CN104575904A - NdFeB magnet formed by sintering NdFeB recycling waste and preparation method of NdFeB magnet - Google Patents
NdFeB magnet formed by sintering NdFeB recycling waste and preparation method of NdFeB magnet Download PDFInfo
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Abstract
The invention relates to an NdFeB magnet formed by sintering NdFeB recycling waste and a preparation method of the NdFeB magnet, and belongs to the technical field of a rare earth magnetic material. The NdFeB magnet is formed by a mixed material formed by the recycling waste and a prepared material by a sintering technology, and the mass percentages of the recycling waste and the prepared material are respectively 2%-50% and 50%-98%; the recycling waste is RxMyBzFe(1-x-y-z) (x=29%-32%, y=0-4% and z=0.9%-1.1%), the prepared material is RxMyBzFe(1-x-y-z) (x=29%-35%, y=0-4% and z=0.9%-1.1%), R is one or more elements selected from La, Ce, Pr, Nd, Gd, Ho and Dy, and M is one of more elements selected form Co, Al, Cu, Nb, Zr and Ga. According to the NdFeB magnet and the preparation method, disclosed by the invention, the comprehensive utilization rate and the preparation efficiency of the recycling waste are increased, and the production cost is reduced.
Description
Technical field
The present invention relates to a kind of neodymium iron boron magnetic body sintered by neodymium iron boron recovery waste material and preparation method thereof, belong to Rare-Earth Magnetic field of material technology.
Technical background
In recent years, along with the rapid expansion of neodymium iron boron magnetic body application, raw-material demand is become increasing, but because the cost of rare earth mining is higher and along with the increasing of national regulation and control dynamics, its material cost also strengthens gradually.When present price amount of increase is excessive, the price endurance of Downstream Market is more limited, portion downstream enterprise have selected the rare earth in the material such as the more cheap ferrite of use or aluminium nickel cobalt, SmCo replacement neodymium iron boron magnetic body raw material, and this brings larger unsteadiness to neodymium iron boron magnetic body market.In addition, Nd-Fe-B magnetic material fragility is high, and specification is mixed, the problem such as very easily occur unfilled corner and size is bad in the course of processing.And the learies of neodymium iron boron magnetic body after processing especially after plating is very large, the scrappage being only finished appearance and size just between 2 ~ 5%, because the otherwise requirement of client also causes that generation is bad scraps phenomenon often.Therefore the cost reducing Sintered NdFeB magnet is one of problem demanding prompt solution.
And in prior art, as Chinese patent application (notification number: CN 1076853C) discloses a kind of method that leftover bits and pieces of material prepares Nd-Fe-B series permanent magnet, the method mixes after neodymium iron boron magnetic body waste material and neodymium iron boron magnetic body virgin material being converted according to a certain percentage and mixing, adopt traditional handicraft and legacy equipment, as intermediate frequency furnace, melting obtains neodymium iron boron magnetic body.But in this approach, the mass percent of described neodymium iron boron magnetic body waste material in compound is usually below 50%, and neodymium iron boron waste material utilance is not high, and the poor-performing of the neodymium iron boron magnetic body obtained, be difficult to the application scenario meeting high request.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, provide a kind of production cost low, the neodymium iron boron magnetic body being reclaimed waste material sintering by neodymium iron boron that performance is high.
Object of the present invention is achieved through the following technical solutions, a kind of neodymium iron boron magnetic body being reclaimed waste material sintering by neodymium iron boron, described neodymium iron boron magnetic body is that the compound formed by neodymium iron boron recovery waste material and neodymium iron boron formulation is prepared from by sintering process, and the mass percent that wherein said neodymium iron boron reclaims waste material and neodymium iron boron formulation is respectively 2% ~ 50% and 50% ~ 98%; Described neodymium iron boron reclaims each composition and mass percent thereof in waste material: R
xm
yb
zfe
(1-x-y-z)(x=29-32wt%, y=0-4wt%, z=0.9-1.1wt%), R be selected from rare earth element La and Ce, Pr, Nd, Gd, Ho, Dy one or more, M is one or more in Co, Al, Cu, Nb, Zr, Ga;
In described neodymium iron boron formulation, each composition and mass percent thereof are: R
xm
yb
zfe
(1-x-y-z)(x=29-35wt%, y=0-4wt%, z=0.9-1.1wt%), R be selected from rare earth element La and Ce, Pr, Nd, Gd, Ho, Dy one or more, M is one or more in Co, Al, Cu, Nb, Zr, Ga.
Relative to prior art, the neodymium iron boron magnetic body in the application mixes with neodymium iron boron formulation by selecting suitable neodymium iron boron to reclaim waste material, and can obtain high-performance by sintering process, low weight-loss ratio, the neodymium iron boron magnetic body that temperature stability is good.And described neodymium iron boron reclaims the mass percent of waste material in compound reaches 50%, substantially increase the utilance of neodymium iron boron waste material, greatly reduce the cost of process waste material Sintered NdFeB magnet, be cost-savingly about 30%.
Another object of the present invention is that providing a kind of prepares as the above-mentioned method being reclaimed the neodymium iron boron magnetic body that waste material sinters by neodymium iron boron, and described method comprises the steps:
S1, take raw material by each composition and mass percent thereof in above-mentioned neodymium iron boron formulation, then neodymium iron boron formulation rejection tablet is made in vacuum melting; Neodymium iron boron is reclaimed waste material cleaning to obtain composition neodymium iron boron described above and reclaim waste material, then neodymium iron boron formulation rejection tablet and neodymium iron boron are reclaimed waste material and carry out that hydrogen is broken obtains neodymium iron boron formulation meal and neodymium iron boron reclaims waste material meal respectively;
S2, neodymium iron boron is reclaimed waste material meal carry out airflow milling powder, making particle mean size is that the neodymium iron boron of 20 μm-100 μm reclaims waste material fine powder, neodymium iron boron is reclaimed waste material fine powder and neodymium iron boron formulation meal is undertaken being mixed to get neodymium iron boron compound by 2-50%:50-98%;
S3, above-mentioned neodymium iron boron compound is carried out secondary gas flow mill, obtained particle mean size is the neodymium iron boron micro mist of 2 μm-4 μm;
S4, make green compact by compressing under the protection of inert gas for above-mentioned obtained neodymium iron boron micro mist, green compact are put into isostatic pressing machine pressurization, pressurize obtains blank;
S5, above-mentioned blank is placed in the first dehydrogenation of vacuum sintering furnace, is evacuated to and is not more than 0.2Pa and sinters, carry out Ageing Treatment again after having sintered, obtained neodymium iron boron magnetic body.
The present invention utilizes by selecting suitable neodymium iron boron recovery waste material and neodymium iron boron formulation mixed sintering to make neodymium iron boron magnetic body, first neodymium iron boron formulation and neodymium iron boron are reclaimed the broken obtained meal of waste material hydrogen, again neodymium iron boron is reclaimed the fine powder that waste material makes 20 μm-100 μm by airflow milling to mix by 2 ~ 50%:50-98% with neodymium iron boron formulation meal again, again compound is ground into the neodymium iron boron micro mist of 2 μm-4 μm by secondary gas flow, not only improve powder process effect, also improve the utilance of rare earth, reduce the loss of rare earth.This scope micro powder granule evenly, granularity concentration degree is better.And powder is thinner, more contribute to the lifting of magnet HCJ, if powder is too thick, then cannot incorporate crystal boundary, but powder is thinner, more easily be oxidized, cause usefulness to reduce, therefore the particle of raw material is when 2 μm of-4 μm of scopes, the control of its oxygen content is relatively easy, the cooperative effect in neodymium iron boron magnetic body between each element can be played further, thus reach greatly improve product HCJ while that the Br of product is reduced is less, reach the requirement of high-performance high-temperature coefficient.
Reclaim in the method for the neodymium iron boron magnetic body that waste material sinters in above-mentioned preparation by neodymium iron boron, as preferably, melting described in step S1 is carry out in the vacuum rapid hardening furnace of 0.3-0.8Pa in vacuum degree, and smelting temperature is 1450-1550 DEG C.
Reclaim in the method for the neodymium iron boron magnetic body that waste material sinters in above-mentioned preparation by neodymium iron boron, as preferably, when step S1 hydrogen is broken, desorption temperature is 530-550 DEG C, and dehydrogenation time is 4-5h.
Reclaim in the method for the neodymium iron boron magnetic body that waste material sinters in above-mentioned preparation by neodymium iron boron, as preferably, inert gas described in step S4 comprises argon gas, nitrogen.
Reclaim in the method for the neodymium iron boron magnetic body that waste material sinters in above-mentioned preparation by neodymium iron boron, as preferably, the pressure of step S4 isostatic pressed process is 180-200MPa, pressurize 20-40s.
Reclaim in the method for the neodymium iron boron magnetic body that waste material sinters in above-mentioned preparation by neodymium iron boron, as preferably, desorption temperature described in step S5 is 530-550 DEG C, and dehydrogenation time is 3-5h.
Reclaim in the method for the neodymium iron boron magnetic body that waste material sinters in above-mentioned preparation by neodymium iron boron, as preferably, sinter described in step S5 and comprise venting section and sintering stage.
Reclaim in the method for the neodymium iron boron magnetic body that waste material sinters in above-mentioned preparation by neodymium iron boron, as preferably, described sintering stage first with the heating rate of 5-9 DEG C/min to 500-600 DEG C, insulation 2-3h, then with the heating rate of 5-9 DEG C/min to 800-900 DEG C, insulation 2-4h, then with the heating rate of 3-5 DEG C/min to 1000-1080 DEG C, insulation 4-6h.
Reclaim in the method for the neodymium iron boron magnetic body that waste material sinters in above-mentioned preparation by neodymium iron boron, as preferably, Ageing Treatment described in step S4 is: be filled with inert gas after being completed by sintering and be quickly cooled to 600-700 DEG C, stop cooling, be evacuated to and be less than 1Pa, then be warming up to 800-900 DEG C and carry out first time Ageing Treatment, insulation 2-4h; After Ageing Treatment terminates for the first time, be filled with inert gas and be quickly cooled to 200-300 DEG C, stop cooling, be evacuated to and be less than 1Pa, be then warming up to 400-500 DEG C and carry out second time Ageing Treatment, insulation 4-6h, after second time Ageing Treatment terminates, be filled with inert gas and be quickly cooled to room temperature.
Principle all contains the diffusion of composition and the process of phase transformation in sintering and ag(e)ing process.Through constantly testing discovery, cool fast after sintering terminates, crystal boundary undergoes phase transition, the epitaxial loayer of main phase grain and the rich neodymium of crystal boundary are formed mutually mutually, but when carrying out first time timeliness, heat up the refuse of crystal boundary rich neodymium phase again, carry out composition diffusion and phase transformation, have the place overlapped each other, in like manner, timeliness and second time timeliness also have the place overlapped each other for the first time.For this phenomenon, sintering and ag(e)ing process link up by the present invention, first by the organic gas in venting section releasing pressed compact and hydrogen etc., then by triphasic sintering, 600-700 DEG C is quickly cooled to after sintering is complete, heat up again and carry out first time Ageing Treatment, then be quickly cooled to 400-500 DEG C to heat up again and carry out second time Ageing Treatment, the temperature section of control composition diffusion and phase transition process effectively, dispense overlapping place, both maintain the magnetic property of magnet excellence, turn improve efficiency.In addition, the temperature of sintering and first time, for the second time temperature of Ageing Treatment are all reasonably selected within the specific limits, if because sintering temperature is too high and the too low performance that all can affect final neodymium iron boron, can not meet the requirements of performance by the present invention.
Compared with prior art, tool of the present invention has the following advantages: mix with 50% ~ 98% ratio in 2% ~ 50% with neodymium iron boron formulation by utilizing neodymium iron boron to reclaim waste material in neodymium iron boron magnetic body of the present invention, substantially increase the comprehensive utilization ratio reclaiming waste material, greatly reduce production cost, and by specific secondary gas flow powder-grinding, effective combination of sintering and Ageing Treatment, the time of preparation method is greatly reduced while improving neodymium iron boron magnetic body performance, improve the efficiency preparing neodymium iron boron magnetic body, and greatly reduce production cost.
Embodiment
Be below specific embodiments of the invention, technical scheme of the present invention is further described, but the present invention is not limited to these embodiments.
Embodiment 1
A kind of neodymium iron boron magnetic body being reclaimed waste material sintering by neodymium iron boron, described neodymium iron boron magnetic body is that the compound formed by neodymium iron boron recovery waste material and neodymium iron boron formulation is prepared from by sintering process, and the mass percent that wherein said neodymium iron boron reclaims waste material and neodymium iron boron formulation is respectively 20% and 80%; Described neodymium iron boron reclaims each composition and mass percent thereof in waste material: (PrNd)
26gd
3dy
0.1co
0.5al
0.8cu
0.1b
0.98fe
bal; In described neodymium iron boron formulation, each composition and mass percent thereof are: (PrNd)
29gd
4co
0.5al
0.8cu
0.1b
0.98fe
bal;
The method preparing the neodymium iron boron magnetic body sintered by neodymium iron boron recovery waste material in the present embodiment comprises the steps:
Take raw material by each composition and mass percent thereof in above-mentioned neodymium iron boron formulation, be then carry out melting in the vacuum rapid hardening furnace of 0.5Pa in vacuum degree, smelting temperature is 1500 DEG C, and neodymium iron boron formulation rejection tablet is made in vacuum melting; Neodymium iron boron is reclaimed waste material cleaning and obtain composition neodymium iron boron recovery described above waste material, then neodymium iron boron formulation rejection tablet and neodymium iron boron recovery waste material are carried out respectively under the condition of 540 DEG C hydrogen broken, dehydrogenation time is 4.5h, obtains neodymium iron boron formulation meal and neodymium iron boron recovery waste material meal;
Neodymium iron boron is reclaimed waste material meal and carry out airflow milling powder, making particle mean size is that the neodymium iron boron of 60 μm reclaims waste material fine powder, neodymium iron boron is reclaimed waste material fine powder and neodymium iron boron formulation meal is undertaken being mixed to get neodymium iron boron compound by 20%:80%;
Above-mentioned neodymium iron boron compound is carried out secondary gas flow mill, and obtained particle mean size is the neodymium iron boron micro mist of 3 μm;
Make green compact by compressing under the protection of inert gas for above-mentioned obtained neodymium iron boron micro mist, green compact being put into isostatic pressing machine is that under the condition of 190MPa, pressurize 30s obtains blank at pressure, and wherein, described inert gas comprises argon gas, nitrogen;
Above-mentioned blank is placed in the first dehydrogenation of vacuum sintering furnace, desorption temperature is 540 DEG C, dehydrogenation time is 4h, is then not more than 0.2Pa sinters being evacuated in sintering furnace, and sintering comprises venting section and sintering stage, sintering stage is first with the heating rate to 560 DEG C of 6 DEG C/min, insulation 2.5h, then with the heating rate to 850 DEG C of 7 DEG C/min, insulation 3h, then with the heating rate to 1040 DEG C of 4 DEG C/min, insulation 5h; Carry out Ageing Treatment again after sintering circuit completes, described Ageing Treatment is: be filled with inert gas after being completed by sintering and be quickly cooled to 650 DEG C, stops cooling, is evacuated to and is less than 1Pa, be then warming up to 850 DEG C and carry out first time Ageing Treatment, insulation 3h; After Ageing Treatment terminates for the first time, be filled with inert gas and be quickly cooled to 250 DEG C, stop cooling, be evacuated to and be less than 1Pa, be then warming up to 450 DEG C and carry out second time Ageing Treatment, insulation 5h, after second time Ageing Treatment terminates, be filled with inert gas and be quickly cooled to room temperature, obtained neodymium iron boron magnetic body.
Embodiment 2
A kind of neodymium iron boron magnetic body being reclaimed waste material sintering by neodymium iron boron, described neodymium iron boron magnetic body is that the compound formed by neodymium iron boron recovery waste material and neodymium iron boron formulation is prepared from by sintering process, and the mass percent that wherein said neodymium iron boron reclaims waste material and neodymium iron boron formulation is respectively 30% and 70%; Described neodymium iron boron reclaims each composition and mass percent thereof in waste material: (PrNd)
26gd
3dy
0.1co
0.5al
0.8cu
0.1b
0.98fe
bal; In described neodymium iron boron formulation, each composition and mass percent thereof are: (PrNd)
29gd
3.5co
0.5al
0.8cu
0.1b
0.98fe
bal;
The method preparing the neodymium iron boron magnetic body sintered by neodymium iron boron recovery waste material in the present embodiment comprises the steps:
Take raw material by each composition and mass percent thereof in above-mentioned neodymium iron boron formulation, be then carry out melting in the vacuum rapid hardening furnace of 0.3Pa in vacuum degree, smelting temperature is 1550 DEG C, and neodymium iron boron formulation rejection tablet is made in vacuum melting; Neodymium iron boron is reclaimed waste material cleaning and obtain composition neodymium iron boron recovery described above waste material, then neodymium iron boron formulation rejection tablet and neodymium iron boron recovery waste material are carried out respectively under the condition of 530 DEG C hydrogen broken, dehydrogenation time is 5h, obtains neodymium iron boron formulation meal and neodymium iron boron recovery waste material meal;
Neodymium iron boron is reclaimed waste material meal and carry out airflow milling powder, making particle mean size is that the neodymium iron boron of 20 μm reclaims waste material fine powder, neodymium iron boron is reclaimed waste material fine powder and neodymium iron boron formulation meal is undertaken being mixed to get neodymium iron boron compound by 30%:70%;
Above-mentioned neodymium iron boron compound is carried out secondary gas flow mill, and obtained particle mean size is the neodymium iron boron micro mist of 4 μm;
Make green compact by compressing under the protection of inert gas for above-mentioned obtained neodymium iron boron micro mist, green compact being put into isostatic pressing machine is that under the condition of 180MPa, pressurize 40s obtains blank at pressure, and wherein, described inert gas comprises argon gas, nitrogen;
Above-mentioned blank is placed in the first dehydrogenation of vacuum sintering furnace, desorption temperature is 530 DEG C, dehydrogenation time is 5h, is then not more than 0.2Pa sinters being evacuated in sintering furnace, and sintering comprises venting section and sintering stage, sintering stage is first with the heating rate to 600 DEG C of 5 DEG C/min, insulation 2h, then with the heating rate to 800 DEG C of 9 DEG C/min, insulation 4h, then with the heating rate to 1080 DEG C of 3 DEG C/min, insulation 4h; Carry out Ageing Treatment again after sintering circuit completes, described Ageing Treatment is: be filled with inert gas after being completed by sintering and be quickly cooled to 700 DEG C, stops cooling, is evacuated to and is less than 1Pa, be then warming up to 800 DEG C and carry out first time Ageing Treatment, insulation 4h; After Ageing Treatment terminates for the first time, be filled with inert gas and be quickly cooled to 200 DEG C, stop cooling, be evacuated to and be less than 1Pa, be then warming up to 500 DEG C and carry out second time Ageing Treatment, insulation 4h, after second time Ageing Treatment terminates, be filled with inert gas and be quickly cooled to room temperature, obtained neodymium iron boron magnetic body.
Embodiment 3
A kind of neodymium iron boron magnetic body being reclaimed waste material sintering by neodymium iron boron, described neodymium iron boron magnetic body is that the compound formed by neodymium iron boron recovery waste material and neodymium iron boron formulation is prepared from by sintering process, and the mass percent that wherein said neodymium iron boron reclaims waste material and neodymium iron boron formulation is respectively 40% and 60%; Described neodymium iron boron reclaims each composition and mass percent thereof in waste material: (PrNd)
26gd
3d
y0.1co
0.5al
0.8cu
0.1b
0.98fe
bal; In described neodymium iron boron formulation, each composition and mass percent thereof are: (PrNd)
30gd
3co
0.5al
0.8cu
0.1b
0.98fe
bal;
The method preparing the neodymium iron boron magnetic body sintered by neodymium iron boron recovery waste material in the present embodiment comprises the steps:
Take raw material by each composition and mass percent thereof in above-mentioned neodymium iron boron formulation, be then carry out melting in the vacuum rapid hardening furnace of 0.8Pa in vacuum degree, smelting temperature is 1450 DEG C, and neodymium iron boron formulation rejection tablet is made in vacuum melting; Neodymium iron boron is reclaimed waste material cleaning and obtain composition neodymium iron boron recovery described above waste material, then neodymium iron boron formulation rejection tablet and neodymium iron boron recovery waste material are carried out respectively under the condition of 550 DEG C hydrogen broken, dehydrogenation time is 4h, obtains neodymium iron boron formulation meal and neodymium iron boron recovery waste material meal;
Neodymium iron boron is reclaimed waste material meal and carry out airflow milling powder, making particle mean size is that the neodymium iron boron of 100 μm reclaims waste material fine powder, neodymium iron boron is reclaimed waste material fine powder and neodymium iron boron formulation meal is undertaken being mixed to get neodymium iron boron compound by 40%:60%;
Above-mentioned neodymium iron boron compound is carried out secondary gas flow mill, and obtained particle mean size is the neodymium iron boron micro mist of 2 μm;
Make green compact by compressing under the protection of inert gas for above-mentioned obtained neodymium iron boron micro mist, green compact being put into isostatic pressing machine is that under the condition of 200MPa, pressurize 20s obtains blank at pressure, and wherein, described inert gas comprises argon gas, nitrogen;
Above-mentioned blank is placed in the first dehydrogenation of vacuum sintering furnace, desorption temperature is 550 DEG C, dehydrogenation time is 3h, is then not more than 0.2Pa sinters being evacuated in sintering furnace, and sintering comprises venting section and sintering stage, sintering stage is first with the heating rate to 500 DEG C of 9 DEG C/min, insulation 3h, then with the heating rate to 900 DEG C of 5 DEG C/min, insulation 2h, then with the heating rate to 1000 DEG C of 5 DEG C/min, insulation 6h; Carry out Ageing Treatment again after sintering circuit completes, described Ageing Treatment is: be filled with inert gas after being completed by sintering and be quickly cooled to 600 DEG C, stops cooling, is evacuated to and is less than 1Pa, be then warming up to 900 DEG C and carry out first time Ageing Treatment, insulation 2h; After Ageing Treatment terminates for the first time, be filled with inert gas and be quickly cooled to 300 DEG C, stop cooling, be evacuated to and be less than 1Pa, be then warming up to 400 DEG C and carry out second time Ageing Treatment, insulation 6h, after second time Ageing Treatment terminates, be filled with inert gas and be quickly cooled to room temperature, obtained neodymium iron boron magnetic body.
Comparative example 1
Neodymium iron boron is not adopted to reclaim waste material in prior art and the neodymium iron boron magnetic body obtained by common powder process and sintering circuit.
Comparative example 2
Mix by a certain percentage but the neodymium iron boron magnetic body obtained by common milling step and ordinary sinter operation with neodymium iron boron formulation as embodiment 1 adopts neodymium iron boron to reclaim waste material.
Comparative example 3
Neodymium iron boron is not adopted to reclaim waste material in prior art but method by preparing neodymium iron boron magnetic body as described in example 1 above, namely by method that secondary powder process and sintering and timeliness are effectively combined.
After pressing neodymium iron boron magnetic body surface grinding obtained in above-described embodiment 1-3 and comparative example 1-3, carry out Performance Detection, shown in the magnetic property table 1 recorded according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method.
The magnetism testing result of neodymium iron boron magnetic body obtained in table 1: embodiment 1-3 and comparative example 1-3
In sum, mix by 2-50%:50-98% with neodymium iron boron formulation by utilizing neodymium iron boron to reclaim waste material in neodymium iron boron magnetic body of the present invention, substantially increase the comprehensive utilization ratio reclaiming waste material, greatly reduce production cost, and by specific secondary gas flow powder-grinding, sintering and effective combination of Ageing Treatment, greatly reduce the time of preparation method while improving neodymium iron boron magnetic body performance, improve the efficiency preparing neodymium iron boron magnetic body, and significantly reduce production cost.
Specific embodiment described herein is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment, but can't depart from spirit of the present invention or surmount the scope that appended claims defines.
Claims (10)
1. one kind is reclaimed the neodymium iron boron magnetic body of waste material sintering by neodymium iron boron, it is characterized in that, described neodymium iron boron magnetic body is that the compound formed by neodymium iron boron recovery waste material and neodymium iron boron formulation is prepared from by sintering process, and the mass percent that wherein said neodymium iron boron reclaims waste material and neodymium iron boron formulation is respectively 2% ~ 50% and 50% ~ 98%; Described neodymium iron boron reclaims each composition and mass percent thereof in waste material: R
xm
yb
zfe
(1-x-y-z)(x=29-32wt%, y=0-4wt%, z=0.9-1.1wt%), R be selected from rare earth element La and Ce, Pr, Nd, Gd, Ho, Dy one or more, M is one or more in Co, Al, Cu, Nb, Zr, Ga;
In described neodymium iron boron formulation, each composition and mass percent thereof are: R
xm
yb
zfe
(1-x-y-z)(x=29-35wt%, y=0-4wt%, z=0.9-1.1wt%), R be selected from rare earth element La and Ce, Pr, Nd, Gd, Ho, Dy one or more, M is one or more in Co, Al, Cu, Nb, Zr, Ga.
2. prepare the method being reclaimed the neodymium iron boron magnetic body that waste material sinters as described in the appended claim 1 by neodymium iron boron, it is characterized in that, described method comprises the steps:
S1, take raw material by composition each in neodymium iron boron formulation described in claim 1 and mass percent thereof, then neodymium iron boron formulation rejection tablet is made in vacuum melting; Neodymium iron boron is reclaimed waste material cleaning to obtain composition neodymium iron boron as described in claim 1 and reclaim waste material, then neodymium iron boron formulation rejection tablet and neodymium iron boron are reclaimed waste material and carry out that hydrogen is broken obtains neodymium iron boron formulation meal and neodymium iron boron reclaims waste material meal respectively;
S2, neodymium iron boron is reclaimed waste material meal carry out airflow milling powder, making particle mean size is that the neodymium iron boron of 20 μm-100 μm reclaims waste material fine powder, neodymium iron boron is reclaimed waste material fine powder and neodymium iron boron formulation meal is undertaken being mixed to get neodymium iron boron compound by 2-50%:50-98%;
S3, above-mentioned neodymium iron boron compound is carried out secondary gas flow mill, obtained particle mean size is the neodymium iron boron micro mist of 2 μm-4 μm;
S4, make green compact by compressing under the protection of inert gas for above-mentioned obtained neodymium iron boron micro mist, green compact are put into isostatic pressing machine pressurization, pressurize obtains blank;
S5, above-mentioned blank is placed in the first dehydrogenation of vacuum sintering furnace, is evacuated to and is not more than 0.2Pa and sinters, carry out Ageing Treatment again after having sintered, obtained neodymium iron boron magnetic body.
3. prepare the method being reclaimed the neodymium iron boron magnetic body that waste material sinters by neodymium iron boron according to claim 2, it is characterized in that, melting described in step S1 is carry out in the vacuum rapid hardening furnace of 0.3-0.8Pa in vacuum degree, and smelting temperature is 1450-1550 DEG C.
4. prepare the method being reclaimed the neodymium iron boron magnetic body that waste material sinters by neodymium iron boron according to claim 2, it is characterized in that, when step S1 hydrogen is broken, desorption temperature is 530-550 DEG C, and dehydrogenation time is 4-5h.
5. prepare the method being reclaimed the neodymium iron boron magnetic body that waste material sinters by neodymium iron boron according to claim 2, it is characterized in that, inert gas described in step S4 comprises argon gas, nitrogen.
6. prepare the method being reclaimed the neodymium iron boron magnetic body that waste material sinters by neodymium iron boron according to claim 2, it is characterized in that, the pressure of step S4 isostatic pressed process is 180-200MPa, pressurize 20-40s.
7. prepare the method being reclaimed the neodymium iron boron magnetic body that waste material sinters by neodymium iron boron according to claim 2, it is characterized in that, desorption temperature described in step S5 is 530-550 DEG C, and dehydrogenation time is 3-5h.
8. prepare the method being reclaimed the neodymium iron boron magnetic body that waste material sinters by neodymium iron boron according to claim 2, it is characterized in that, described in step S5, sintering comprises venting section and sintering stage.
9. prepare the method being reclaimed the neodymium iron boron magnetic body that waste material sinters by neodymium iron boron according to claim 8, it is characterized in that, described sintering stage first with the heating rate of 5-9 DEG C/min to 500-600 DEG C, insulation 2-3h, then with the heating rate of 5-9 DEG C/min to 800-900 DEG C, insulation 2-4h, then with the heating rate of 3-5 DEG C/min to 1000-1080 DEG C, insulation 4-6h.
10. prepare the method being reclaimed the neodymium iron boron magnetic body that waste material sinters by neodymium iron boron according to claim 2, it is characterized in that, Ageing Treatment described in step S4 is: be filled with inert gas after being completed by sintering and be quickly cooled to 600-700 DEG C, stop cooling, be evacuated to and be less than 1Pa, then be warming up to 800-900 DEG C and carry out first time Ageing Treatment, insulation 2-4h; After Ageing Treatment terminates for the first time, be filled with inert gas and be quickly cooled to 200-300 DEG C, stop cooling, be evacuated to and be less than 1Pa, be then warming up to 400-500 DEG C and carry out second time Ageing Treatment, insulation 4-6h, after second time Ageing Treatment terminates, be filled with inert gas and be quickly cooled to room temperature.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050081959A1 (en) * | 2003-10-15 | 2005-04-21 | Kim Andrew S. | Method of preparing micro-structured powder for bonded magnets having high coercivity and magnet powder prepared by the same |
| CN102031445A (en) * | 2010-12-17 | 2011-04-27 | 中国科学院宁波材料技术与工程研究所 | Method for preparing high-magnetic energy product high-coercive force low-cost sintered neodymium iron boron |
| CN102211192B (en) * | 2011-06-09 | 2012-12-26 | 天津一阳磁性材料有限责任公司 | Method for preparing high-performance neodymium iron boron by using secondary recycled materials |
-
2014
- 2014-11-26 CN CN201410695948.3A patent/CN104575904A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050081959A1 (en) * | 2003-10-15 | 2005-04-21 | Kim Andrew S. | Method of preparing micro-structured powder for bonded magnets having high coercivity and magnet powder prepared by the same |
| CN102031445A (en) * | 2010-12-17 | 2011-04-27 | 中国科学院宁波材料技术与工程研究所 | Method for preparing high-magnetic energy product high-coercive force low-cost sintered neodymium iron boron |
| CN102211192B (en) * | 2011-06-09 | 2012-12-26 | 天津一阳磁性材料有限责任公司 | Method for preparing high-performance neodymium iron boron by using secondary recycled materials |
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