CN103572083A - Sintering method for neodymium iron boron magnet - Google Patents
Sintering method for neodymium iron boron magnet Download PDFInfo
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- CN103572083A CN103572083A CN201210249301.9A CN201210249301A CN103572083A CN 103572083 A CN103572083 A CN 103572083A CN 201210249301 A CN201210249301 A CN 201210249301A CN 103572083 A CN103572083 A CN 103572083A
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Abstract
The invention relates to a sintering method for a neodymium iron boron magnet. The method comprises the processes of: material stacking, first section degassing, second section degassing, sintering and tempering. The method is characterized in that: the method also includes a pre-sintering process between the second section degassing and the sintering processes. By adopting a closed sintering material box, increasing the pre-sintering process, lowering the heating and cooling speed, controlling the degassing temperature and other means, the sintering method provided by the invention reduces the escape speed of hydrogen, greatly reduces the proportion of microcracks on large neodymium iron boron blanks, improves the qualified rate of the blanks, and the blanks can have good magnetic performance.
Description
Technical field
Invention relates to a kind of permanent magnet sintering method, the particularly sintering method of rare earth permanent-magnetic material neodymium iron boron magnetic body.
Background technology
As the third generation rare earth permanent-magnetic material with Good All-around Property, neodymium iron boron magnetic body has just received sizable concern since coming out.In the evolution of more than ten years, successively developed multiple production technique, magnet performance improves constantly.Adopt the quick-fried technique of up-to-date rapid hardening (Strip Casting) hydrogenation, be aided with other means (control of powder process granularity, moulding additive etc.) and can produce high-performance magnet.The quick-fried technique of hydrogen, to improving milling efficiency and preventing from playing important effect in magnetic oxidation, has been widely used in the preparation of neodymium iron boron in addition.The quick-fried technique of hydrogen is exactly smelting neodymium-iron-boron alloy pig or gets rid of strap and inhale hydrogen process under certain hydrogen pressure, when inhaling after hydrogen finishes, carries out certain embodiments under vacuum environment.Comparatively speaking the magnet of preparing with the quick-fried technique of non-hydrogen, is used the ratio that the magnet inside of the quick-fried technique of hydrogen cracks to want high, especially prepares some larger-size bulk magnets, and it is high that its crackle proportion is more wanted.The major cause that crackle produces be use the quick-fried technique of hydrogen slug press in sintering process due under high vacuum environment in sintering oven, blank inside especially centre not dehydrogenation completely hydrogen because external and internal pressure missionary society discharges rapidly, like this at the inner tiny crack that forms of magnet.Certain embodiments is an endothermic process, need to alloy in hydrogen blasting furnace be heated and be vacuumized, and just can carry out dehydrogenation.In actual production, on the one hand owing to considering that alloy pig after the quick-fried processing of hydrogen is clayed into power, need to contain the oxidation that certain hydrogen prevents powder, on the other hand, due to the alloy pig of the quick-fried processing of hydrogen in enormous quantities or get rid of in strap certain embodiments, be heated inhomogeneous, chronic hydrogen richness could being reduced to below 500ppm, therefore the alloy pig through the quick-fried processing of hydrogen all contains certain hydrogen, has increased like this ratio of magnet generation hydrogen crackle.
At present in neodymium iron boron is produced, first to or get rid of band and carry out coarse breaking alloy pig, be broken into the alloying pellet of 200～400 microns in then, finally by ball milling or airflow milling, wear into the powdered alloy of approximately 3～5 μ m sizes, carry out, after the compression moulding of magnetic field, entering sintering oven sintering.During the central quick-fried technique of broken use hydrogen, need to inhale hydrogen and certain embodiments, in powdered alloy, also leave the hydrogen of certain content.In existing sintering process, generally have 2 sections of degasification process, at 300～500 ℃, remaining hydrogen and lubricant are carried out to dehydrogenation and degassed, proceed certain embodiments for 700～1000 ℃.When hydrogen richness is higher, in sintering process, due to sintering oven inner vacuum environment, the inner residual hydrogen of magnet, because pressure difference is overflowed rapidly, at the inner hydrogen evolution passage that produces of magnet, thereby produces tiny crack.
When in the central quick-fried rear alloy pig of broken hydrogen, hydrogen richness is higher than 2000ppm, after the powder process operation through thereafter, hydrogen richness in magnetic can not decrease, when magnetic is pressed into weight and surpasses the bulk magnet of 800g, in sintering process, the effusion meeting of hydrogen is very violent, very easily cracks, and the ratio regular meeting that produces hydrogen crackle nearly reaches 100%.Patent publication No. be CN101359529A's " degas method before a kind of Nd-Fe-B permanent magnet sintering ", it discloses the degas method before a kind of Nd-Fe-B permanent magnet sintering, the method comprise by compacting after neodymium iron boron blank be placed in sintering oven cavity, at the degassed temperature of the degassed and second segment of first paragraph, carry out first paragraph and second segment degassed, wherein said first paragraph and second segment are degassed to carry out under inert gas atmosphere.Be filled with the speed that a certain amount of rare gas element can suppress hydrogen evolution, this can reduce for small size blank the probability that it cracks, but the bulk blank role of suppressing for the magnetic of high hydrogen richness is limited, and the ratio that produces tiny crack in sintering process is still very high.
Summary of the invention
The object of the invention is to provide a kind of ratio that can reduce the neodymium iron boron bulk blank generation hydrogen crack defect that adopts high hydrogen richness magnetic compacting, improves the neodymium iron boron magnetic body sintering technology of the qualification rate of magnet.
A sintering method for neodymium iron boron magnetic body, it comprises a yard material process, first paragraph is degassed, second segment is degassed, sintering circuit and tempering process, it is characterized in that: the method also comprises a presintering operation at second segment between degassed and sintering circuit.
Preferably, described presintering operation is for to continue to vacuumize to sintering oven after the degassed insulation of second segment finishes, and is warming up to the pre-sintering temperature lower than 10～20 ℃ of sintering temperatures with the speed of 3 ℃～10 ℃; Arrive after pre-sintering temperature, be again filled with a certain amount of purity higher than 99.9% argon gas, keep furnace pressure to carry out presintering at 500～1000Pa, be incubated 1～2h.
Preferably, described code material process is put into sintering oven after the neodymium iron boron blank after compacting being piled up in a sealing sintering magazine.
Preferably, described first paragraph is degassed for sintering oven is vacuumized, and vacuum tightness reaches 10
-1after Pa, sintering oven is heated up and is heated to 300～500 ℃ of the degassed temperature of first paragraph, heat-up rate is controlled at 3 ℃～10 ℃/min, at the degassed temperature of first paragraph, is incubated 1～2h.
Preferably, described second segment is degassed is warming up to 700～1000 ℃ of the degassed temperature of second segment for the degassed insulation of first paragraph finishes rear continuation by sintering oven, heat-up rate is controlled at 3 ℃～10 ℃/min, when temperature reaches the degassed temperature of second segment, close vacuum valve, being filled with a certain amount of purity is more than 99.9% argon gas, forms the pressure of 1000～3000Pa in stove, then open vacuum valve and continue to vacuumize, and be incubated 3～6h at the degassed temperature of second segment.
Preferably, the degassed holding temperature of described second segment is preferably 5～6h, and furnace pressure is preferably 1500～2000Pa.
Preferably, described sintering circuit, for after presintering finishes, rises to sintering oven temperature the sintering temperature of 1050～1080 ℃, vacuumizes and carries out heat preservation sintering 3～5h.
Preferably, described tempering process is after heat preservation sintering finishes, and is filled with argon gas after sintering oven being cooled to below 600 ℃ with the speed of cooling of 2～5 ℃/min under vacuum condition, continues air-cooled to below 100 ℃; Continue to vacuumize and be warming up to 900～950 ℃ of insulation 1.5～3h and carry out first step temper, be then cooled to 150 ℃ and be warming up to 470～500 ℃ of insulation 4.5～6h after following and carry out second stage temper.
Because sintering method of the present invention has adopted sealing sintering magazine, increased presintering operation, reduce and heat up and cooling rate, control the means such as degassed temperature, reduced the effusion speed of hydrogen, bulk blank prepared by high hydrogen richness magnetic occurs that the ratio of tiny crack significantly reduces, and improved the qualification rate of blank, and magnetic property is good.
Embodiment
Sintering technology provided by the invention comprises: the slug press of high hydrogen richness powder is piled up in a sealing sintering magazine, after sealing magazine, put into sintering oven.Stove evacuation to be sintered reaches 10
-1after Pa, starting to heat up is heated to 300～500 ℃ of the degassed temperature of first paragraph, and heat-up rate is controlled at 3 ℃～10 ℃/min(minute).After arriving the degassed temperature of first paragraph, be incubated 1～2h(hour), then continue to be warming up to 700～1000 ℃ of the degassed temperature of second segment, heat-up rate is controlled at 3～10 ℃/min, when temperature reaches the degassed temperature of second segment, close vacuum valve, being filled with a certain amount of purity is more than 99.9% argon gas, in stove, form the pressure of 1000～3000Pa, then opening vacuum valve continues to vacuumize, insulation 3～6h, vacuumizes after insulation finishes, and continues to be warming up to the temperature lower than 10～20 ℃ of sintering temperatures with 3 ℃～10 ℃/min speed, carry out presintering, be incubated 1～2h.Arrive after pre-sintering temperature, be again filled with a certain amount of purity higher than 99.9% argon gas, keep furnace pressure at 500～1000Pa.After presintering finishes, vacuumize and carry out heat preservation sintering, heat preservation sintering 2.5～7h under the sintering temperature of 1040～1090 ℃.After below being cooled to 600 ℃ with 1～5 ℃/min of speed of cooling after end to be sintered, be filled with argon gas, and air-cooled to after below 100 ℃, continue to vacuumize and be warming up to 900～950 ℃ of insulation 1.5～3h and carry out first step temper, be then cooled to 150 ℃ and be warming up to 470～500 ℃ of insulation 4.5～6h after following and carry out second stage temper.
The present invention is different from other patent parts and is:
1) used sealing magazine as sintering magazine, sealing magazine makes the bulk magnet Speed Reduction of overflowing in sintering process.
2) reduced degassed temperature to 300～500 ℃ of first paragraph, soaking time is 1～2h, makes to concentrate and occur in the second deaeration stage in the dehydrogenation of sintering process, can not produce the violent hydrogen of putting in this stage.
3) in the second deaeration stage, 700～900 ℃ of degassed temperature, soaking time 3～6h, be preferably 5～6h, by passing into rare gas element argon gas, Controlling System internal pressure 1000～3000Pa, preferred pressure is 1500～2000Pa, reduce the effusion speed of hydrogen, that reduces hydrogen acutely emits the crackle bringing.
4) increased the stage of a pre-burning, pre-sintering temperature is lower than 10～20 ℃ of sintering temperatures, and soaking time is 1～2h, and continues to pass into a certain amount of argon gas, and maintenance furnace pressure is 500～1000Pa, continues to maintain the slow effusion speed of hydrogen.In the sintered heat insulating stage, vacuumize, the hydrogen of staying magnet inside is discharged completely, thereby reduce the ratio of crackle.
5) in whole sintering process, employing be slowly to control 3～10 ℃/min of heat-up rate, and the mode of slowly controlling 2～5 ℃/min of speed of cooling, further reduces the generation of crackle.
Below in conjunction with embodiment, illustrate the present invention.
Embodiment 1: after the quick-fried technique of hydrogen, measuring hydrogen richness is the middle flour of 2000～2100ppm, carry out 30 of the square magnets that pressing weight is 800g after airflow milling powder, blank is piled up in the airtight sintering magazine of a with closure, magazine is put into vacuum sintering furnace, and stove evacuation to be sintered reaches 10
-1after Pa, starting to heat up is heated to 300 ℃ of the degassed temperature of first paragraph, and heat-up rate is controlled at 5 ℃/min.After arriving the degassed temperature of first paragraph, be incubated 1.5h, then continue to be warming up to 700 ℃ of the degassed temperature of second segment, heat-up rate is controlled at 5 ℃/min, when temperature reaches the degassed temperature of second segment, being filled with a certain amount of purity is more than 99.9% argon gas, in stove, form the pressure of 1000Pa, insulation 3h, after insulation finishes, vacuumize, continue to be warming up to 1045 ℃ of pre-sintering temperatures with 5 ℃/min speed, carry out presintering, arrive after pre-sintering temperature, again be filled with a certain amount of purity higher than 99.9% argon gas, pressure 500Pa, insulation 1.0h.After presintering finishes, be warming up to 1065 ℃ of sintering temperatures, vacuumize and be incubated 3.5h sintering.
After below being cooled to 600 ℃ with 2 ℃/min of speed of cooling after end to be sintered, be filled with argon gas, air-cooledly after below 100 ℃, continue to vacuumize, laying equal stress on is newly warming up to 920 ℃ of insulation 2h and carries out first step temper, is then cooled to 150 ℃ and is again warming up to 480 ℃ of insulation 5.5h after following and carries out obtaining neodymium iron boron magnetic body after the temper of the second stage.
Embodiment 2: after the quick-fried technique of hydrogen, measuring hydrogen richness is the middle flour of 2000～2100ppm, carry out 30 of the square magnets that pressing weight is 1000g after airflow milling powder, blank is piled up in the airtight sintering magazine of a with closure, magazine is put into vacuum sintering furnace, and stove evacuation to be sintered reaches 10
-1after Pa, starting to heat up is heated to 400 ℃ of the degassed temperature of first paragraph, and heat-up rate is controlled at 3 ℃/min.After arriving the degassed temperature of first paragraph, be incubated 1.0h, then continue to be warming up to 800 ℃ of the degassed temperature of second segment, heat-up rate is controlled at 3 ℃/min, when temperature reaches the degassed temperature of second segment, being filled with a certain amount of purity is more than 99.9% argon gas, in stove, form the pressure of 2500Pa, insulation 4.5h, after insulation finishes, vacuumize, continue to be warming up to 1030 ℃ of pre-sintering temperatures with 3 ℃/min speed, carry out presintering, arrive after pre-sintering temperature, again be filled with a certain amount of purity higher than 99.9% argon gas, pressure 500Pa, insulation 1.5h.After presintering finishes, continue to keep this pressure to be warming up to 1050 ℃ of sintering temperatures, vacuumize and be incubated 5h sintering.
After end to be sintered, but to 600 of 3 ℃/min of speed of cooling ℃ is filled with argon gas after following, air-cooledly after below 100 ℃, continue to vacuumize, laying equal stress on is newly warming up to 930 ℃ of insulation 2.5h and carries out first step temper, is then cooled to 150 ℃ and is again warming up to 490 ℃ of insulation 6h after following and carries out obtaining neodymium iron boron magnetic body after the temper of the second stage.
Embodiment 3: after the quick-fried technique of hydrogen, measuring hydrogen richness is the middle flour of 2000～2100ppm, carry out 30 of the square magnets that pressing weight is 1500g after airflow milling powder, blank is piled up in the airtight sintering magazine of a with closure, magazine is put into vacuum sintering furnace, and stove evacuation to be sintered reaches 10
-1after Pa, starting to heat up is heated to 450 ℃ of the degassed temperature of first paragraph, and heat-up rate is controlled at 7 ℃/min.After arriving the degassed temperature of first paragraph, be incubated 1.5h, then continue to be warming up to 1000 ℃ of the degassed temperature of second segment, heat-up rate is controlled at 7 ℃/min, when temperature reaches the degassed temperature of second segment, being filled with a certain amount of purity is more than 99.9% argon gas, in stove, form the pressure of 1500Pa, insulation 5h, after insulation finishes, vacuumize, continue to be warming up to 1060 ℃ of pre-sintering temperatures with 7 ℃/min speed, carry out presintering, arrive after pre-sintering temperature, again be filled with a certain amount of purity higher than 99.9% argon gas, pressure 800Pa, insulation 1.5h.After presintering finishes, continue to keep this pressure to be warming up to 1070 ℃ of sintering temperatures, vacuumize and be incubated 3.5h sintering.
After below being cooled to 600 ℃ with 5 ℃/min of speed of cooling after end to be sintered, be filled with argon gas, air-cooledly to continuing to vacuumize after below 100 ℃ to lay equal stress on, be newly warming up to 900 ℃ of insulation 2h and carry out first step temper, be then cooled to 150 ℃ and be again warming up to 500 ℃ of insulation 5h after following and carry out obtaining neodymium iron boron magnetic body after the temper of the second stage.
Embodiment 4: after the quick-fried technique of hydrogen, measuring hydrogen richness is the middle flour of 2000～2100ppm, carry out 30 of the square magnets that pressing weight is 2000g after airflow milling powder, blank is piled up in the airtight sintering magazine of a with closure, magazine is put into vacuum sintering furnace, and stove evacuation to be sintered reaches 10
-1after Pa, starting to heat up is heated to 500 ℃ of the degassed temperature of first paragraph, and heat-up rate is controlled at 5 ℃/min.After arriving the degassed temperature of first paragraph, be incubated 1.0h, then continue to be warming up to 900 ℃ of the degassed temperature of second segment, heat-up rate is controlled at 10 ℃/min, when temperature reaches the degassed temperature of second segment, being filled with a certain amount of purity is more than 99.9% argon gas, in stove, form the pressure of 3000Pa, insulation 4h, after insulation finishes, vacuumize, continue to be warming up to 1055 ℃ of pre-sintering temperatures with 10 ℃/min speed, carry out presintering, arrive after pre-sintering temperature, again be filled with a certain amount of purity higher than 99.9% argon gas, pressure 1000Pa, insulation 2h.After presintering finishes, continue to keep this pressure to be warming up to 1065 ℃ of sintering temperatures, vacuumize and be incubated 4h sintering.
After below being cooled to 600 ℃ with 2.5 ℃/min of speed of cooling after end to be sintered, be filled with argon gas, air-cooledly after below 100 ℃, continue to vacuumize, lay equal stress on to be newly warming up to and carry out 920 ℃ of insulation 3h and carry out first step temper, be then cooled to 150 ℃ and be again warming up to 470 ℃ of insulation 5h after following and carry out obtaining neodymium iron boron magnetic body after the temper of the second stage.
Embodiment 5: after the quick-fried technique of hydrogen, measuring hydrogen richness is the middle flour of 2500～2600ppm, carry out 30 of the square magnets that pressing weight is 1000g after airflow milling powder, blank is piled up in the airtight sintering magazine of a with closure, magazine is put into vacuum sintering furnace, and stove evacuation to be sintered reaches 10
-1after Pa, starting to heat up is heated to 450 ℃ of the degassed temperature of first paragraph, and heat-up rate is controlled at 5 ℃/min.After arriving the degassed temperature of first paragraph, be incubated 2.0h, then continue to be warming up to 800 ℃ of the degassed temperature of second segment, heat-up rate is controlled at 5 ℃/min, when temperature reaches the degassed temperature of second segment, being filled with a certain amount of purity is more than 99.9% argon gas, in stove, form the pressure of 1800Pa, insulation 5.5h, after insulation finishes, vacuumize, continue to be warming up to 1070 ℃ of pre-sintering temperatures with 5 ℃/min speed, carry out presintering, arrive after pre-sintering temperature, again be filled with a certain amount of purity higher than 99.9% argon gas, pressure 700Pa, insulation 2h.After presintering finishes, continue to keep this pressure to be warming up to 1080 ℃ of sintering temperatures, vacuumize and be incubated 3h sintering.
After below being cooled to 600 ℃ with 3 ℃/min of speed of cooling after end to be sintered, be filled with argon gas, air-cooledly after below 100 ℃, continue to vacuumize, laying equal stress on is newly warming up to 950 ℃ of insulation 1.5h and carries out first step temper, is then cooled to 150 ℃ and is again warming up to 480 ℃ of insulation 6h after following and carries out obtaining neodymium iron boron magnetic body after the temper of the second stage.
Embodiment 6: after the quick-fried technique of hydrogen, measuring hydrogen richness is the middle flour of 2900～3000ppm, carry out 30 of the square magnets that pressing weight is 1000g after airflow milling powder, blank is piled up in the airtight sintering magazine of a with closure, magazine is put into vacuum sintering furnace, and stove evacuation to be sintered reaches 10
-1after Pa, starting to heat up is heated to 500 ℃ of the degassed temperature of first paragraph, and heat-up rate is controlled at 10 ℃/min.After arriving the degassed temperature of first paragraph, be incubated 1.0h, then continue to be warming up to 800 ℃ of the degassed temperature of second segment, heat-up rate is controlled at 5 ℃/min, when temperature reaches the degassed temperature of second segment, being filled with a certain amount of purity is more than 99.9% argon gas, forms the pressure of 2000Pa in stove, insulation 6h.After insulation finishes, vacuumize, continue to be warming up to 1050 ℃ of pre-sintering temperatures with 5 ℃/min speed, carry out presintering, arrive after pre-sintering temperature, be again filled with a certain amount of purity higher than 99.9% argon gas, pressure 800Pa, insulation 1.5h.After presintering finishes, be warming up to 1065 ℃ of sintering temperatures, vacuumize and carry out sintering, insulation 4.5h.
After below being cooled to 600 ℃ with 4 ℃/min of speed of cooling after end to be sintered, be filled with argon gas, air-cooledly to continuing to vacuumize after below 100 ℃, carry out 920 ℃ of insulation 2h and carry out first step temper, be then cooled to 150 ℃ and be again warming up to 480 ℃ of insulation 4.5h after following and carry out obtaining neodymium iron boron magnetic body after the temper of the second stage.
Comparative example 1: measuring hydrogen richness after the quick-fried technique of hydrogen is the middle flour of 2000～2100ppm, carries out 30 of the square magnets that pressing weight is 1000g after airflow milling powder, and blank is piled up in the can of a non-tight, and sintering oven is evacuated to 2x10
-2after Pa, with 10 ℃/min heat-up rate, being heated to 600 ℃ of the degassed temperature of first paragraph, is simultaneously 99.9% argon gas to passing into purity in sintering body of heater, and making sintering oven internal pressure is 500Pa, insulation 1h.Sintering oven is evacuated to 10 again
-1after Pa, continue to be heated to 820 ℃ with 10 ℃/min heat-up rate, be 99.9% argon gas to passing into a certain amount of purity in body of heater simultaneously, and making furnace pressure is 500Pa, carries out second segment degassed at this temperature insulation 1h.
Follow-up continuous being warming up to after 1065 ℃ of insulation 5h of the degassed end of second segment, pass into that argon gas is air-cooled to be newly warming up to 920 ℃ of insulation 2h and to carry out first step temper to continuing to vacuumize after 100 ℃ to lay equal stress on, be then cooled to 150 ℃ and be again warming up to 480 ℃ of insulation 5h after following and carry out obtaining neodymium iron boron magnetic body after the temper of the second stage.
After sintering prepared by above-described embodiment and comparative example, blank carries out the detection of internal fissure.
30 blocks of blanks after above-mentioned each embodiment and comparative example sintering are cut into the slice, thin piece that some 5mm are thick along differently-oriented directivity, if wherein there is a slice to find crackle, the blank that cuts out this slice, thin piece is designated as the blank of crackle, is considered as defective.Detecting data results lists in table 1.
Measure the magnetic property of blank after above-described embodiment and comparative example sintering simultaneously.Embodiment 1～6 and the resulting blank product of comparative example 1 sintering are randomly drawed respectively to 5 and carry out magnetism testing, adopt line cutting to draw the cylinder standard specimen of D10*10mm, the blank cracking is avoided to crackle sampling, it is carried out to the measurement of magnetic hysteresis loop.Result data is listed in table 1.
In table 1, the blank of data presentation the technical program embodiment 1～6 preparation occurs that tiny crack ratio will reduce much with respect to comparative example 1, improved the qualification rate of blank, its qualification rate reaches 80～100%, 67% qualification rate with respect to comparative example 1 significantly rises, and magnetic property is good, because of the change of technique, do not make magnetic property reduce.
Table 1 implementation column and comparative example data statistics
Claims (8)
1. a sintering method for neodymium iron boron magnetic body, it comprises a yard material process, first paragraph is degassed, second segment is degassed, sintering circuit and tempering process, it is characterized in that: the method also comprises a presintering operation at second segment between degassed and sintering circuit.
2. sintering method as claimed in claim 1, is characterized in that: described presintering operation is for to continue to vacuumize to sintering oven after the degassed insulation of second segment finishes, and is warming up to the pre-sintering temperature lower than 10～20 ℃ of sintering temperatures with the speed of 3 ℃～10 ℃; Arrive after pre-sintering temperature, be again filled with a certain amount of purity higher than 99.9% argon gas, keep furnace pressure to carry out presintering at 500～1000Pa, be incubated 1～2h.
3. sintering method as claimed in claim 1, is characterized in that: described code material process is put into sintering oven after the neodymium iron boron blank after compacting being piled up in a sealing sintering magazine.
4. sintering method as claimed in claim 1, is characterized in that: described first paragraph is degassed for sintering oven is vacuumized, and vacuum tightness reaches 10
-1after Pa, sintering oven is heated up and is heated to 300～500 ℃ of the degassed temperature of first paragraph, heat-up rate is controlled at 3 ℃～10 ℃/min, at the degassed temperature of first paragraph, is incubated 1～2h.
5. sintering method as claimed in claim 1, it is characterized in that: described second segment is degassed is warming up to 700～1000 ℃ of the degassed temperature of second segment for the degassed insulation of first paragraph finishes rear continuation by sintering oven, heat-up rate is controlled at 3 ℃～10 ℃/min, when temperature reaches the degassed temperature of second segment, close vacuum valve, being filled with a certain amount of purity is more than 99.9% argon gas, in stove, form the pressure of 1000～3000Pa, then open vacuum valve and continue to vacuumize, and be incubated 3～6h at the degassed temperature of second segment.
6. sintering method as claimed in claim 5, is characterized in that: the degassed holding temperature of described second segment is preferably 5～6h, and furnace pressure is preferably 1500～2000Pa.
7. sintering method as claimed in claim 1, is characterized in that: described sintering circuit, for after presintering finishes, rises to sintering oven temperature the sintering temperature of 1050～1080 ℃, vacuumizes and carries out heat preservation sintering 3～5h.
8. sintering method as claimed in claim 1, is characterized in that: described tempering process is after heat preservation sintering finishes, and is filled with argon gas after sintering oven being cooled to below 600 ℃ with the speed of cooling of 2～5 ℃/min under vacuum condition, continues air-cooled to below 100 ℃; Continue to vacuumize and be warming up to 900～950 ℃ of insulation 1.5～3h and carry out first step temper, be then cooled to 150 ℃ and be warming up to 470～500 ℃ of insulation 4.5～6h after following and carry out second stage temper.
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| CN103971919A (en) * | 2014-05-21 | 2014-08-06 | 北京京磁强磁材料有限公司 | Method for sintering neodymium-iron-boron magnet |
| CN103996521A (en) * | 2014-05-11 | 2014-08-20 | 沈阳中北通磁科技股份有限公司 | Vacuum presintering method and device of neodymium iron boron rare earth permanent magnet |
| CN103996520A (en) * | 2014-05-11 | 2014-08-20 | 沈阳中北通磁科技股份有限公司 | Sintering method and equipment of neodymium iron boron rare earth permanent magnet |
| CN104907560A (en) * | 2015-06-18 | 2015-09-16 | 包头金山磁材有限公司 | Sintering method capable of reducing cracks of neodymium iron boron products |
| CN105405573A (en) * | 2015-12-18 | 2016-03-16 | 上海洛克磁业有限公司 | Demagnetization method of sintered Nd-Fe-B |
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| CN106399731A (en) * | 2015-07-27 | 2017-02-15 | 三环瓦克华（北京）磁性器件有限公司 | Degassing method for producing sintered neodymium-iron-boron |
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| CN108231397A (en) * | 2018-03-12 | 2018-06-29 | 百琪达智能科技（宁波）股份有限公司 | A kind of molding sintering integrated machine of code-disc |
| CN109411225A (en) * | 2018-09-07 | 2019-03-01 | 杭州永磁集团有限公司 | A kind of preparation process of samarium-cobalt magnet |
| CN110021467A (en) * | 2018-01-10 | 2019-07-16 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of Sintered NdFeB magnet |
| CN111243806A (en) * | 2020-01-10 | 2020-06-05 | 太原科技大学 | Preparation method of high-performance sintered neodymium-iron-boron magnet |
| CN113948303A (en) * | 2021-10-20 | 2022-01-18 | 合肥工业大学 | High-yield and high-performance sintered NdFeB radiation ring and preparation method thereof |
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| CN103996520A (en) * | 2014-05-11 | 2014-08-20 | 沈阳中北通磁科技股份有限公司 | Sintering method and equipment of neodymium iron boron rare earth permanent magnet |
| CN103996521B (en) * | 2014-05-11 | 2016-05-25 | 沈阳中北通磁科技股份有限公司 | A kind of vacuum presintering method and apparatus of Fe-B rare-earth permanent magnet |
| CN103996520B (en) * | 2014-05-11 | 2016-10-05 | 沈阳中北通磁科技股份有限公司 | The sintering method of a kind of Fe-B rare-earth permanent magnet and equipment |
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| CN104907560A (en) * | 2015-06-18 | 2015-09-16 | 包头金山磁材有限公司 | Sintering method capable of reducing cracks of neodymium iron boron products |
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| CN105405573A (en) * | 2015-12-18 | 2016-03-16 | 上海洛克磁业有限公司 | Demagnetization method of sintered Nd-Fe-B |
| CN105405573B (en) * | 2015-12-18 | 2018-05-22 | 上海洛克磁业有限公司 | A kind of demagnetizing method of sintered NdFeB |
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| CN106169345A (en) * | 2016-08-29 | 2016-11-30 | 海安县建业磁材有限公司 | A kind of neodymium iron boron magnetic body and preparation method and neodymium iron boron magnetic body photo frame |
| CN106169345B (en) * | 2016-08-29 | 2018-05-01 | 海安县建业磁材有限公司 | A kind of preparation method of neodymium iron boron magnetic body |
| CN106623916A (en) * | 2016-12-28 | 2017-05-10 | 京磁新材料有限公司 | Low-temperature sintering method for preparing neodymium-iron-boron magnet |
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| CN110021467A (en) * | 2018-01-10 | 2019-07-16 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of Sintered NdFeB magnet |
| CN108231397A (en) * | 2018-03-12 | 2018-06-29 | 百琪达智能科技（宁波）股份有限公司 | A kind of molding sintering integrated machine of code-disc |
| CN109411225A (en) * | 2018-09-07 | 2019-03-01 | 杭州永磁集团有限公司 | A kind of preparation process of samarium-cobalt magnet |
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