CN108281245A - A kind of preparation method of samarium cobalt permanent magnet body - Google Patents
A kind of preparation method of samarium cobalt permanent magnet body Download PDFInfo
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- CN108281245A CN108281245A CN201810067697.2A CN201810067697A CN108281245A CN 108281245 A CN108281245 A CN 108281245A CN 201810067697 A CN201810067697 A CN 201810067697A CN 108281245 A CN108281245 A CN 108281245A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
- H01F1/0557—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together sintered
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/07—Alloys based on nickel or cobalt based on cobalt
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0266—Moulding; Pressing
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Abstract
The invention discloses a kind of preparation methods of samarium cobalt permanent magnet body, including：Raw material is configured by weight percentage, contains samarium 23 29%, cobalt 46 54%, iron 9 17%, copper 3 8%, zirconium 1 5% in raw material；The raw material of preparation is placed in melting in intermediate frequency electromagnetic stove, obtains alloy molten solution；Alloy molten solution is poured into ingot casting die cavity, ingot casting is obtained；Ingot casting is crushed, then powder processed using forcing press, is refined, pressure treatment shapes twice by forcing press, cold isostatic press by the powder after fine grinding, forms regular prism or the blank of cylinder；It unsintered blank will be shaped is piled into multilayer and be directly placed into sintering furnace, be sintered, be then heat-treated, obtain samarium cobalt permanent magnet body；In the present invention, it is designed using composition of raw materials and is met the requirements so that accumulating the permanent magnet half end properties obtained after multi-layer sintering, sintering efficiency is significantly improved, simultaneously, after eliminating grid tray, since there are holes for blank itself, and there is no grid blocking around blank, the phenomenon that smooth in exhaust, blank deformation, almost disappears.
Description
Technical field
The present invention relates to a kind of preparation method of permanent magnet, especially a kind of preparation method of samarium cobalt permanent magnet body.
Background technology
The magnet that can keep it magnetic for a long time claims permanent magnet.Such as natural magnetite (magnetic iron ore) and artificial magnet's (aluminium
Nickel cobalt (alloy)) etc..Samarium-cobalt permanent-magnetic material is by samarium, cobalt and other metal-rare-earth materials through proportioning, smelting at alloy, through crushing,
Manufactured a kind of magnetic material after die mould, sintering.With high energy product, extremely low temperature coefficient, very strong anticorrosive and antioxygen
The property changed, so it is widely used in aerospace, defence and military, microwave device, communication, Medical Devices, instrument, instrument, it is various
Magnetic driving device, sensor, magnetic processor, motor, magnet crane etc..
In the prior art, during the blank sintering of samarium cobalt permanent magnet body, usually blank is placed in grid tray, single
The blank quantity of sintering is few, and after being used for multiple times, the grid in grid tray easily deforms, and grid tray surrounds blank
Afterwards, it causes blank exhaust unsmooth, deformation is easy, while using old burning plate in roasting process, such as iron sheet or the scraps of paper, using iron sheet
The permanent magnet bottom crack unfilled corner that is easy to cause of mode, influence to be sintered environment, shape after paper carbonization by the way of the scraps of paper
At break flour, product quality is influenced.Meanwhile the mechanical property of samarium-cobalt permanent-magnetic material that the prior art obtains is generally poor, bending resistance is strong
Degree is only 80-120MPa, and theres are one deadly defect, be exactly it brittleness it is very big, fracture toughness is less than 2.0MPam1/
2, seriously restrict its application range.
Invention content
It is excellent it is an object of the invention to solve at least the above and/or defect, and provide at least to will be described later
Point.
In order to realize these purposes and other advantages according to the present invention, a kind of preparation side of samarium cobalt permanent magnet body is provided
Method includes the following steps：
Step 1: raw material is configured, and 23-29% containing samarium, cobalt 46-54%, iron 9-17%, copper 3-8% in the raw material, zirconium 1-
5%, the above percentage is weight ratio；
Step 2: the raw material prepared in step 1 is placed in melting in intermediate frequency electromagnetic stove, alloy molten solution is obtained；Alloy is melted
Liquid pours into ingot casting die cavity, obtains ingot casting；Ingot casting is crushed, then powder processed using forcing press, is refined, by the powder after fine grinding
By forcing press, cold isostatic press, pressure treatment shapes material twice, forms regular prism or the blank of cylinder；The forcing press
Pressure is not less than 10 tons, and cold isostatic press pressure is 200~300 megapascal；
It is directly placed into sintering furnace Step 3: unsintered blank will be shaped and be piled into multilayer, is burnt at 1200~1300 DEG C
30~60min of knot, is then heat-treated, and samarium cobalt permanent magnet body is obtained.
Preferably, in the step 3, the mode that base is piled into multilayer is stacked offset.
Preferably, in the step 3, it includes 2 heat treatment steps to be heat-treated, soaking time 1-3 hours first time,
1200-1300 degrees Celsius of temperature；Second soaking time 5-15 hours, 800-900 degrees Celsius of temperature.
Preferably, in the step 3, the process of heat treatment is：500 are warming up to the speed of 5~10 DEG C/min~
800 DEG C, 30~60min is kept the temperature, is then warming up to 1200~1300 DEG C with the speed of 10~15 DEG C/min, heat preservation 90~
Then 120min is cooled to 900~1000 DEG C with the speed of 1~5 DEG C/min, keep the temperature 3~5 hours, continues with 1~5 DEG C/min
Speed be cooled to 600~800 DEG C, keep the temperature 1~3 hour.
Preferably, in the step 2, the process of powder processed is：Broken material is put into vibrator, is pressed
It takes care of: ball=1: 5~8 ratio is added Ceramic Balls and carries out coarse crushing；By weight, 30~50 parts of coarse powder particle, binder 1 are taken
~5 parts, 0.3~0.5 part of dispersant, 1~3 part of antioxidant, 80~100 parts of ethyl alcohol be added in polytetrafluoroethylene (PTFE) ball grinders, add
Goal abrading-ball is placed on planetary ball mill, carries out ball mill mixing；Obtained ball milling material is added in sponging granulator, passes through control
Atomizing granulating technology parameter obtains being granulated powder.
Preferably, the sponging granulator selects centrifugal spray dryer；Mist projection granulating condition is：Hot-air enters
250~300 DEG C of temperature of mouth, control outlet temperature are 80~100 DEG C, 150~250m of import air quantity3/ h, outlet air quantity 250~
350m3/h；Centrifugal type atomizer rotating speed is 5000~18000r/min；Slurry pumping rate is 25~35mL/min.
Preferably, it is 1 that the dispersant, which is weight ratio,:1:2 tetramethylammonium hydroxide, 1- ethyl-3-methylimidazoles
Lactic acid, polyethylene glycol；The antioxidant is that weight ratio is 1:2:1 butane group phenol polyethenoxy ether, zinc stearate and triphen
Methanol；The binder is weight ratio 3:1:1 sodium metasilicate, high-temperature-resistant epoxy resin and polyacrylamide.
Preferably, in the step 2, the powder after fine grinding is passed through into forcing press, cold isostatic press pressure treatment twice
Glass fibre is added before the process of forming, in the powder after fine grinding to be uniformly mixed, then passes through forcing press, cold isostatic press
Pressure treatment shapes twice；The weight ratio of powder and glass fibre after the fine grinding is 10~15:1.
Preferably, the glass fibre is modified glass-fiber, and the preparation method of the modified glass-fiber is：By weight
Part is measured, takes 15~25 parts of glass fibre, 120~150 parts of 3~5wt% rare earth surface modifying agents solution that the sealing with stirring is added
In container, then the sealing container is placed in the electron accelerator of 1.5MeV, 30mA and carries out irradiation stir process 60min, mistake
Filter, drying, obtains pretreated glass fiber；Take 20~25 parts of pretreated glass fibers and 150~200 parts a concentration of 0.2~
The graphene dispersion solution of 0.8mg/mL is added in supercritical reaction apparatus, be passed through after device sealing carbon dioxide to 30~
It is stirred to react 2~3 hours, pressure release, filters under conditions of 40MPa, 100~120 DEG C of temperature, it is dry, obtain modified glass-fiber.
Preferably, the modified glass-fiber further includes following processing procedure：By weight, modified glass-fiber 10 is taken
~15 parts, 20~30 parts of polystyrene, 5~10 parts of N- vinyl imidazoles, 0.1~0.3 part of ammonium persulfate, water 100~120 is added
Part, it is stirred to react 2~3 hours under conditions of carbon dioxide to 30~40MPa, 70~80 DEG C of temperature is passed through after device sealing,
Release, filtering are eluted crude product acetone until removing the homopolymer of dereaction generation with Soxhlet extractor, and drying is changed
Property glass fibre.
The present invention includes at least following advantageous effect：
(1) in the present invention, original grid tray is eliminated in sintering process, is designed using composition of raw materials so that accumulating
The permanent magnet half end properties obtained after multi-layer sintering meet the requirements, and have significantly improved sintering efficiency, meanwhile, eliminate grid support
After disk, since there are holes for blank itself, and there is no grid blocking around blank, the phenomenon that smooth in exhaust, blank deformation almost
It disappears.
(2) in the present invention, by melting, be crushed, the processes such as powder processed, introduced in samarium-cobalt permanent-magnetic material combined with matrix it is good
It is good and with the reinforcing glass fiber compared with high-strength tenacity, significantly improve the mechanical properties such as the obdurability of permanent magnet.
Part is illustrated to embody by further advantage, target and the feature of the present invention by following, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Specific implementation mode：
With reference to embodiment, the present invention is described in further detail, to enable those skilled in the art with reference to specification
Word can be implemented according to this.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more
The presence or addition of a other elements or combinations thereof.
Embodiment 1：
A kind of preparation method of samarium cobalt permanent magnet body, includes the following steps：
Step 1: raw material is configured, containing samarium 28%, cobalt 50%, iron 12%, copper 5%, zirconium 5%, the above percentage in the raw material
Than being weight ratio；
Step 2: the raw material prepared in step 1 is placed in melting in intermediate frequency electromagnetic stove, alloy molten solution is obtained；Alloy is melted
Liquid pours into ingot casting die cavity, obtains ingot casting；Ingot casting is crushed using 5 tons of forcing presses, is crushed and then with 20 mesh with overwood
Sieve carries out sieve powder, and wood sieve sieve powder will not destroy and adsorb feed particles, while will not introduce new impurity, and fine grinding uses refiner
Carry out, by the powder after fine grinding by forcing press, cold isostatic press twice pressure treatment shape, formed regular prism or cylinder
Blank；The pressure of the forcing press is not less than 10 tons, and cold isostatic press pressure is 200 megapascal；After forcing press preliminarily forming, then make
With cold isostatic press after-treatment solid, the mechanical strength of obtained crude green body more preferably, is convenient for secondary operation, cold isostatic press be by
The material being fitted into sealing, elastic mould is placed in the container for containing liquid or gas, is applied it with one with liquid or gas
Material is pressed into entity by fixed pressure, obtains the green body of original-shape, and green body is that cylinder or regular prism shape, cylindricality are convenient for
Following process is cut, while having larger surface area, convenient for stacking and the smooth in exhaust of heap poststack；
Step 3: will shape unsintered blank stacked offset is directly placed into sintering furnace at multilayer, it is sintered at 1200 DEG C
Then 60min is heat-treated, samarium cobalt permanent magnet body is obtained；Heat treatment includes 2 heat treatment steps, and first time soaking time 1 is small
When, 1200 degrees Celsius of temperature；Second soaking time 15 hours, 800 degrees Celsius of temperature.
Embodiment 2：
A kind of preparation method of samarium cobalt permanent magnet body, includes the following steps：
Step 1: raw material is configured, containing samarium 25%, cobalt 52%, iron 10%, copper 8%, zirconium 5%, the above percentage in the raw material
Than being weight ratio；
Step 2: the raw material prepared in step 1 is placed in melting in intermediate frequency electromagnetic stove, alloy molten solution is obtained；Alloy is melted
Liquid pours into ingot casting die cavity, obtains ingot casting；Ingot casting is crushed using 5 tons of forcing presses, is crushed and then with 20 mesh with overwood
Sieve carries out sieve powder, and wood sieve sieve powder will not destroy and adsorb feed particles, while will not introduce new impurity, and fine grinding uses refiner
Carry out, by the powder after fine grinding by forcing press, cold isostatic press twice pressure treatment shape, formed regular prism or cylinder
Blank；The pressure of the forcing press is not less than 10 tons, and cold isostatic press pressure is 200 megapascal；After forcing press preliminarily forming, then make
With cold isostatic press after-treatment solid, the mechanical strength of obtained crude green body more preferably, is convenient for secondary operation, cold isostatic press be by
The material being fitted into sealing, elastic mould is placed in the container for containing liquid or gas, is applied it with one with liquid or gas
Material is pressed into entity by fixed pressure, obtains the green body of original-shape, and green body is that cylinder or regular prism shape, cylindricality are convenient for
Following process is cut, while having larger surface area, convenient for stacking and the smooth in exhaust of heap poststack；
Step 3: will shape unsintered blank stacked offset is directly placed into sintering furnace at multilayer, it is sintered at 1300 DEG C
Then 30min is heat-treated, samarium cobalt permanent magnet body is obtained；Heat treatment includes 2 heat treatment steps, and first time soaking time 3 is small
When, 1300 degrees Celsius of temperature；Second soaking time 10 hours, 900 degrees Celsius of temperature.
Embodiment 3：
In the step 3, the process of heat treatment replaces with：800 DEG C are warming up to the speed of 5 DEG C/min, keeps the temperature 60min,
Then 1300 DEG C are warming up to the speed of 10 DEG C/min, keep the temperature 120min, is then cooled to 1000 DEG C with the speed of 1 DEG C/min,
Heat preservation 5 hours continues to be cooled to 600 DEG C with the speed of 5 DEG C/min, keeps the temperature 1 hour；Each temperature can be played using temperature programming
The greatest benefit for spending section, reduces the mean temperature of whole process, reduces total energy loss, improve whole capacity usage ratio,
Meanwhile temperature programming reduces the working time of heating device at high temperature, to reduce to heating device high-temperature stability
Requirement, improve the utilization rate and reliability of heating equipment, and then keep the permanent magnet end properties being prepared further
It improves.
Remaining technical process and parameter with it is identical in embodiment 2.
Embodiment 4：
In the step 3, the process of heat treatment is：500 DEG C are warming up to the speed of 10 DEG C/min, keeps the temperature 60min, so
1200 DEG C are warming up to the speed of 15 DEG C/min afterwards, keeps the temperature 90min, is then cooled to 1000 DEG C with the speed of 5 DEG C/min, heat preservation
5 hours, continues to be cooled to 800 DEG C with the speed of 1 DEG C/min, keep the temperature 3 hours.
Remaining technical process and parameter with it is identical in embodiment 2.
Embodiment 5：
The process of the step 2 replaces with：The raw material prepared in step 1 is placed in melting in intermediate frequency electromagnetic stove, is obtained
Alloy molten solution；Alloy molten solution is poured into ingot casting die cavity, ingot casting is obtained；Ingot casting is crushed using 5 tons of forcing presses, will be crushed
Material afterwards is put into vibrator, according to material: ball=1: 5 ratio is added Ceramic Balls and carries out coarse crushing；By weight, it takes
100 parts of 50 parts of coarse powder particle, 5 parts of binder, 0.3 part of dispersant, 1 part of antioxidant, ethyl alcohol addition polytetrafluoroethylene (PTFE) ball grinders
In, ball milling ball is added and is placed on planetary ball mill, carries out ball mill mixing；Obtained ball milling material is added in sponging granulator, leads to
Cross control atomizing granulating technology parameter obtain be granulated powder, will be granulated powder by forcing press, cold isostatic press twice pressure at
Reason forming forms regular prism or the blank of cylinder；The pressure of the forcing press is not less than 10 tons, and cold isostatic press pressure is
200 megapascal；
The sponging granulator selects centrifugal spray dryer；Mist projection granulating condition is：The inlet temperature 250 of hot-air
DEG C, control outlet temperature is 100 DEG C, import air quantity 250m3/ h, outlet air quantity 250m3/h；Centrifugal type atomizer rotating speed is
10000r/min；Slurry pumping rate is 30mL/min；
The dispersant is that weight ratio is 1:1:2 tetramethylammonium hydroxide, 1- ethyl-3-methylimidazoles lactic acid, poly- second
Glycol；The antioxidant is that weight ratio is 1:2:1 butane group phenol polyethenoxy ether, zinc stearate and triphenylcarbinol；It is described
Binder is weight ratio 3:1:1 sodium metasilicate, high-temperature-resistant epoxy resin and polyacrylamide.
Remaining technical process and parameter with it is identical in embodiment 2.
Embodiment 6：
The process of the step 2 replaces with：The raw material prepared in step 1 is placed in melting in intermediate frequency electromagnetic stove, is obtained
Alloy molten solution；Alloy molten solution is poured into ingot casting die cavity, ingot casting is obtained；Ingot casting is crushed using 5 tons of forcing presses, will be crushed
Material afterwards is put into vibrator, according to material: ball=1: 8 ratio is added Ceramic Balls and carries out coarse crushing；By weight, it takes
80 parts of 45 parts of coarse powder particle, 3 parts of binder, 0.5 part of dispersant, 2 parts of antioxidant, ethyl alcohol addition polytetrafluoroethylene (PTFE) ball grinders
In, ball milling ball is added and is placed on planetary ball mill, carries out ball mill mixing；Obtained ball milling material is added in sponging granulator, leads to
Cross control atomizing granulating technology parameter obtain be granulated powder, will be granulated powder by forcing press, cold isostatic press twice pressure at
Reason forming forms regular prism or the blank of cylinder；The pressure of the forcing press is not less than 10 tons, and cold isostatic press pressure is
200 megapascal；
The sponging granulator selects centrifugal spray dryer；Mist projection granulating condition is：The inlet temperature 300 of hot-air
DEG C, control outlet temperature is 100 DEG C, import air quantity 200m3/ h, outlet air quantity 300m3/h；Centrifugal type atomizer rotating speed is
5000r/min；Slurry pumping rate is 25mL/min；
The dispersant is that weight ratio is 1:1:2 tetramethylammonium hydroxide, 1- ethyl-3-methylimidazoles lactic acid, poly- second
Glycol；The antioxidant is that weight ratio is 1:2:1 butane group phenol polyethenoxy ether, zinc stearate and triphenylcarbinol；It is described
Binder is weight ratio 3:1:1 sodium metasilicate, high-temperature-resistant epoxy resin and polyacrylamide.
Remaining technical process and parameter with it is identical in embodiment 2.
Embodiment 7：
In the step 2, the powder after fine grinding is passed through into the mistake of forcing press, cold isostatic press pressure treatment forming twice
Glass fibre is added before journey, in the powder after fine grinding to be uniformly mixed, then passes through forcing press, cold isostatic press pressure twice
Processing forming；The weight ratio of powder and glass fibre after the fine grinding is 10:1；
The glass fibre is modified glass-fiber, and the preparation method of the modified glass-fiber is：By weight, glass is taken
15 parts of glass fiber, 150 parts of 3wt% rare earth surface modifying agents solution are added in the sealing container with stirring, then hold the sealing
Device, which is placed in the electron accelerator of 1.5MeV, 30mA, carries out irradiation stir process 60min, filters, drying obtains pretreated glass
Fiber；The graphene dispersion solution of 25 parts of pretreated glass fibers and 150 parts of a concentration of 0.8mg/mL is taken, supercritical reaction is added
In device, it is stirred to react 3 hours under conditions of carbon dioxide to 40MPa, 120 DEG C of temperature is passed through after device sealing, pressure release, mistake
Filter, it is dry, obtain modified glass-fiber.
Remaining technical process and parameter with it is identical in embodiment 2.
Embodiment 8：
In the step 2, the powder after fine grinding is passed through into the mistake of forcing press, cold isostatic press pressure treatment forming twice
Glass fibre is added before journey, in the powder after fine grinding to be uniformly mixed, then passes through forcing press, cold isostatic press pressure twice
Processing forming；The weight ratio of powder and glass fibre after the fine grinding is 15:1；
The glass fibre is modified glass-fiber, and the preparation method of the modified glass-fiber is：By weight, glass is taken
25 parts of glass fiber, 150 parts of 5wt% rare earth surface modifying agents solution are added in the sealing container with stirring, then hold the sealing
Device, which is placed in the electron accelerator of 1.5MeV, 30mA, carries out irradiation stir process 60min, filters, drying obtains pretreated glass
Fiber；The graphene dispersion solution of 20~25 parts of pretreated glass fibers and 200 parts of a concentration of 0.2mg/mL is taken, is added overcritical
In reaction unit, it is stirred to react 3 hours, lets out under conditions of carbon dioxide to 40MPa, 100 DEG C of temperature is passed through after device sealing
Pressure filters, dry, obtains modified glass-fiber, by being modified processing to glass fibre, improves its mechanical property and resistance to
Warm nature energy.
Remaining technical process and parameter with it is identical in embodiment 2.
Embodiment 9：
The modified glass-fiber further includes following processing procedure：By weight, 10 parts of modified glass-fiber is taken, is added poly-
30 parts of styrene, 10 parts of N- vinyl imidazoles, 0.3 part of ammonium persulfate, 120 parts of water are passed through carbon dioxide extremely after device sealing
It is stirred to react 3 hours under conditions of 40MPa, 80 DEG C of temperature, release, filters, eluted crude product with acetone with Soxhlet extractor
It is dry until except the homopolymer that dereaction generates, obtain modified glass-fiber, by glass fibre it is further be modified at
Reason, improves its mechanical property and heat resistance.
Remaining technical process and parameter with it is identical in embodiment 8.
Embodiment 10：
The modified glass-fiber further includes following processing procedure：By weight, 15 parts of modified glass fibre is taken, polyphenyl is added
20 parts of ethylene, 5 parts of N- vinyl imidazoles, 0.2 part of ammonium persulfate, 100 parts of water are passed through carbon dioxide extremely after device sealing
It is stirred to react 3 hours under conditions of 40MPa, 80 DEG C of temperature, release, filters, eluted crude product with acetone with Soxhlet extractor
Until except the homopolymer that dereaction generates, it is dry, obtain modified glass-fiber.
Remaining technical process and parameter with it is identical in embodiment 8.
The samarium cobalt permanent magnet body prepared to Examples 1 to 10 is tested for the property, as a result as shown in Tables 1 and 2；
Table 1
Table 2
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and example shown and described herein.
Claims (10)
1. a kind of preparation method of samarium cobalt permanent magnet body, which is characterized in that include the following steps：
Step 1: raw material is configured, and 23-29% containing samarium, cobalt 46-54%, iron 9-17%, copper 3-8% in the raw material, zirconium 1-5%,
The above percentage is weight ratio；
Step 2: the raw material prepared in step 1 is placed in melting in intermediate frequency electromagnetic stove, alloy molten solution is obtained；Alloy molten solution is poured
Enter in ingot casting die cavity, obtains ingot casting；Ingot casting is crushed, then powder processed using forcing press, refines, the powder after fine grinding is led to
Pressure treatment shapes twice for excess pressure machine, cold isostatic press, forms regular prism or the blank of cylinder；The pressure of the forcing press
Not less than 10 tons, cold isostatic press pressure is 200~300 megapascal；
It is directly placed into sintering furnace Step 3: unsintered blank will be shaped and be piled into multilayer, 30 are sintered at 1200~1300 DEG C
~60min, is then heat-treated, and samarium cobalt permanent magnet body is obtained.
2. the preparation method of samarium cobalt permanent magnet body as described in claim 1, which is characterized in that in the step 3, base is piled into
The mode of multilayer is stacked offset.
3. the preparation method of samarium cobalt permanent magnet body as described in claim 1, which is characterized in that in the step 3, heat treatment packet
Include 2 heat treatment steps, soaking time 1-3 hours first time, 1200-1300 degrees Celsius of temperature；Second of soaking time 5-15
Hour, 800-900 degrees Celsius of temperature.
4. the preparation method of samarium cobalt permanent magnet body as described in claim 1, which is characterized in that in the step 3, heat treatment
Process is：500~800 DEG C are warming up to the speed of 5~10 DEG C/min, 30~60min is kept the temperature, then with 10~15 DEG C/min's
Speed is warming up to 1200~1300 DEG C, keeps the temperature 90~120min, is then cooled to 900~1000 with the speed of 1~5 DEG C/min
DEG C, 3~5 hours are kept the temperature, continues to be cooled to 600~800 DEG C with the speed of 1~5 DEG C/min, keeps the temperature 1~3 hour.
5. the preparation method of samarium cobalt permanent magnet body as described in claim 1, which is characterized in that in the step 2, the mistake of powder processed
Cheng Wei：Broken material is put into vibrator, according to material: ball=1: 5~8 ratio is added Ceramic Balls and carries out coarse powder
It is broken；By weight, take 30~50 parts of coarse powder particle, 1~5 part of binder, 0.3~0.5 part of dispersant, 1~3 part of antioxidant,
80~100 parts of ethyl alcohol is added in polytetrafluoroethylene (PTFE) ball grinder, and ball milling ball is added and is placed on planetary ball mill, carries out ball mill mixing；
Obtained ball milling material is added in sponging granulator, obtains being granulated powder by controlling atomizing granulating technology parameter.
6. the preparation method of samarium cobalt permanent magnet body as claimed in claim 5, which is characterized in that the sponging granulator selects centrifugation
Formula spray dryer；Mist projection granulating condition is：250~300 DEG C of the inlet temperature of hot-air, control outlet temperature are 80~100
DEG C, 150~250m of import air quantity3/ h, outlet 250~350m of air quantity3/h；Centrifugal type atomizer rotating speed is 5000~18000r/
min；Slurry pumping rate is 25~35mL/min.
7. the preparation method of samarium cobalt permanent magnet body as claimed in claim 5, which is characterized in that the dispersant is that weight ratio is 1:
1:2 tetramethylammonium hydroxide, 1- ethyl-3-methylimidazoles lactic acid, polyethylene glycol；The antioxidant is that weight ratio is 1:2:
1 butane group phenol polyethenoxy ether, zinc stearate and triphenylcarbinol；The binder is weight ratio 3:1:1 sodium metasilicate, resistance to height
Temperature epoxy resin and polyacrylamide.
8. the preparation method of samarium cobalt permanent magnet body as described in claim 1, which is characterized in that in the step 2, after fine grinding
Powder by forcing press, cold isostatic press twice pressure treatment forming process before, glass is added in the powder after fine grinding
Glass fiber is uniformly mixed, and then by forcing press, cold isostatic press, pressure treatment shapes twice；Powder after the fine grinding and glass
The weight ratio of glass fiber is 10~15:1.
9. the preparation method of samarium cobalt permanent magnet body as claimed in claim 8, which is characterized in that the glass fibre is modified glass
The preparation method of fiber, the modified glass-fiber is：By weight, 15~25 parts of glass fibre, 3~5wt% rare earth tables are taken
120~150 parts of surface treatment agent solution is added in the sealing container with stirring, and the sealing container is then placed in 1.5MeV, 30mA
Electron accelerator in carry out irradiation stir process 60min, filter, drying, obtain pretreated glass fiber；Take 20~25 parts it is pre-
The graphene dispersion solution of glass fibre and 150~200 parts of a concentration of 0.2~0.8mg/mL is handled, supercritical reaction dress is added
It is small it to be stirred to react 2~3 in setting, under conditions of carbon dioxide to 30~40MPa, 100~120 DEG C of temperature is passed through after device sealing
When, pressure release is filtered, dry, obtains modified glass-fiber.
10. the preparation method of samarium cobalt permanent magnet body as claimed in claim 9, which is characterized in that the modified glass-fiber also wraps
Include following processing procedure：By weight, 10~15 parts of modified glass-fiber is taken, 20~30 parts of polystyrene, N- vinyl is added
5~10 parts of imidazoles, 0.1~0.3 part of ammonium persulfate, 100~120 parts of water, be passed through after device sealing carbon dioxide to 30~
It is stirred to react 2~3 hours, release, filters under conditions of 40MPa, 70~80 DEG C of temperature, with Soxhlet extractor by crude product with third
Ketone elution is until except the homopolymer that dereaction generates, drying obtains modified glass-fiber.
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