Summary of the invention
For above-mentioned weak point of the prior art, the invention provides a kind of Sintered NdFeB magnet preparation method, directly magnetic can be sintered into the magnet of various sizes and complicated shape, not only reliable and stable, strong operability, repeatability is high, product size precision is high, and can significantly conservation cost, shorten the production cycle, enhance productivity.
The object of the invention is to be achieved through the following technical solutions:
A preparation method for Sintered NdFeB magnet, comprises the following steps:
Steps A, mixes the submicron order neodymium iron boron powder of 20 ~ 100 mass parts, the high molecular polymer powder of 3 ~ 6 mass parts mutually with the antioxidant of 1 ~ 2 mass parts, obtains mixed material powder; Wherein, described high molecular polymer is at least one in rubber, plastics or resin;
Step B, successively lays mixing material powder on the table, and successively carries out laser presintering to every layer of mixed material powder according to default magnet shape, until obtain the presintering metal base meeting default magnet shape; Wherein, the thickness of individual layer mixed material powder is 0.05 ~ 0.30mm, and the beam diameter of laser is 0.05 ~ 1.00mm;
Step C, removes the high molecular polymer in presintering metal base;
Step D, in vacuum or protective gas environment, carry out double sintering to the presintering metal base after step C process, its sintering temperature is 900 ~ 1400 DEG C, and its sintering time is 2 ~ 8 hours, thus obtains the Sintered NdFeB magnet after double sintering;
Step e, cools to the Sintered NdFeB magnet after double sintering with the furnace 15 ~ 30 DEG C, and carries out 2 ~ 8 hours annealing in process at 500 ~ 600 DEG C, namely obtains the finished product Sintered NdFeB magnet meeting default magnet shape.
Preferably; the described high molecular polymer removed in presintering metal base comprises: by the vacuumize 1 ~ 10 hour at 40 ~ 80 DEG C of presintering metal base; and with 600 ~ 800 DEG C of insulations 2 ~ 5 hours in vacuum or protective gas environment, thus remove the high molecular polymer in presintering metal base.
Preferably, in step e, the Sintered NdFeB magnet after annealing in process is magnetized, after magnetizing, namely obtain the finished product Sintered NdFeB magnet meeting default magnet shape.
Preferably, the particle size diameter of described high molecular polymer powder is 400 ~ 1 μm.
Preferably, submicron order neodymium iron boron powder refers to the neodymium iron boron powder of particle size diameter between 100nm ~ 10 μm.
As seen from the above technical solution provided by the invention, the preparation method of the Sintered NdFeB magnet that the embodiment of the present invention provides carries out plastotype by laser presintering to submicron order neodymium iron boron powder, thus obtains the presintering metal base that size and dimension meets required part requirements; Remove the high molecular polymer in presintering metal base again, and successively double sintering, annealing in process are carried out to presintering metal base after removal of impurities, thus make presintering metal base form the finished product Sintered NdFeB magnet meeting default magnet shape.Prepare silk material because this preparation method does not relate to extruding, avoid magnetic silk material in sintering process and melt accumulation, therefore this preparation method effectively can avoid the unmanageable problem of dimensional accuracy because magnetic silk material diameter excessively slightly causes.Meanwhile, because this preparation method is without the need to processing thin-walled parts, not to the process of the interior zone filling cast material of thin-walled parts, therefore this preparation method can not produce in later stage filling process and form the problem such as dead angle and thin-walled parts generation thawing.Thus, magnetic directly can be sintered into the magnet of various sizes and complicated shape by this preparation method, not only reliable and stable, strong operability, repeatability is high, product size precision is high, and can significantly conservation cost, shorten the production cycle, enhance productivity.
Embodiment
Be clearly and completely described the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on embodiments of the invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to protection scope of the present invention.
Below the preparation method of the Sintered NdFeB magnet that the embodiment of the present invention provides is described in detail.
A preparation method for Sintered NdFeB magnet, it specifically can comprise the following steps:
Steps A, mixes the submicron order neodymium iron boron powder of 20 ~ 100 mass parts, the high molecular polymer powder of 3 ~ 6 mass parts mutually with the antioxidant of 1 ~ 2 mass parts, obtains mixed material powder.
Wherein, submicron order neodymium iron boron powder refers to the neodymium iron boron powder of particle size diameter between 100nm ~ 10 μm, and in actual applications, the mean particle diameter of submicron order neodymium iron boron powder is preferably 200nm ~ 10 μm.Adopt submicron order neodymium iron boron powder not only to contribute to preparing performance Nd Fe B sintered magnet, and contribute to controlling element precision exactly in follow-up laser presintering process, thus the demand of preparation various sizes and complicated shape magnet can be met.
Particularly, high molecular polymer is at least one in rubber, plastics or resin, and its particle size diameter is preferably 400 ~ 1 μm, these high molecular polymers can play the effect be bonded together by neodymium iron boron powder in laser presintering process, and removing in high molecular polymer process and can not reacting with neodymium iron boron powder, the overall performance of neodymium iron boron powder thus can not be weakened.In the submicron order neodymium iron boron powder of 20 ~ 100 mass parts, the consumption of high molecular polymer powder preferably adopts 3 ~ 6 mass parts, and this can reach the effect be bonded together by neodymium iron boron powder; If high molecular polymer powder consumption is excessive, presintering metal body in follow-up scouring processes then can be caused defeated and dispersed, if high molecular polymer powder consumption is too small, then can cause in follow-up laser sintered process, neodymium iron boron powder is difficult to bond together, and thus can not be shaped to presintering metal body.Antioxidant can prevent submicron order neodymium iron boron powder to be oxidized in laser sintered process, thus has ensured the properties of presintering metal body; In the submicron order neodymium iron boron powder of 20 ~ 100 mass parts, the consumption of antioxidant preferably adopts 1 ~ 2 mass parts, and this can reach the effect preventing submicron order neodymium iron boron Powder Oxidation; If antioxidant consumption is excessive, then do not have necessity, the unnecessary waste of antioxidant can be caused, if antioxidant consumption is too small, then can cause sintering process sub-micron level oxidization of metal powder.
Step B, successively lays mixing material powder on the table, and successively carries out laser presintering to every layer of mixed material powder according to default magnet shape, until obtain the presintering metal base meeting default magnet shape.
Wherein, default magnet shape can be make CAD structure chart according to the size and dimension of required part, then is transferred on existing generating laser controller by this CAD structure chart, as default magnet shape; Generating laser controller can sinter the mixed material powder that workbench is successively laid according to default magnet shape.Laser presintering is a fusing high molecular polymer powder and process to neodymium iron boron powder plastotype, mainly in order to stable, reliably, process the idiosome that size and dimension meets required part requirements accurately, do not need to sinter idiosome into hard magnet, therefore the laser temperature required for laser presintering is not very high (usually at 200 ~ 400 DEG C), this generating laser making performance lower just can meet process requirements, even common 3D printer can meet temperature requirement laser sintered in this step B, therefore the equipment cost realized needed for this preparation method is very low.Because the laser sintered energy needed in the unit interval is lower, the translational speed of laser beam can also be improve, thus enhance productivity.
Particularly, the general principle of laser presintering is superposed by continuous print physical layer, and successively carry out laser sintered to increasing material thus form the presintering idiosome with 3D solid; Carrying out in laser presintering process, the scanning accuracy of laser on mixed material powder can be controlled by regulating laser beam spot sizes, and the precision of every layer of physical layer can be controlled by the thickness of individual layer mixed material powder on adjustment workbench, therefore by effectively adjusting the thickness of laser beam spot sizes and individual layer mixed material powder, the machining accuracy at each position of part can be controlled exactly.In actual applications, the thickness of individual layer mixed material powder is preferably 0.05 ~ 0.30mm, this not only contributes to the machining accuracy controlling each position of part in laser presintering process exactly, and can ensure that laser presintering process has working (machining) efficiency faster; If the thickness of individual layer mixed material powder is excessively thin, so working (machining) efficiency can be excessively slow; If the thickness of individual layer mixed material powder is blocked up, so the machining accuracy at each position of part can be difficult to control.The beam diameter of laser is preferably 0.05 ~ 1.00mm, and this contributes to the machining accuracy controlling each position of part exactly, and can ensure that laser presintering process has working (machining) efficiency faster; If the beam diameter of laser is meticulous, so working (machining) efficiency can be excessively slow; If the beam diameter of laser is excessively thick, so the machining accuracy at each position of part can be difficult to control.
Step C, removes the high molecular polymer in presintering metal base
Particularly; the high molecular polymer removed in presintering metal base can carry out in existing Muffle furnace; its concrete steps can comprise: by the vacuumize 1 ~ 10 hour at 40 ~ 80 DEG C of presintering metal base; and with 600 ~ 800 DEG C of insulations 2 ~ 5 hours in vacuum or protective gas environment, thus remove the high molecular polymer in presintering metal base.Because the fusing point of high molecular polymer is lower, therefore in insulating process, high molecular polymer can melt and remove, because the content of high molecular polymer is lower, in the process removing high molecular polymer, presintering metal base can not be out of shape, and the purity of presintering metal base can get a promotion, thus the Sintered NdFeB magnet of excellent performance can be obtained.In actual applications, this subtractive process can observe heating rate by setting heating curves, the speed of heating rate is mainly determined by neodymium iron boron powder, proportionate relationship between high molecular polymer and antioxidant, belong to empirical value, be generally 1 ~ 10 DEG C/min, but can adjust flexibly according to actual conditions.
Step D, in vacuum or protective gas environment, carry out double sintering to the presintering metal base after step C process, its sintering temperature is 900 ~ 1400 DEG C, and its sintering time is 2 ~ 8 hours, thus obtains the Sintered NdFeB magnet after double sintering.
Particularly, double sintering can adopt identical equipment (such as: Muffle furnace) with removing high molecular polymer, and this not only can save the equipment cost of this preparation method, can also avoid the damage caused in presintering metal body transfer process.The Main Function of double sintering is that to carry out final sinter molding to presintering metal base be finished product magnet, thus makes finished product Sintered NdFeB magnet meet default magnet shape requirement.
Step e, cools to the Sintered NdFeB magnet after double sintering with the furnace 15 ~ 30 DEG C, then carries out 2 ~ 8 hours annealing in process at 500 ~ 600 DEG C, namely obtains the finished product Sintered NdFeB magnet meeting default magnet shape.
Particularly, the Sintered NdFeB magnet after annealing in process is magnetized, after magnetizing, namely obtain the finished product Sintered NdFeB magnet meeting default magnet shape.
It should be noted that, the principle of the preparation method of this Sintered NdFeB magnet is as follows: this preparation method first carries out plastotype by laser presintering to submicron order neodymium iron boron powder, thus obtains the presintering metal base that size and dimension meets required part requirements; Remove the high molecular polymer in presintering metal base again, and carry out double sintering and annealing in process successively to removing the metal base after high molecular polymer, thus presintering metal base is sintered meet into the finished product Sintered NdFeB magnet of default magnet shape.Silk material is prepared because this preparation method does not relate to extruding, avoid magnetic silk material in sintering process and melt accumulation, the series of problems easily occurred when therefore this preparation method can effectively avoid the unmanageable problem of dimensional accuracy because magnetic silk material diameter excessively slightly causes and silk material to extrude.Meanwhile, because this preparation method is without the need to processing thin-walled parts, not to the process of the interior zone filling cast material of thin-walled parts, therefore this preparation method can not produce in later stage filling process and form the problem such as dead angle and thin-walled parts generation thawing.
As can be seen here, magnetic directly can be sintered into the magnet of various sizes (the thinnest reach 0.2mm) and complicated shape by this preparation method, not only reliable and stable, strong operability, repeatability is high, product size precision is high, and can significantly conservation cost, shorten the production cycle, enhance productivity.
In order to the technique effect more clearly showing technical scheme provided by the present invention and produce, be described in detail with the preparation method of several specific embodiment to Sintered NdFeB magnet provided by the present invention below.
Embodiment one
Sinter a preparation method for ring-type neodymium iron boron magnetic body, need to process that internal diameter is 8mm, external diameter is 12mm, be highly the ring-type neodymium iron boron magnetic body of 6mm, it specifically comprises the steps:
Steps A
1: by 80 mass parts particle size diameters between 100nm ~ 10 μm and mean particle diameter be the neodymium iron boron powder of 270nm, the particle size diameter of 3 mass parts is that the plastic powders of 300nm mixes mutually with the antioxidant of 1 mass parts, obtains mixed material powder.
Step B
1: making internal diameter is 8mm, external diameter is 12mm, be highly the CAD structure chart of magnet ring of 6mm, and it can be used as default magnet shape to be transferred in existing generating laser controller; Successively lay mixing material powder on the table, the thickness of individual layer mixed material powder is preferably 0.10mm, and successively laser presintering is carried out to every layer of mixed material powder according to default magnet shape, until obtain the presintering metal base meeting default magnet shape.Wherein, the laser sintered temperature that can reach is more than 240 DEG C, and the beam diameter of laser is preferably 0.1mm.
Step C
1: presintering metal base is inserted in Muffle furnace; and vacuumize 4 hours at 60 DEG C; then heat up with the speed of 7 DEG C/min in vacuum or protective gas environment, after reaching 800 DEG C, be incubated 2 hours, thus remove the plastics in presintering metal base.
Step D
1: in vacuum or protective gas environment, to step C in same Muffle furnace
1presintering metal base after process carries out double sintering, and its sintering temperature is 1160 DEG C, and its sintering time is 4 hours, thus obtains the Sintered NdFeB magnet after double sintering.
Step e
1: cool to the Sintered NdFeB magnet after double sintering with the furnace 21 DEG C, then 2 hours annealing in process are carried out at 600 DEG C, again the Sintered NdFeB magnet after annealing in process is magnetized, after magnetizing, namely obtain the finished product Sintered NdFeB magnet meeting default magnet shape.
Embodiment two
A preparation method for agglomerant font neodymium iron boron magnetic body, it specifically comprises the steps:
Steps A
2: by 90 mass parts particle size diameters between 100nm ~ 10 μm and mean particle diameter be the neodymium iron boron powder of 500nm, the particle size diameter of 4 mass parts is that the rubber powder of 500nm mixes mutually with the antioxidant of 1 mass parts, obtains mixed material powder.
Step B
2: the CAD structure chart making I shape magnet, and it can be used as default magnet shape to be transferred in existing generating laser controller; Successively lay mixing material powder on the table, the thickness of individual layer mixed material powder is preferably 0.08mm, and successively laser presintering is carried out to every layer of mixed material powder according to default magnet shape, until obtain the presintering metal base meeting default magnet shape.Wherein, the laser sintered temperature that can reach is more than 300 DEG C, and the beam diameter of laser is preferably 0.1mm.
Step C
2: presintering metal base is inserted in Muffle furnace; and vacuumize 2 hours at 80 DEG C; then heat up with the speed of 6 DEG C/min in vacuum or protective gas environment, after reaching 600 DEG C, be incubated 3 hours, thus remove the rubber in presintering metal base.
Step D
2: in vacuum or protective gas environment, to step C in same Muffle furnace
1presintering metal base after process carries out double sintering, and its sintering temperature is 1040 DEG C, and its sintering time is 5 hours, thus obtains the Sintered NdFeB magnet after double sintering.
Step e
2: cool to the Sintered NdFeB magnet after double sintering with the furnace 15 DEG C, then 3 hours annealing in process are carried out at 500 DEG C, again the Sintered NdFeB magnet after annealing in process is magnetized, after magnetizing, namely obtain the finished product Sintered NdFeB magnet meeting default magnet shape.
Embodiment three
Sinter a preparation method for complicated shape neodymium iron boron magnetic body, it specifically comprises the steps:
Steps A
3: by 70 mass parts particle size diameters between 200nm ~ 700nm and mean particle diameter be the neodymium iron boron powder of 400nm, the particle size diameter of 3 mass parts is that the rubber powder of 300nm mixes mutually with the antioxidant of 1 mass parts, obtains mixed material powder.
Step B
3: make CAD structure chart according to the complicated shape of demand, and it can be used as default magnet shape to be transferred in existing generating laser controller; Successively lay mixing material powder on the table, the thickness of individual layer mixed material powder is preferably 0.12mm, and successively laser presintering is carried out to every layer of mixed material powder according to default magnet shape, until obtain the presintering metal base meeting default magnet shape.Wherein, the laser sintered temperature that can reach is more than 300 DEG C, and the beam diameter of laser is preferably 0.1mm.
Step C
3: presintering metal base is inserted in Muffle furnace; and vacuumize 2 hours at 70 DEG C; then heat up with the speed of 6 DEG C/min in vacuum or protective gas environment, after reaching 650 DEG C, insulation carries out preliminary treatment in 4.5 hours, thus removes the rubber in presintering metal base.
Step D
3: in vacuum or protective gas environment, to step C in same Muffle furnace
1presintering metal base after process carries out double sintering, and its sintering temperature is 950 DEG C, and its sintering time is 7 hours, thus obtains the Sintered NdFeB magnet after double sintering.
Step e
3: cool to the Sintered NdFeB magnet after double sintering with the furnace 22 DEG C, then 3 hours annealing in process are carried out at 500 DEG C, again the Sintered NdFeB magnet after annealing in process is magnetized, after magnetizing, namely obtain the finished product Sintered NdFeB magnet meeting default magnet shape.
Embodiment four
Sinter a preparation method for complicated shape neodymium iron boron magnetic body, it specifically comprises the steps:
Steps A
4: by 100 mass parts particle size diameters between 200nm ~ 500nm and mean particle diameter be the neodymium iron boron powder of 300nm, the particle size diameter of 5 mass parts is that the rubber powder of 400nm mixes mutually with the antioxidant of 2 mass parts, obtains mixed material powder.
Step B
4: make CAD structure chart according to the complicated shape of demand, and it can be used as default magnet shape to be transferred in existing generating laser controller; Successively lay mixing material powder on the table, the thickness of individual layer mixed material powder is preferably 0.12mm, and successively laser presintering is carried out to every layer of mixed material powder according to default magnet shape, until obtain the presintering metal base meeting default magnet shape.Wherein, the laser sintered temperature that can reach is more than 300 DEG C, and the beam diameter of laser is preferably 0.15mm.
Step C
4: presintering metal base is inserted in Muffle furnace; and vacuumize 3 hours at 50 DEG C; then heat up with the speed of 10 DEG C/min in vacuum or protective gas environment, after reaching 700 DEG C, insulation carries out preliminary treatment in 5 hours, thus removes the rubber in presintering metal base.
Step D
4: in vacuum or protective gas environment, to step C in same Muffle furnace
1presintering metal base after process carries out double sintering, and its sintering temperature is 1200 DEG C, and its sintering time is 5 hours, thus obtains the Sintered NdFeB magnet after double sintering.
Step e
4: cool to the Sintered NdFeB magnet after double sintering with the furnace 17 DEG C, then 3 hours annealing in process are carried out at 550 DEG C, again the Sintered NdFeB magnet after annealing in process is magnetized, after magnetizing, namely obtain the finished product Sintered NdFeB magnet meeting default magnet shape.
Embodiment five
Sinter a preparation method for complicated shape neodymium iron boron magnetic body, it specifically comprises the steps:
Steps A
5: by 95 mass parts particle size diameters between 400nm ~ 700nm and mean particle diameter be the neodymium iron boron powder of 550nm, the particle size diameter of 3 mass parts is that the toner of 450nm mixes mutually with the antioxidant of 1.5 mass parts, obtains mixed material powder.
Step B
5: make CAD structure chart according to the complicated shape of demand, and it can be used as default magnet shape to be transferred in existing generating laser controller; Successively lay mixing material powder on the table, the thickness of individual layer mixed material powder is preferably 0.05mm, and successively laser presintering is carried out to every layer of mixed material powder according to default magnet shape, until obtain the presintering metal base meeting default magnet shape.Wherein, the laser sintered temperature that can reach is more than 300 DEG C, and the beam diameter of laser is preferably 0.08mm.
Step C
5: presintering metal base is inserted in Muffle furnace; and vacuumize 7 hours at 40 DEG C; then heat up with the speed of 6 DEG C/min in vacuum or protective gas environment, after reaching 600 DEG C, insulation carries out preliminary treatment in 4 hours, thus removes the resin in presintering metal base.
Step D
5: in vacuum or protective gas environment, to step C in same Muffle furnace
1presintering metal base after process carries out double sintering, and its sintering temperature is 1300 DEG C, and its sintering time is 4.5 hours, thus obtains the Sintered NdFeB magnet after double sintering.
Step e
5: cool to the Sintered NdFeB magnet after double sintering with the furnace 23 DEG C, then 4 hours annealing in process are carried out at 600 DEG C, again the Sintered NdFeB magnet after annealing in process is magnetized, after magnetizing, namely obtain the finished product Sintered NdFeB magnet meeting default magnet shape.
Embodiment six
Sinter a preparation method for complicated shape neodymium iron boron magnetic body, it specifically comprises the steps:
Steps A
6: by 50 mass parts particle size diameters between 400nm ~ 2 μm and mean particle diameter be the neodymium iron boron powder of 700nm, the particle size diameter of 3 mass parts is that the toner of 700nm mixes mutually with the antioxidant of 1 mass parts, obtains mixed material powder.
Step B
6: make CAD structure chart according to the complicated shape of demand, and it can be used as default magnet shape to be transferred in existing generating laser controller; Successively lay mixing material powder on the table, the thickness of individual layer mixed material powder is preferably 0.2mm, and successively laser presintering is carried out to every layer of mixed material powder according to default magnet shape, until obtain the presintering metal base meeting default magnet shape.Wherein, the laser sintered temperature that can reach is more than 300 DEG C, and the beam diameter of laser is preferably 0.15mm.
Step C
6: presintering metal base is inserted in Muffle furnace; and vacuumize 4 hours at 60 DEG C; then heat up with the speed of 5 DEG C/min in vacuum or protective gas environment, after reaching 700 DEG C, insulation carries out preliminary treatment in 3 hours, thus removes the resin in presintering metal base.
Step D
6: in vacuum or protective gas environment, to step C in same Muffle furnace
1presintering metal base after process carries out double sintering, and its sintering temperature is 1100 DEG C, and its sintering time is 6 hours, thus obtains the Sintered NdFeB magnet after double sintering.
Step e
6: cool to the Sintered NdFeB magnet after double sintering with the furnace 20 DEG C, then 3 hours annealing in process are carried out at 600 DEG C, again the Sintered NdFeB magnet after annealing in process is magnetized, after magnetizing, namely obtain the finished product Sintered NdFeB magnet meeting default magnet shape.
As fully visible, magnetic directly can be sintered into the magnet of various sizes and complicated shape by the embodiment of the present invention, not only reliable and stable, strong operability, repeatability is high, product size precision is high, and can significantly conservation cost, shorten the production cycle, enhance productivity.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection range of claims.