original then obtained
Material just can be carried out subsequent precompressed processing.It is largely fully operational that the charging of ball-grinding machine, discharging require the special hilllock of special messenger, leads to ball
It is low to grind charging efficiency.
(5) scheduling arranges more difficult.Described in 4th point as above, after ball milling is completed, special messenger is needed to fall material
Out, it filters, is dry, the second day progress aforesaid operations usually to feed intake in ball milling.These operations take around consumption time half a day,
Process precompressed work must could be carried out after powder is dry afterwards.So existing ball-milling technology results in samarium-cobalt magnet
The job placement of production preparation becomes more difficult, and production efficiency is affected.
Airflow milling is widely used in Nd-Fe-B magnetic powder preparation process, samarium-cobalt magnet is hard as a kind of high efficiency grinding technique
Degree is higher, and quality is more crisp, temporarily has not seen the report that powder processed is carried out using airflow milling.Airflow milling is not applied to the life of samarium-cobalt magnet
Produce processing, main reason is that the technical maturity of airflow milling is bad, especially the magnet powder roughness of airflow milling processing compared with
Height influences the mobility of powder, prepares being affected for samarium-cobalt magnet blank for powder metallurgy.Even if being attempted, also can
Encounter airflow milling processing powder corner angle it is more, samarium-cobalt alloy powder is orientated bad problem.
Summary of the invention
It is an object of the invention to existing during overcoming ball milling in the prior art to prepare samarium-cobalt magnet powder raw material
The problems such as cost, uniformity, security risk, scheduling, provide a kind of sintered samarium cobalt magnet preparation method.The present invention uses completely new
Airflow milling processing prepares samarium-cobalt magnet powder, and specific aim is carried out the characteristics of for samarium-cobalt magnet and is optimized and revised, and realizes that airflow milling is high
The comprehensive coordinate that efficiency and samarium-cobalt magnet powder processing high-quality require.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical schemes:
A kind of sintered samarium cobalt magnet preparation method, comprising the following steps:
(1) sintered samarium cobalt alloy pig is crushed, obtains samarium-cobalt alloy particle.
(2) it by samarium-cobalt alloy particle, puts into the airflow milling equipment of nitrogen protection, in the case where stream of nitrogen gas is blown, powder
Grain mutually collision is broken；Broken samarium-cobalt alloy powder screens removal coarse granule by grading wheel, using cyclone separator
Screening removal fine grained, obtains samarium-cobalt alloy powder of the average grain diameter at 2~10 μm.
Then (3) samarium-cobalt alloy powder is carried out to be orientated in magnetic field and pre-molding, the static pressure suppressions molding such as, is finally existed
1170-1199 DEG C of sinter molding obtains sintered samarium cobalt magnet.
The method that the present invention prepares sintered samarium cobalt magnet replaces ball-grinding machine in the prior art, air-flow using airflow milling
Ball grinding technique is avoided in mill process there are solvent use cost height, has the deficiencies of security risk, while airflow milling is processed
When samarium-cobalt alloy particle, efficiency is very high, and powder preparation can be rapidly completed, and solves ball milling processing speed in the prior art
Degree is slow, the problem for causing scheduling difficult.
Alloy powder particle is passed through grading wheel by the roughness control for airflow milling processing samarium-cobalt magnet powder, the present invention
Screening and cyclone separator screening, the average particle size range of samarium-cobalt alloy powder are controlled at 2~10 μm.In this way, which one can
Good to control alloy powder epigranular degree, test result shows that overall particle size consistency is very good；Second, SmCo after screening
Alloy powder pre-molding in magnetic field has preferable mobility；By the collaboration of two aspect effects, so that airflow milling technology
It is combined with each other with samarium-cobalt magnet powder metallurgy and reaches good accurate control meaning, improve airflow milling processing samarium-cobalt magnet product
Performance.
Samarium-cobalt magnet powder entirety uniformity controlling by airflow milling working process is more preferable, meanwhile, in conjunction with conjunction appropriate
Bronze end particle screen selecting overcomes the problems, such as that the alloy powder corner angle that airflow milling crushes influence mixing, so that airflow milling and powder smelting
Gold prepares the combination of samarium-cobalt magnet blank, and final magnet sinter molding temperature control obtains letter to a certain extent
Change.For common ball milling processing, it is more careful that airflow milling of the present invention obtains samarium-cobalt alloy powder raw material, sintering process
Middle temperature reduces 5-30 DEG C, and the overall performance performance of samarium-cobalt magnet gets a promotion after being sintered.Moreover, because sintering temperature drops
Low, the energy consumption in sintering process is slightly reduced, and the thermal requirements of sintering furnace is also reduced accordingly, so that service life of equipment
Synchronizing is improved.
Further, step 2, airflow milling equipment is protected using high pure nitrogen, blows samarium-cobalt alloy particle as certain driving air-flow
Mutually collision is broken.The effect protected using high pure nitrogen is very good, and the problem of oxidation of airflow milling is resolved, and material
Preferably, the efficiency of powder metallurgy and alloy powder local temperature rise are coordinated, and can be very good to guarantee finally to prepare for temperature control
The efficiency and quality of powder metallurgy samarium-cobalt magnet.
Preferably, the high pure nitrogen is the nitrogen that purity is greater than 99.999v%.By optimizing the high pure nitrogen used
Degree of purity can effectively control the oxygen content in carrier gas, and then control the oxygen content of the SmCo powder of airflow milling processing, so that
Oxygen content in the samarium-cobalt magnet of final sinter molding is kept within the appropriate range, it is ensured that the comprehensive performance of samarium-cobalt magnet is excellent
It is good.
Further, the airflow milling is the airflow milling that power is 30-200kw.The relatively large airflow milling of power is selected to set
Standby be more advantageous to ensures that for collision crashing at the grain size category of powder particle, power gets over high gas flow to samarium-cobalt alloy particle in airflow milling
The rate of mill is faster, and processing efficiency is higher.But too high power be easy to cause energy waste to lose for production requirement.
Further, powder particle mutually collide it is broken after, remove coarse granule by rotation grading wheel screening.
Further, the coarse granule is the particle for the granularity that size is greater than process stipulation.Coarse granule is used for sintered samarium cobalt magnetic
Body is larger for qualitative effects, broken by continuing cycling through in the isolated coarse granule importing airflow milling of screening.It can be revolved using high speed
Turn grading wheel screening and remove coarse granule, such as can be removed using rotation grading wheel screening and be greater than 10 μm, 15 μm, 20 μm of
The specific partial size of grain, particle can need to be adjusted according to different processing technologys, to realize power consumption of polymer processing, efficiency and difference
Production requirement before coordination.
Further, the fine grained refers to that size is less than the particle of the granularity of process stipulation.Grain diameter is too small, is easy oxygen
Change, the samarium-cobalt magnet performance that compression moulding obtains will receive influence, be unfavorable for preparing high-quality samarium-cobalt magnet product.It can use
Cyclone separator is separated, other efficient separation equipments can also be used, preferably by cyclone separator, separative efficiency
Height will not introduce other disturbing factors.The fine grained that cyclone separator can be sieved is reused for melting and is sintered
To samarium-cobalt alloy ingot.
Further, during airflow milling milling, it is additionally added organic solvent.The effect of organic solvent be it is anti-oxidation, point
Dissipate and rise lubricating action so that during airflow milling is broken samarium-cobalt alloy Powder Oxidation extent control within the appropriate range,
The reunion of powder is reduced, and has lubrication facilitation well to later period compression moulding.
Preferably, the dosage of the organic solvent is 0~2% relative to samarium-cobalt alloy particle weight ratio.Preferably
0.1-1%
Further, step 3, in 1175-1199 DEG C of sinter molding.It is preferred that in 1175-1195 DEG C of sinter molding, such as can be with
It is 1180 DEG C, 1185 DEG C, 1190 DEG C of sinter moldings.
Compared with prior art, beneficial effects of the present invention:
1, after samarium-cobalt magnet preparation method of the present invention replaces ball powder-grinding using airflow milling, powder cost per kilogram processed is reduced about
20-30%, and flammable solvent is not used, exclude security risk.
2, samarium-cobalt magnet preparation method of the present invention prepares samarium-cobalt alloy powder using airflow milling processing, has high efficiency, high
The characteristics of quality, the samarium-cobalt alloy powder diameter range processed are suitable for that powder uniformity improves.Finally it is sintered obtained magnetic
Body magnetic property is more stable, can prepare high-performance and property requires product.
3, the alloy powder particle size range control that samarium-cobalt magnet preparation method of the present invention is milled later using airflow milling is outstanding,
So that being more easier to control during pre-molding and sintering, sintering temperature reduces 5-30 DEG C compared with prior art, and sintering is set
Standby temperature controlling range is widened, and sintered products consistency improves, and property improved stability.
4, samarium-cobalt magnet coercivity, remanent magnetism, maximum magnetic energy product that samarium-cobalt magnet preparation method of the present invention is prepared etc. be all
There is different degrees of promotion/improvement, the samarium-cobalt magnet product of higher quality grade can be obtained.
5, samarium-cobalt magnet preparation method processing temperature of the present invention is lower, and the load of sinter molding equipment is smaller, reduces equipment
High temperature consumption extends the service life of agglomerating plant.
Detailed description of the invention:
Fig. 1 is the samarium-cobalt alloy powder that airflow milling obtains, the photo of 1000 times of amplification.
Fig. 2 is the samarium-cobalt alloy powder that airflow milling obtains, the photo of 2000 times of amplification.
Specific embodiment
Further, organic solvent can be added during airflow milling milling is: 2,6- di-tert-butyl-4-methy phenols
(BHT), BHA, isopropanol, solvent naphtha or 6# solvent naphtha.Organic solvent can optimize sintered samarium cobalt alloy and crush in airflow milling
Collision difficulty, bulky grain during airflow milling, which is crushed, has certain facilitation, preferably keeps alloy powder
Uniformity.The amount of oxidation that processing samarium-cobalt alloy powder is ground at the same time it can also optimization airflow, so that samarium-cobalt alloy powder is pressed into base
It is more excellent that block is sintered later magnet product oxygen content.And optimize the steering difficulty of samarium-cobalt alloy powder compacting briquet process, it improves
The briquet degree of orientation, it is comprehensive to improve the quality grade that samarium-cobalt magnet is made.
Samarium-cobalt magnet processing method of the present invention has used airflow milling to process samarium-cobalt alloy raw material powder, and samarium-cobalt alloy is because originally
Body is harder, also without suitable precrushing technique, causes its broken difficulty much higher than neodymium iron boron.Directly using conventional air-flow grinder
Skill is processed, and can have the defects that the broken granulation uniformity of processing is bad.Meanwhile samarium-cobalt alloy is in airflow milling process
In be easy to appear that oxygen content is exceeded, lead to the poor quality of sintered samarium cobalt magnet, you must use ball-milling technology.The present invention is logical
The technological parameter for crossing optimization airflow mill, selects carrier and organic solvent appropriate, so that jet milling process can be good at applying
In the processing of samarium-cobalt magnet, many disadvantages are overcome, reduce the energy consumption cost of samarium-cobalt magnet processing.
Below with reference to test example and specific embodiment, the present invention is described in further detail.But this should not be understood
It is all that this is belonged to based on the technology that the content of present invention is realized for the scope of the above subject matter of the present invention is limited to the following embodiments
The range of invention.High pure nitrogen used in the following embodiment is the nitrogen that purity is greater than 99.999%.
<comparative example 1>
Samarium-cobalt alloy powder is prepared using prior art ball-milling method, 200 kilograms of melted 2:17 type samarium-cobalt alloy ingots are used broken
Broken machine is broken into the alloying pellet that partial size is less than 2mm.Then, ball grinder is added in samarium-cobalt alloy powder, solvent naphtha conduct is added
Ball milling solvent, is proportionally added into big ball, bead, and ball milling 12h is stayed overnight.After the completion of ball milling, filter, it is dry, obtain samarium-cobalt alloy powder
This powder is orientated in the magnetic field of 1.5T, and obtains SmCo powder mass with 12MPa pressure pre-molding by end, by this SmCo powder
The static pressure such as last block 280MPa 3 minutes, obtain blank.Blank is put into sintering furnace, adjusts 1200 DEG C of sintering temperature, is sintered 150 points
Sintering 2:17 type samarium-cobalt magnet is made in clock.
<embodiment 1>
By 200 kilograms of melted 2:17 type samarium-cobalt alloy ingot crushers, it is broken into the alloying pellet that partial size is less than 2mm.
The organic solvent of 0.5wt% is added, is uniformly mixed.With high-purity N2Protective atmosphere and carrier gas are carried out, this samarium-cobalt alloy particle is thrown
In the airflow milling equipment entered, in high speed N2Air-flow is blown down, and mutually collision is broken between powder particle, using high speed rotation point
10 μm of partial size of removal of step cone screening or more of coarse granule is obtained using 2 μm of partial size of removal of cyclone separator screening or less fine graineds
Obtain powder particle of the average particle size at 2~10 μm.During entire airflow milling, Control for Oxygen Content is in 100~300ppm.By this powder
Last particle is orientated in the magnetic field of 1.5T, and obtains SmCo powder mass with 12MPa pressure pre-molding, by this SmCo powder mass
The static pressure such as 280MPa 3 minutes, obtain blank.Blank is put into sintering furnace, adjusts 1195 DEG C of sintering temperature, is sintered 150 minutes, system
2:17 type samarium-cobalt magnet must be sintered.
Airflow milling is widely used in neodymium iron boron magnetic body processing in the prior art, has the characteristics that efficient, the present invention
It is exclusively used in 2:17 type Sm-Co magnetic powder preparation process, still belong to the first time innovation test.
<embodiment 2>
By 200 kilograms of melted 2:17 type samarium-cobalt alloy ingot crushers, it is broken into the alloying pellet that partial size is less than 2mm.
The organic solvent of 0.05wt% is added, is uniformly mixed.With high-purity N2Protective atmosphere and carrier gas are carried out, this samarium-cobalt alloy particle is thrown
Enter in airflow milling equipment, in high speed N2Air-flow is blown down, and mutually collision is broken between powder particle, is classified using high speed rotation
10 μm of partial size of removal of wheel screening or more of coarse granule is obtained using 2 μm of partial size of removal of cyclone separator screening or less fine graineds
Powder particle of the average particle size at 2~10 μm.During entire airflow milling, Control for Oxygen Content is in 100~300ppm.By this powder
Particle is orientated in the magnetic field of 1.5T, and obtains SmCo powder mass with 12MPa pressure pre-molding, by this SmCo powder mass
The static pressure such as 280MPa 3 minutes, obtain blank.Blank is put into sintering furnace, adjusts 1195 DEG C of sintering temperature, is sintered 150 minutes, system
2:17 type samarium-cobalt magnet must be sintered.
<embodiment 3>
By 200 kilograms of melted 2:17 type samarium-cobalt alloy ingot crushers, it is broken into the alloying pellet that partial size is less than 2mm.
1wt% organic solvent is added, is uniformly mixed.With high-purity N2Protective atmosphere and carrier gas are carried out, this samarium-cobalt alloy particle is put into gas
In stream mill equipment, in high speed N2Air-flow is blown down, and mutually collision is broken between powder particle, is sieved using high speed rotation grading wheel
The coarse granule of 10 μm of partial size of choosing removal or more is averaged using 2 μm of partial size of removal of cyclone separator screening or less fine graineds
Powder particle of the granularity at 2~10 μm.During entire airflow milling, Control for Oxygen Content is in 100~300ppm.By this powder particle
It is orientated in the magnetic field of 1.5T, and obtains SmCo powder mass with 12MPa pressure pre-molding, by this SmCo powder mass 280MPa etc.
Static pressure 3 minutes, obtain blank.Blank is put into sintering furnace, adjusts 1195 DEG C of sintering temperature, is sintered 150 minutes, sintering 2 is made:
17 type samarium-cobalt magnets.
The airflow milling samarium-cobalt alloy powder being prepared is subjected to micro- sem observation, as a result as shown in Figs. 1-2, amplification 1000
Again, 2000 times of photo shows that the broken uniformity of samarium-cobalt alloy powder is preferable respectively,
When previous trial thinks that airflow milling prepares samarium-cobalt magnet powder, there are crushed particles corner angle are more；SmCo
Alloy brittleness is big, and airflow milling impact several times cause part to be easy to appear the excessively subtle deficiency of part samarium-cobalt alloy powder, if
It is too tiny to crush samarium-cobalt alloy particle, then being also easy to aoxidize, so that the property-deterioration of samarium-cobalt alloy particle.It is suitable by being added
When BHT and solvent naphtha realize the accelerating auxiliaries that crush for airflow milling so that air-flow fine grinding particle and coarse granule obtain very well
Control, avoid excessive fine grained from generating, improve the utilization efficiency of material, also guarantee the later product of samarium-cobalt magnet sinter molding
Matter is more excellent.
<comparative example 2>
By 200 kilograms of melted 2:17 type samarium-cobalt alloy ingot crushers, it is broken into the alloying pellet that partial size is less than 2mm.
The organic solvent of 0.5wt% is added, is uniformly mixed.By the N of this samarium-cobalt alloy particle investment high-purity2The airflow milling equipment of protection
In, in high speed N2Air-flow is blown down, and mutually collision is broken between powder particle, screens removal grain using high speed rotation grading wheel
8 μm of diameter or more of coarse granule, using cyclone separator screening 1 μm of partial size or less fine grained of removal, obtain average particle size 1~
8 μm of powder particle.During entire airflow milling, Control for Oxygen Content is in 100~300ppm.By this powder particle 1.5T magnetic
It is orientated in, and obtains SmCo powder mass with 12MPa pressure pre-molding, by this SmCo powder mass 280MPa etc. static pressure 3 minutes,
Obtain blank.Blank is put into sintering furnace, adjusts 1195 DEG C of sintering temperature, is sintered 150 minutes, sintering 2:17 type SmCo magnetic is made
Body.
<comparative example 3>
By 200 kilograms of melted 2:17 type samarium-cobalt alloy ingot crushers, it is broken into the alloying pellet that partial size is less than 2mm.
The organic solvent of 0.5wt% is added, is uniformly mixed.By this samarium-cobalt alloy particle high-purity N2In the airflow milling equipment of protection, in height
Fast N2Air-flow is blown down, and mutually collision is broken between powder particle, using 15 μm of partial size of removal of the screening of high speed rotation grading wheel
Above coarse granule obtains average particle size at 3~15 μm using 3 μm of partial size of removal of cyclone separator screening or less fine graineds
Powder particle.During entire airflow milling, Control for Oxygen Content is in 100~300ppm.By this powder particle in the magnetic field of 1.5T
Middle orientation, and SmCo powder mass is obtained with 12MPa pressure pre-molding, this SmCo powder mass 280MPa etc. static pressure 3 minutes obtain
To blank.Blank is put into sintering furnace, adjusts 1195 DEG C of sintering temperature, is sintered 150 minutes, sintering 2:17 type SmCo magnetic is made
Body.
<comparative example 4>
By 200 kilograms of melted 2:17 type samarium-cobalt alloy ingot crushers, it is broken into the alloying pellet that partial size is less than 2mm.
The organic solvent of 0.5wt% is added, is uniformly mixed.By this samarium-cobalt alloy particle high-purity N2In the airflow milling equipment of protection, in height
Fast N2Air-flow is blown down, and mutually collision is broken between powder particle, using 10 μm of partial size of removal of the screening of high speed rotation grading wheel
Above coarse granule obtains average particle size at 2~10 μm using 2 μm of partial size of removal of cyclone separator screening or less fine graineds
Powder particle.During entire airflow milling, Control for Oxygen Content is in 500~1000ppm.By this powder particle in the magnetic field of 1.5T
Middle orientation, and SmCo powder mass is obtained with 12MPa pressure pre-molding, this SmCo powder mass 280MPa etc. static pressure 3 minutes obtain
To blank.Blank is put into sintering furnace, adjusts 1185 DEG C of sintering temperature, is sintered 150 minutes, sintering 2:17 type SmCo magnetic is made
Body.
<comparative example 5>
By 200 kilograms of melted 2:17 type samarium-cobalt alloy ingot crushers, it is broken into the alloying pellet that partial size is less than 2mm.
The organic solvent of 0.5wt% is added, is uniformly mixed.By this samarium-cobalt alloy particle high-purity N2In the airflow milling equipment of protection, in height
Fast N2Air-flow is blown down, and mutually collision is broken between powder particle, using 10 μm of partial size of removal of the screening of high speed rotation grading wheel
Above coarse granule obtains average particle size at 2~10 μm using 2 μm of partial size of removal of cyclone separator screening or less fine graineds
Powder particle.During entire airflow milling, Control for Oxygen Content is in 100~300ppm.By this powder particle in the magnetic field of 1.5T
Middle orientation, and SmCo powder mass is obtained with 12MPa pressure pre-molding, this SmCo powder mass 280MPa etc. static pressure 3 minutes obtain
To blank.Blank is put into sintering furnace, adjusts 1175 DEG C of sintering temperature, is sintered 150 minutes, sintering 2:17 type SmCo magnetic is made
Body.
<test>
Samarium-cobalt magnet prepared by above-described embodiment and comparative example is tested, measure respectively density, remanent magnetism, coercivity,
The samarium-cobalt magnets major parameter such as maximum magnetic energy product, as a result as shown in the table.
1 samarium-cobalt magnet properties of product of table
* sintering energy consumption comprehensively considers estimation energy consumption and saves ratio according to sintering temperature and blank sintering time.
Test result shows, when the method for preparing samarium-cobalt magnet is used instead after airflow milling prepares samarium-cobalt magnet powder raw material,
Although sintering temperature reduces, the magnet powder particle size reduction being mainly sintered simultaneously optimizes, so sintering temperature can be reduced slightly,
Soaking time required for being sintered simultaneously is also shortened, and comprehensive sintering energy consumption reduces.By test analysis, airflow milling is through excessively high
Purity nitrogen gas shielded, and assist the SmCo magnetic for the final sinter molding of alloy powder for enabling to airflow milling broken with organic solvent
Body is best in quality, obtains best samarium-cobalt magnet quality grade.
If, must since samarium-cobalt alloy has inflammability after airflow milling crushing during preparing samarium-cobalt magnet
Nitrogen protection must be used.If do not protected using high pure nitrogen in airflow milling process, then samarium-cobalt magnet powder is processed
Poor quality, one side fine particle fraction increases, and the utilization rate of samarium-cobalt alloy ingot reduces, powder oxygen obtained by another aspect airflow milling
Content is higher, and samarium-cobalt alloy powder compacting briquet sintering quality decreases.
When airflow milling processes samarium-cobalt magnet powder, by selecting suitable samarium-cobalt alloy airflow milling treatment process to join
Said conditions carry out airflow milling using appropriate carrier gas and screen suitable alloy powder partial size in conjunction with the auxiliary of organic solvent, make
Airflow milling processing the control of samarium-cobalt alloy oxygen content in power in lower range, the oxygen content of the samarium-cobalt magnet of final molding compared with
Low, final sintered samarium cobalt magnet quality-improving improves, and the samarium-cobalt magnet comprehensive performance being prepared has greatly improved optimization.
Claims (9)
1. a kind of sintered samarium cobalt magnet preparation method, comprising the following steps:
(1) sintered samarium cobalt alloy pig is crushed, obtains samarium-cobalt alloy particle；
(2) it by samarium-cobalt alloy particle, puts into the airflow milling equipment of nitrogen protection, in the case where stream of nitrogen gas is blown, powder particle phase
Mutually collision is broken；Broken samarium-cobalt alloy powder screens removal coarse granule by grading wheel, screens using cyclone separator
Fine grained is removed, samarium-cobalt alloy powder of the average grain diameter at 2 ~ 10 μm is obtained；
Then (3) samarium-cobalt alloy powder is carried out to be orientated in magnetic field and pre-molding, the static pressure suppressions molding such as, is finally existed
1170-1199 DEG C of sinter molding obtains sintered samarium cobalt magnet.
2. sintered samarium cobalt magnet preparation method as described in claim 1, which is characterized in that step 2, airflow milling equipment is using high-purity
Nitrogen protection, as certain driving air-flow blow samarium-cobalt alloy particle mutually collide it is broken.
3. sintered samarium cobalt magnet preparation method as described in claim 1, which is characterized in that high pure nitrogen is greater than using purity
99.999% nitrogen.
4. sintered samarium cobalt magnet preparation method as described in claim 1, which is characterized in that the airflow milling is that power is 30-
The airflow milling of 200kw.
5. sintered samarium cobalt magnet preparation method as described in claim 1, which is characterized in that powder particle mutually collide it is broken with
Afterwards, coarse granule is removed by rotation grading wheel screening.
6. sintered samarium cobalt magnet preparation method as described in claim 1, which is characterized in that the coarse granule is that size is greater than technique
The particle of defined granularity.
7. sintered samarium cobalt magnet preparation method as described in claim 1, which is characterized in that the fine grained refers to that size is less than work
The particle of granularity as defined in skill.
8. sintered samarium cobalt magnet preparation method as described in claim 1, which is characterized in that airflow milling be milled during, also plus
Enter organic solvent.
9. sintered samarium cobalt magnet preparation method as described in claim 1, which is characterized in that the dosage of the organic solvent is opposite
In the 0 ~ 2% of samarium-cobalt alloy particle weight ratio.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112435846A (en) * | 2020-10-28 | 2021-03-02 | 包头市沃野对外贸易有限责任公司 | Manufacturing method of 550-DEG C-resistant samarium-cobalt permanent magnet material |
| CN112570719A (en) * | 2019-09-27 | 2021-03-30 | 河北泛磁聚智电子元件制造有限公司 | Additive adding method and device for preparing samarium cobalt magnetic powder |
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| CN103065788A (en) * | 2012-12-26 | 2013-04-24 | 宁波韵升股份有限公司 | Method for preparing sintered samarium-cobalt magnet |
| CN105355352A (en) * | 2015-12-14 | 2016-02-24 | 成都银河磁体股份有限公司 | Low-coercive-force samarium-cobalt magnet and preparation method thereof |
| CN107316726A (en) * | 2017-07-14 | 2017-11-03 | 钢铁研究总院 | A kind of preparation method of sintered samarium cobalt magnet |
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| CN103065788A (en) * | 2012-12-26 | 2013-04-24 | 宁波韵升股份有限公司 | Method for preparing sintered samarium-cobalt magnet |
| CN105355352A (en) * | 2015-12-14 | 2016-02-24 | 成都银河磁体股份有限公司 | Low-coercive-force samarium-cobalt magnet and preparation method thereof |
| CN107316726A (en) * | 2017-07-14 | 2017-11-03 | 钢铁研究总院 | A kind of preparation method of sintered samarium cobalt magnet |
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| CN112570719A (en) * | 2019-09-27 | 2021-03-30 | 河北泛磁聚智电子元件制造有限公司 | Additive adding method and device for preparing samarium cobalt magnetic powder |
| CN112570719B (en) * | 2019-09-27 | 2023-02-03 | 河北泛磁聚智电子元件制造有限公司 | Additive adding method and device for preparing samarium cobalt magnetic powder |
| CN112435846A (en) * | 2020-10-28 | 2021-03-02 | 包头市沃野对外贸易有限责任公司 | Manufacturing method of 550-DEG C-resistant samarium-cobalt permanent magnet material |
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