CN103617853A - Neodymium iron boron magnetic material with good temperature stability - Google Patents
Neodymium iron boron magnetic material with good temperature stability Download PDFInfo
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- CN103617853A CN103617853A CN201310622018.0A CN201310622018A CN103617853A CN 103617853 A CN103617853 A CN 103617853A CN 201310622018 A CN201310622018 A CN 201310622018A CN 103617853 A CN103617853 A CN 103617853A
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Abstract
The invention relates to a neodymium iron boron magnetic material with good temperature stability. The neodymium iron boron magnetic material with good temperature stability is formed by mixing principal phase alloy and auxiliary phase alloy. The principal phase alloy comprises, by weight, 64.5-68.5% of iron, 1.0-1.2% of boron, 30.2-34.3% of neodymium, 0.05-0.4% of gadolinium and 0.1-0.4% of aluminum. The auxiliary phase alloy comprises, by weight, 50.8-54.2% of iron, 0.8-1.2% of boron, 18.9-21.1% of neodymium, 12.8-16.3% of zirconium, 8.9-11.1% of samarium and 0.8-1.2% of copper. By the adoption of the technical scheme, the prepared neodymium iron boron magnetic material can have good temperature stability.
Description
Technical field
The present invention relates to a kind of magnetic material and production technology thereof, neodymium-iron-boron magnetic material and production technology thereof that especially a kind of temperature stability is good.
Background technology
Neodymium-iron-boron magnetic material, as the latest result of rare earth permanent-magnetic material development, because its excellent magnetic property is able to extensive utilization.Yet, still there is many deficiencies in the sintering of the neodymium iron boron magnetic body of present stage, be embodied in, the NdFeB material that traditional handicraft sintering forms is due to sintering method and itself chemical property, cause the temperature stability of magnet material not good, thereby make it in use have inconvenience part.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of neodymium-iron-boron magnetic material and production technology thereof, and it can have the better temperature stability of more general neodymium-iron-boron magnetic material.
For solving the problems of the technologies described above, the present invention relates to the good neodymium-iron-boron magnetic material of a kind of temperature stability, it is formed by main-phase alloy and auxiliary phase alloy mixed configuration; Described main-phase alloy is configured and forms by weight percentage by following raw materials according: iron 64.5～68.5%, boron 1.0～1.2%, neodymium 30.2～34.3%, gadolinium 0.05～0.4%, aluminium 0.1～0.4%; Auxiliary phase alloy is equipped by weight percentage by following raw materials according: iron 50.8～54.2%, boron 0.8～1.2%, neodymium 18.9～21.1%, zirconium 12.8～16.3%, samarium 8.9～11.1%, copper 0.8～1.2%.
In such scheme, the gadolinium in main-phase alloy can improve by suppressing the generation of α-Fe phase the magnet performance of sintered NdFeB magnet, improves respectively magnet temperature stability by what improve rich neodymium phase simultaneously; And aluminium can improve the wetability of liquid phase and principal phase in sintering process, make grain surface more level and smooth, and can refinement main phase grain, thereby temperature stability is further improved.In auxiliary phase alloy, the samarium element of interpolation, due to himself chemical property, can effectively improve the stability of neodymium iron boron magnetic body; Zirconium can reduce the sensitiveness of neodymium iron boron magnetic body to sintering temperature, thereby improved the resistance to sintering temperature of neodymium iron boron magnetic body, and there is not the abnormal growth of crystal grain, make it obtain high energy product, simultaneous temperature stability is more good, in addition, zirconium also can make NdFeB material obtain good corrosion resistance and mechanical property; The interpolation of copper can improve Grain-Boundary Phase, increases wetability.
In the raw material of described main-phase alloy, the purity of iron, boron and aluminium is all at least 99.9%, and the purity of neodymium and gadolinium is at least 99.8%; In the raw material of described auxiliary phase alloy, the purity of iron, boron and copper is at least 99.9%, and the purity of neodymium, zirconium and samarium is at least 99.8%.
The production technology of the neodymium-iron-boron magnetic material that said temperature has good stability comprises following processing step:
1) to main-phase alloy and auxiliary phase alloy prepare burden respectively, smelting and ingot casting operation, obtain main-phase alloy ingot casting and auxiliary phase alloy ingot casting;
2) main-phase alloy ingot casting is carried out to high annealing operation;
3) main-phase alloy ingot casting and auxiliary phase alloy ingot casting are carried out respectively to the quick-fried operation of hydrogen, obtain main-phase alloy powder and auxiliary phase alloy powder;
4) main-phase alloy powder is mixed according to a certain percentage with auxiliary phase alloy powder;
5) to the mixed-powder of main-phase alloy and auxiliary phase alloy grind, moulding, sintering and heat treatment step.
Ternary sintered NdFeB magnet is mainly by three phase compositions, principal phase, boron-rich phase and rich neodymium phase.When in magnet, boron content is lower, it only has principal phase and rich neodymium phase.The percentage by volume of principal phase in magnet determined remanent magnetism and the magnetic energy product of neodymium-iron-boron magnetic material, the quantity of rich neodymium phase and its raising of favourable magnet HCJ of distributing homogeneity around principal phase, and the coercitive raising of magnet can promote the lifting of magnet temperature stability.
In the production technology of the neodymium-iron-boron magnetic material that described temperature stability is good, the row batching of main-phase alloy and auxiliary phase alloy, smelting and ingot casting operation, and the high annealing operation of main-phase alloy ingot casting is:
1) according to the percentage by weight of main-phase alloy and auxiliary phase alloy, get appropriate raw material, packed in the crucible of induction heating type vacuum smelting furnace, wherein the loading sequence of main-phase alloy is followed successively by boron, iron, gadolinium, neodymium, and metallic aluminium is positioned in the loading hopper of smelting furnace; The loading sequence of auxiliary phase alloy is followed successively by boron, zirconium, iron, samarium, copper, samarium, neodymium;
2) smelting furnace is vacuumized to processing, and raw material in stove is carried out to preheating, complete in backward smelting furnace and be filled with high purity argon, make the relative atmospheric pressure of argon pressure in stove be-0.5Mpa; Smelting furnace heating power is promoted to 18～27KW, until metal all melts in stove;
3) after metal in stove melts, add metallic aluminium; Temperature with 1600 to 1900 ℃ heats raw material in smelting furnace, carries out sufficient electromagnetic agitation simultaneously;
4) utilizing funnel that molten steel is poured into cooling thickness is that in 15 to 30mm two-sided water cooled copper mould, cooling water temperature is 15 to 30 ℃, and hydraulic pressure is 4MPa, and be 65 to 85 minutes cooling time;
5) open smelting furnace, take out ingot casting, its surface finish is smooth, and encapsulation is preserved;
6) alloy cast ingot after processing is placed in high vacuum sintering furnace, and it is vacuumized to processing, after completing, alloy cast ingot in sintering furnace is carried out to annealing in process, be heated, programming rate is 5 ℃/min, until in stove, temperature reaches 900 to 1050 ℃, and under this temperature environment, be incubated 6 to 8 hours;
7) make main-phase alloy ingot casting with stove cooling 55 to 70 minutes, its taking-up is naturally cooled to room temperature.
Smelt with ingot casting and can form the principal phase that determines magnet performance in neodymium-iron-boron magnetic material.In smelting process, alloy can be rare goes out α-Fe phase, α-Fe has not only reduced the generation quantity of principal phase in ingot casting mutually, also can produce harmful effect to operations such as follow-up grinding flour, moulding, thereby the performance of harm neodymium-iron-boron magnetic material, α-Fe meets simultaneously affects the distribution of the inner rich neodymium phase of magnet, thereby affects the temperature stability of magnet.
Adopt above-mentioned processing step, its tool has the following advantages:
1) loading sequence of main-phase alloy and auxiliary phase alloy is according to its raw material fusing point order from high to low, thereby guarantees that first the raw metal of upper end melts, and forms liquid phase, and then accelerates the thawing of its lower end raw material;
2) adopt induction heating type vacuum smelting furnace, it has, and metal inside degasifying effect is good, crystallization is fast, clean type good, can Fast Heating, and to the unconfined advantage of raw material shape;
3) before smelting, vacuumize processing, and pass into argon gas, first can avoid oxygen, carbon dioxide etc. in the interior raw material of stove and air to react; Secondly because argon gas is inert gas, it can play a protective role; Meanwhile, passing into of argon gas makes stove internal gas pressure be less than atmospheric pressure, and the fusing point of raw material in stove is decreased, and reduced process time;
4) main-phase alloy ingot casting is carried out to high annealing, can eliminate its inner α-Fe phase, promoted magnet performance and the temperature stability of ingot casting.
In the production technology of the neodymium-iron-boron magnetic material that described temperature stability is good, main-phase alloy ingot casting and auxiliary phase alloy ingot casting carry out respectively the quick-fried operation of hydrogen and are:
1) the main-phase alloy ingot casting of annealed processing and auxiliary phase alloy ingot casting are broken into respectively to fritter, make it large as far as possible at the basic material loading piece that can put into hydrogen blasting furnace, and it is inserted respectively to hydrogen blasting furnace and carry out the quick-fried processing of hydrogen;
2) hydrogen blasting furnace is vacuumized after processing, complete backward its inside and pass into high-purity hydrogen, Hydrogen Vapor Pressure remains on 2MPa;
3) treat that temperature starts to raise in hydrogen blasting furnace, to water spray in stove, to reduce temperature in stove, make temperature in hydrogen blasting furnace remain on 80 to 120 ℃, during hydrogen blasting furnace keep rotation;
4) above-mentioned steps continues, after 1 to 2 hour, to stop passing into hydrogen, and find time, and hydrogen in stove is disclosed to heating, and heating-up temperature is 450 to 780 ℃, and be 5 to 7 hours heating time, makes main-phase alloy and auxiliary phase alloy ingot casting all after hydrogen is quick-fried, become alloy powder;
5) end to be heated, adopts powder in water quench stove, and cooling water temperature is 15 to 30 ℃.
Neodymium-iron-boron magnetic material is comprised of a plurality of isolated main phase grains each other, and described crystal grain has sharp-pointed corner angle or the polyhedral at outstanding position for occupying, and corner angle or outstanding position can produce magnetic field.So the quantity of main phase grain increase the performance that is all conducive to neodymium-iron-boron magnetic material with the minimizing at its corner angle or outstanding position.
Adopt above-mentioned processing step, tool has the following advantages:
1) main-phase alloy ingot casting and auxiliary phase alloy ingot casting are broken into respectively to the maximum fragment that can pack hydrogen blasting furnace into, can reduce the infringement of Mechanical Crushing to ingot structure, thereby avoid wherein main phase grain to be damaged;
2) adopt the quick-fried technique of hydrogen, alloy cast ingot in the quick-fried process of hydrogen by along brilliant and transgranular fracture and fragmentation can reduce the infringement to ingot casting crystal grain in pulverizing process, thereby make the proportion increase of single crystal grain in magnetic, it is conducive to improve the degree of orientation of magnetic, improves the magnetic property of sintered magnet;
3) the quick-fried gained powder of hydrogen fragility is large, can save the abrasive dust time of follow-up airflow milling operation; The quick-fried technique of hydrogen can be improved the pattern of powder simultaneously, powder particle shape is more approaching circle or oval-shaped polyhedron, and the quick-fried particle size distribution of improving of hydrogen, reduces excessive and meticulous powder, thereby make its more easily processing in the operations such as follow-up moulding and sintering, be heated more even.
In the production technology of the neodymium-iron-boron magnetic material that described temperature stability is good, main-phase alloy powder and auxiliary phase alloy powder mixed processes, and the grinding of the mixed-powder of main-phase alloy and auxiliary phase alloy, moulding, sintering and heat treatment step are:
1) main-phase alloy and auxiliary phase alloy powder are sieved respectively, sieve out coarse granules more than 8 orders, to it, adopt mechanical mill broken, after fragmentation, it is mixed with fine powder, utilize batch mixer to mix 1.2 to 2.5 hours;
2) main-phase alloy mixing and auxiliary phase alloy powder are inserted to Gas grinding machine and carry out fine grinding, in grinder, Control for Oxygen Content is at 15ppm;
3) main-phase alloy powder and auxiliary mixed powder for alloy are made respectively after the fine powder of 2 to 4 μ m, by 90～98:10～2 proportioning, mixed, add after the antioxidant of 1 ‰ weight ratios and the mixture of lubricant simultaneously, mixed 1.5 to 2.5 hours; Described lubricant is mixed and is equipped by weight percentage by following raw materials according: 1～12 part of industrial lubricants, 0.3～5 part of Sodium Benzoate, 0.5～6 part of vegetable oil acid, 0.2～6 part of nitrite, 25～85 parts, water;
4) adopt Magnetic field press to carry out vertical mold pressing to said mixture, forming magnetic field Wei1.8 tesla, briquetting pressure is 3MPa, adopts afterwards isostatic pressing machine, and the mixture of processing through mold pressing is waited to static pressure, obtains slug press, isostatic pressure is 10MPa;
5) above-mentioned slug press is incubated to 45 to 68 minutes under the environment of 310 to 400 ℃, under the environment of 410 to 500 ℃, is incubated 45 to 68 minutes, under the environment of 610 to 700 ℃, be incubated 145 to 230 minutes;
6) the temperature high temperature sintering with 1080 to 1250 ℃ by the slug press through above-mentioned processing, sintering time is 167 to 256 minutes;
7) neodymium-iron-boron magnetic material after sintering is carried out to temper, first order tempering for to be incubated 95 to 145 minutes under the environment of 780～950 ℃, and second level tempering for to be incubated 165 to 195 minutes under the environment of 530～680 ℃.
In the quick-fried operation of hydrogen, the residual certain hydrogen of meeting in alloy powder, it not only can cause the cracking of product in sintering process, and can make product partially hard, and follow-up plating afterwards easy electrodeposited coating comes off, therefore tackle it, arranges hydrogen technique.
Adopt above-mentioned processing step, tool has the following advantages:
1) meal after hydrogen is quick-fried is mixed into row airflow milling with fine powder again after machine mill, and it can make alloy powder volume less, and more even, makes in subsequent forming operation powder bonding more even;
2) in sintering circuit, blank is carried out to the insulation under various temperature, it can realize row's hydrogen of blank, thereby avoids because hydrogen is got rid of the clean product generation the problems referred to above that cause;
3) lubricating oil that adopts above-mentioned formula to make, compares conventional diesel fuel lubricity oil, has cooling, corrosion-resistant effect, and its volatility is little simultaneously, and environment is not polluted;
4) after sintering, to magnet, adopt tempering process to process, can effectively improve magnet performance.
As a modification of the present invention, after being equipped with, the raw material of described main-phase alloy and auxiliary phase alloy all needs to cut off and the work of polishing, and it can be so that raw metal be convenient to weighing, and can reduce impurity.
As a modification of the present invention, vacuumizing in the smelting procedure of described main-phase alloy and auxiliary phase alloy is treated to: adopt vacuum pump to vacuumize processing to smelting furnace, in stove, vacuum degree reaches 2.5 * 10
-2after Pa, induction coil power transmission, carries out preheating to raw material in smelting furnace, and heating power is 8～12KW; Stable after changing until vacuum degree in smelting furnace, stop vacuumizing; Vacuumizing in the high annealing operation of main-phase alloy is treated to: in heating process, guarantee that vacuum degree reaches 2.5 * 10
-2pa, guarantees that in insulating process vacuum degree reaches 5.0 * 10
-2pa; Vacuumizing in the quick-fried operation of hydrogen of main-phase alloy and auxiliary phase alloy ingot casting is treated to: adopt vacuum pump to vacuumize processing to hydrogen blasting furnace, after 25 to 40 minutes duration, stop vacuumizing, and pass into nitrogen in hydrogen blasting furnace, and again vacuumize, until in hydrogen blasting furnace, vacuum degree reaches 0.2Pa.
As another kind of improvement of the present invention, described in vacuumize that to process the vacuum furnace adopting be oil-sealed rotary pump, Roots vacuum pump and three grades of pumped vacuum systems of diffusion vacuum pump.
Than prior art, tool of the present invention has the following advantages:
1) by adding the elements such as gadolinium, zirconium, samarium, the temperature stability of neodymium iron boron magnetic body is promoted to some extent, make its temperature fluctuation in the use procedure of smelting process and neodymium iron boron magnetic body more stable, thereby be beneficial to processing and use;
2) adopt pairing gold legal system for neodymium-iron-boron magnetic material, it can obtain the magnetic material higher than the magnetic property of single alloyage, and it has good corrosion resistance and stability simultaneously;
3) by main-phase alloy and auxiliary phase alloy, smelt respectively and mixed sintering, avoid main-phase alloy in smelting process, to have that α-Fe is mutually rare to be gone out, can make simultaneously rich neodymium in auxiliary phase alloy be uniformly distributed mutually with main-phase alloy in principal phase around, effectively improved the magnetic behavior of neodymium-iron-boron magnetic material;
4) the rich neodymium in auxiliary phase alloy can be realized liquid-phase sintering mutually in sintering process, realize densification sintering, simultaneously the rich neodymium crystal boundary that hands down distributes, and principal phase particle is isolated mutually, play the effect of exchange coupling, be conducive to the raising of magnet coercive force and temperature stability;
5) by techniques such as the quick-fried powder process of hydrogen, in neodymium-iron-boron magnetic material production process, avoid its performance impaired, make its product compare existing product and all make moderate progress in magnet performance and coercive force performance, promote the improvement of magnet temperature stability.
Embodiment
Below in conjunction with embodiment, further illustrate the present invention, should understand following embodiment and only for the present invention is described, is not used in and limits the scope of the invention.
Embodiment 1
The neodymium-iron-boron magnetic material that temperature stability is good, it is formed by main-phase alloy and auxiliary phase alloy mixed configuration; Described main-phase alloy is configured and forms by weight percentage by following raw materials according: iron 64.5%, boron 1.2%, neodymium 34.1%, gadolinium 0.1%, aluminium 0.1%; Auxiliary phase alloy is equipped by weight percentage by following raw materials according: iron 53.8%, boron 1.2%, neodymium 19.5%, zirconium 14.3%, samarium 10.2%, copper 1.0%.
In such scheme, the gadolinium in main-phase alloy can improve by suppressing the generation of α-Fe phase the magnet performance of sintered NdFeB magnet, improves respectively magnet temperature stability by what improve rich neodymium phase simultaneously; And aluminium can improve the wetability of liquid phase and principal phase in sintering process, make grain surface more level and smooth, and can refinement main phase grain, thereby temperature stability is further improved.In auxiliary phase alloy, the samarium element of interpolation, due to himself chemical property, can effectively improve the stability of neodymium iron boron magnetic body; Zirconium can reduce the sensitiveness of neodymium iron boron magnetic body to sintering temperature, thereby improved the resistance to sintering temperature of neodymium iron boron magnetic body, and there is not the abnormal growth of crystal grain, make it obtain high energy product, simultaneous temperature stability is more good, in addition, zirconium also can make NdFeB material obtain good corrosion resistance and mechanical property; The interpolation of copper can improve Grain-Boundary Phase, increases wetability.
In the raw material of described main-phase alloy, the purity of iron is 99.99%.The purity of boron and aluminium is 99.9%, and the purity of neodymium and gadolinium is 99.8%; In the raw material of described auxiliary phase alloy, the purity of iron is 99.99%, and the purity of boron and copper is 99.9%, and the purity of neodymium, zirconium and samarium is 99.8%.
The production technology of the neodymium-iron-boron magnetic material that said temperature has good stability comprises following processing step:
1) to main-phase alloy and auxiliary phase alloy prepare burden respectively, smelting and ingot casting operation, obtain main-phase alloy ingot casting and auxiliary phase alloy ingot casting;
2) main-phase alloy ingot casting is carried out to high annealing operation;
3) main-phase alloy ingot casting and auxiliary phase alloy ingot casting are carried out respectively to the quick-fried operation of hydrogen, obtain main-phase alloy powder and auxiliary phase alloy powder;
4) main-phase alloy powder is mixed according to a certain percentage with auxiliary phase alloy powder;
5) to the mixed-powder of main-phase alloy and auxiliary phase alloy grind, moulding, sintering and heat treatment step.
Ternary sintered NdFeB magnet is mainly by three phase compositions, principal phase, boron-rich phase and rich neodymium phase.When in magnet, boron content is lower, it only has principal phase and rich neodymium phase.The percentage by volume of principal phase in magnet determined remanent magnetism and the magnetic energy product of neodymium-iron-boron magnetic material, the quantity of rich neodymium phase and its raising of favourable magnet HCJ of distributing homogeneity around principal phase, and the coercitive raising of magnet can promote the lifting of magnet temperature stability.
In the production technology of the neodymium-iron-boron magnetic material that described temperature stability is good, the row batching of main-phase alloy and auxiliary phase alloy, smelting and ingot casting operation, and the high annealing operation of main-phase alloy ingot casting is:
1) according to the percentage by weight of main-phase alloy and auxiliary phase alloy, get appropriate raw material, packed in the crucible of induction heating type vacuum smelting furnace, wherein the loading sequence of main-phase alloy is followed successively by boron, iron, gadolinium, neodymium, and metallic aluminium is positioned in the loading hopper of smelting furnace; The loading sequence of auxiliary phase alloy is followed successively by boron, zirconium, iron, samarium, copper, samarium, neodymium;
2) smelting furnace is vacuumized to processing, and raw material in stove is carried out to preheating, complete in backward smelting furnace and be filled with high purity argon, make the relative atmospheric pressure of argon pressure in stove be-0.5Mpa; Smelting furnace heating power is promoted to 18～27KW, until metal all melts in stove;
3) after metal in stove melts, add metallic aluminium; With the temperature of 1600 ℃, raw material in smelting furnace is heated, carry out sufficient electromagnetic agitation simultaneously;
4) utilize funnel that molten steel is poured in the two-sided water cooled copper mould that cooling thickness is 15 mm, cooling water temperature is 30 ℃, and hydraulic pressure is 4MPa, and be 65 minutes cooling time;
5) open smelting furnace, take out ingot casting, its surface finish is smooth, and encapsulation is preserved;
6) alloy cast ingot after processing is placed in high vacuum sintering furnace, and it is vacuumized to processing, after completing, alloy cast ingot in sintering furnace is carried out to annealing in process, be heated, programming rate is 5 ℃/min, until temperature reaches 900 ℃ in stove, and is incubated 8 hours under this temperature environment;
7) make main-phase alloy ingot casting with stove cooling 55 minutes, its taking-up is naturally cooled to room temperature.
Smelt with ingot casting and can form the principal phase that determines magnet performance in neodymium-iron-boron magnetic material.In smelting process, alloy can be rare goes out α-Fe phase, α-Fe has not only reduced the generation quantity of principal phase in ingot casting mutually, also can produce harmful effect to operations such as follow-up grinding flour, moulding, thereby the performance of harm neodymium-iron-boron magnetic material, α-Fe meets simultaneously affects the distribution of the inner rich neodymium phase of magnet, thereby affects the temperature stability of magnet.
Adopt above-mentioned processing step, its tool has the following advantages:
1) loading sequence of main-phase alloy and auxiliary phase alloy is according to its raw material fusing point order from high to low, thereby guarantees that first the raw metal of upper end melts, and forms liquid phase, and then accelerates the thawing of its lower end raw material;
2) adopt induction heating type vacuum smelting furnace, it has, and metal inside degasifying effect is good, crystallization is fast, clean type good, can Fast Heating, and to the unconfined advantage of raw material shape;
3) before smelting, vacuumize processing, and pass into argon gas, first can avoid oxygen, carbon dioxide etc. in the interior raw material of stove and air to react; Secondly because argon gas is inert gas, it can play a protective role; Meanwhile, passing into of argon gas makes stove internal gas pressure be less than atmospheric pressure, and the fusing point of raw material in stove is decreased, and reduced process time;
4) main-phase alloy ingot casting is carried out to high annealing, can eliminate its inner α-Fe phase, promoted magnet performance and the temperature stability of ingot casting.
In the production technology of the neodymium-iron-boron magnetic material that described temperature stability is good, main-phase alloy ingot casting and auxiliary phase alloy ingot casting carry out respectively the quick-fried operation of hydrogen and are:
1) the main-phase alloy ingot casting of annealed processing and auxiliary phase alloy ingot casting are broken into respectively to fritter, make it large as far as possible at the basic material loading piece that can put into hydrogen blasting furnace, and it is inserted respectively to hydrogen blasting furnace and carry out the quick-fried processing of hydrogen;
2) hydrogen blasting furnace is vacuumized after processing, complete backward its inside and pass into high-purity hydrogen, Hydrogen Vapor Pressure remains on 2MPa;
3) treat that temperature starts to raise in hydrogen blasting furnace, to water spray in stove, to reduce temperature in stove, make temperature in hydrogen blasting furnace remain on 80 ℃, during hydrogen blasting furnace keep rotation;
4) above-mentioned steps continues, after 1 hour, to stop passing into hydrogen, and find time, and hydrogen in stove is disclosed to heating, and heating-up temperature is 450 ℃, and be 7 hours heating time, makes main-phase alloy and auxiliary phase alloy ingot casting all after hydrogen is quick-fried, become alloy powder;
5) end to be heated, adopts powder in water quench stove, and cooling water temperature is 30 ℃.
Neodymium-iron-boron magnetic material is comprised of a plurality of isolated main phase grains each other, and described crystal grain has sharp-pointed corner angle or the polyhedral at outstanding position for occupying, and corner angle or outstanding position can produce magnetic field.So the quantity of main phase grain increase the performance that is all conducive to neodymium-iron-boron magnetic material with the minimizing at its corner angle or outstanding position.
Adopt above-mentioned processing step, tool has the following advantages:
1) main-phase alloy ingot casting and auxiliary phase alloy ingot casting are broken into respectively to the maximum fragment that can pack hydrogen blasting furnace into, can reduce the infringement of Mechanical Crushing to ingot structure, thereby avoid wherein main phase grain to be damaged;
2) adopt the quick-fried technique of hydrogen, alloy cast ingot in the quick-fried process of hydrogen by along brilliant and transgranular fracture and fragmentation can reduce the infringement to ingot casting crystal grain in pulverizing process, thereby make the proportion increase of single crystal grain in magnetic, it is conducive to improve the degree of orientation of magnetic, improves the magnetic property of sintered magnet;
3) the quick-fried gained powder of hydrogen fragility is large, can save the abrasive dust time of follow-up airflow milling operation; The quick-fried technique of hydrogen can be improved the pattern of powder simultaneously, powder particle shape is more approaching circle or oval-shaped polyhedron, and the quick-fried particle size distribution of improving of hydrogen, reduces excessive and meticulous powder, thereby make its more easily processing in the operations such as follow-up moulding and sintering, be heated more even.
In the production technology of the neodymium-iron-boron magnetic material that described temperature stability is good, main-phase alloy powder and auxiliary phase alloy powder mixed processes, and the grinding of the mixed-powder of main-phase alloy and auxiliary phase alloy, moulding, sintering and heat treatment step are:
1) main-phase alloy and auxiliary phase alloy powder are sieved respectively, sieve out coarse granules more than 8 orders, to it, adopt mechanical mill broken, after fragmentation, it is mixed with fine powder, utilize batch mixer to mix 1.2 hours;
2) main-phase alloy mixing and auxiliary phase alloy powder are inserted to Gas grinding machine and carry out fine grinding, in grinder, Control for Oxygen Content is at 15ppm;
3) main-phase alloy powder and auxiliary mixed powder for alloy are made respectively after the fine powder of 2 μ m, by 90～98:10～2 proportioning, mixed, add after the antioxidant of 1 ‰ weight ratios and the mixture of lubricant simultaneously, mixed 1.5 hours; Described lubricant is mixed and is equipped by weight percentage by following raw materials according: 8 parts of industrial lubricants, 5 parts of Sodium Benzoates, 5 parts of vegetable oil acids, 6 parts of nitrite, 76 parts, water;
4) adopt Magnetic field press to carry out vertical mold pressing to said mixture, forming magnetic field Wei1.8 tesla, briquetting pressure is 3MPa, adopts afterwards isostatic pressing machine, and the mixture of processing through mold pressing is waited to static pressure, obtains slug press, isostatic pressure is 10MPa;
5) above-mentioned slug press is incubated to 68 minutes under the environment of 310 ℃, under the environment of 500 ℃, is incubated 68 minutes, under the environment of 700 ℃, be incubated 230 minutes;
6) the temperature high temperature sintering with 1080 ℃ by the slug press through above-mentioned processing, sintering time is 167 minutes;
7) neodymium-iron-boron magnetic material after sintering is carried out to temper, first order tempering for to be incubated 145 minutes under the environment of 780 ℃, and second level tempering for to be incubated 195 minutes under the environment of 530 ℃.
In the quick-fried operation of hydrogen, the residual certain hydrogen of meeting in alloy powder, it not only can cause the cracking of product in sintering process, and can make product partially hard, and follow-up plating afterwards easy electrodeposited coating comes off, therefore tackle it, arranges hydrogen technique.
Adopt above-mentioned processing step, tool has the following advantages:
1) meal after hydrogen is quick-fried is mixed into row airflow milling with fine powder again after machine mill, and it can make alloy powder volume less, and more even, makes in subsequent forming operation powder bonding more even;
2) in sintering circuit, blank is carried out to the insulation under various temperature, it can realize row's hydrogen of blank, thereby avoids because hydrogen is got rid of the clean product generation the problems referred to above that cause;
3) lubricating oil that adopts above-mentioned formula to make, compares conventional diesel fuel lubricity oil, has cooling, corrosion-resistant effect, and its volatility is little simultaneously, and environment is not polluted;
4) after sintering, to magnet, adopt tempering process to process, can effectively improve magnet performance.
As a modification of the present invention, after being equipped with, the raw material of described main-phase alloy and auxiliary phase alloy all needs to cut off and the work of polishing, and it can be so that raw metal be convenient to weighing, and can reduce impurity.
As a modification of the present invention, vacuumizing in the smelting procedure of described main-phase alloy and auxiliary phase alloy is treated to: adopt vacuum pump to vacuumize processing to smelting furnace, in stove, vacuum degree reaches 2.5 * 10
-2after Pa, induction coil power transmission, carries out preheating to raw material in smelting furnace, and heating power is 8 KW; Stable after changing until vacuum degree in smelting furnace, stop vacuumizing; Vacuumizing in the high annealing operation of main-phase alloy is treated to: in heating process, guarantee that vacuum degree reaches 2.5 * 10
-2pa, guarantees that in insulating process vacuum degree reaches 5.0 * 10
-2pa; Vacuumizing in the quick-fried operation of hydrogen of main-phase alloy and auxiliary phase alloy ingot casting is treated to: adopt vacuum pump to vacuumize processing to hydrogen blasting furnace, after 25 minutes duration, stop vacuumizing, and pass into nitrogen in hydrogen blasting furnace, and again vacuumize, until in hydrogen blasting furnace, vacuum degree reaches 0.2Pa.
As another kind of improvement of the present invention, described in vacuumize that to process the vacuum furnace adopting be oil-sealed rotary pump, Roots vacuum pump and three grades of pumped vacuum systems of diffusion vacuum pump.
Than prior art, tool of the present invention has the following advantages:
1) by adding the elements such as gadolinium, zirconium, samarium, the temperature stability of neodymium iron boron magnetic body is promoted to some extent, make its temperature fluctuation in the use procedure of smelting process and neodymium iron boron magnetic body more stable, thereby be beneficial to processing and use;
2) adopt pairing gold legal system for neodymium-iron-boron magnetic material, it can obtain the magnetic material higher than the magnetic property of single alloyage, and it has good corrosion resistance and stability simultaneously;
3) by main-phase alloy and auxiliary phase alloy, smelt respectively and mixed sintering, avoid main-phase alloy in smelting process, to have that α-Fe is mutually rare to be gone out, can make simultaneously rich neodymium in auxiliary phase alloy be uniformly distributed mutually with main-phase alloy in principal phase around, effectively improved the magnetic behavior of neodymium-iron-boron magnetic material;
4) the rich neodymium in auxiliary phase alloy can be realized liquid-phase sintering mutually in sintering process, realize densification sintering, simultaneously the rich neodymium crystal boundary that hands down distributes, and principal phase particle is isolated mutually, play the effect of exchange coupling, be conducive to the raising of magnet coercive force and temperature stability;
5) by techniques such as the quick-fried powder process of hydrogen, in neodymium-iron-boron magnetic material production process, avoid its performance impaired, make its product compare existing product and all make moderate progress in magnet performance and coercive force performance, promote the improvement of magnet temperature stability.
Embodiment 2
The neodymium-iron-boron magnetic material that temperature stability is good, it is formed by main-phase alloy and auxiliary phase alloy mixed configuration; Described main-phase alloy is configured and forms by weight percentage by following raw materials according: iron 68.2%, boron 1.2%, neodymium 30.2%, gadolinium 0.2%, aluminium 0.2%; Auxiliary phase alloy is equipped by weight percentage by following raw materials according: iron 54.2%, boron 0.8%, neodymium 20.2%, zirconium 13.4%, samarium 10.6%, copper 0.8%.
In such scheme, the gadolinium in main-phase alloy can improve by suppressing the generation of α-Fe phase the magnet performance of sintered NdFeB magnet, improves respectively magnet temperature stability by what improve rich neodymium phase simultaneously; And aluminium can improve the wetability of liquid phase and principal phase in sintering process, make grain surface more level and smooth, and can refinement main phase grain, thereby temperature stability is further improved.In auxiliary phase alloy, the samarium element of interpolation, due to himself chemical property, can effectively improve the stability of neodymium iron boron magnetic body; Zirconium can reduce the sensitiveness of neodymium iron boron magnetic body to sintering temperature, thereby improved the resistance to sintering temperature of neodymium iron boron magnetic body, and there is not the abnormal growth of crystal grain, make it obtain high energy product, simultaneous temperature stability is more good, in addition, zirconium also can make NdFeB material obtain good corrosion resistance and mechanical property; The interpolation of copper can improve Grain-Boundary Phase, increases wetability.
In the raw material of described main-phase alloy, the purity of iron is 99.99%.The purity of boron and aluminium is 99.9%, and the purity of neodymium and gadolinium is 99.8%; In the raw material of described auxiliary phase alloy, the purity of iron is 99.99%, and the purity of boron and copper is 99.9%, and the purity of neodymium, zirconium and samarium is 99.8%.
The production technology of the neodymium-iron-boron magnetic material that said temperature has good stability comprises following processing step:
1) to main-phase alloy and auxiliary phase alloy prepare burden respectively, smelting and ingot casting operation, obtain main-phase alloy ingot casting and auxiliary phase alloy ingot casting;
2) main-phase alloy ingot casting is carried out to high annealing operation;
3) main-phase alloy ingot casting and auxiliary phase alloy ingot casting are carried out respectively to the quick-fried operation of hydrogen, obtain main-phase alloy powder and auxiliary phase alloy powder;
4) main-phase alloy powder is mixed according to a certain percentage with auxiliary phase alloy powder;
5) to the mixed-powder of main-phase alloy and auxiliary phase alloy grind, moulding, sintering and heat treatment step.
Ternary sintered NdFeB magnet is mainly by three phase compositions, principal phase, boron-rich phase and rich neodymium phase.When in magnet, boron content is lower, it only has principal phase and rich neodymium phase.The percentage by volume of principal phase in magnet determined remanent magnetism and the magnetic energy product of neodymium-iron-boron magnetic material, the quantity of rich neodymium phase and its raising of favourable magnet HCJ of distributing homogeneity around principal phase, and the coercitive raising of magnet can promote the lifting of magnet temperature stability.
In the production technology of the neodymium-iron-boron magnetic material that described temperature stability is good, the row batching of main-phase alloy and auxiliary phase alloy, smelting and ingot casting operation, and the high annealing operation of main-phase alloy ingot casting is:
1) according to the percentage by weight of main-phase alloy and auxiliary phase alloy, get appropriate raw material, packed in the crucible of induction heating type vacuum smelting furnace, wherein the loading sequence of main-phase alloy is followed successively by boron, iron, gadolinium, neodymium, and metallic aluminium is positioned in the loading hopper of smelting furnace; The loading sequence of auxiliary phase alloy is followed successively by boron, zirconium, iron, samarium, copper, samarium, neodymium;
2) smelting furnace is vacuumized to processing, and raw material in stove is carried out to preheating, complete in backward smelting furnace and be filled with high purity argon, make the relative atmospheric pressure of argon pressure in stove be-0.5Mpa; Smelting furnace heating power is promoted to 27KW, until metal all melts in stove;
3) after metal in stove melts, add metallic aluminium; With the temperature of 1900 ℃, raw material in smelting furnace is heated, carry out sufficient electromagnetic agitation simultaneously;
4) utilize funnel that molten steel is poured in the two-sided water cooled copper mould that cooling thickness is 30mm, cooling water temperature is 15 ℃, and hydraulic pressure is 4MPa, and be 85 minutes cooling time;
5) open smelting furnace, take out ingot casting, its surface finish is smooth, and encapsulation is preserved;
6) alloy cast ingot after processing is placed in high vacuum sintering furnace, and it is vacuumized to processing, after completing, alloy cast ingot in sintering furnace is carried out to annealing in process, be heated, programming rate is 5 ℃/min, until temperature reaches 1050 ℃ in stove, and is incubated 6 hours under this temperature environment;
7) make main-phase alloy ingot casting with stove cooling 70 minutes, its taking-up is naturally cooled to room temperature.
Smelt with ingot casting and can form the principal phase that determines magnet performance in neodymium-iron-boron magnetic material.In smelting process, alloy can be rare goes out α-Fe phase, α-Fe has not only reduced the generation quantity of principal phase in ingot casting mutually, also can produce harmful effect to operations such as follow-up grinding flour, moulding, thereby the performance of harm neodymium-iron-boron magnetic material, α-Fe meets simultaneously affects the distribution of the inner rich neodymium phase of magnet, thereby affects the temperature stability of magnet.
Adopt above-mentioned processing step, its tool has the following advantages:
1) loading sequence of main-phase alloy and auxiliary phase alloy is according to its raw material fusing point order from high to low, thereby guarantees that first the raw metal of upper end melts, and forms liquid phase, and then accelerates the thawing of its lower end raw material;
2) adopt induction heating type vacuum smelting furnace, it has, and metal inside degasifying effect is good, crystallization is fast, clean type good, can Fast Heating, and to the unconfined advantage of raw material shape;
3) before smelting, vacuumize processing, and pass into argon gas, first can avoid oxygen, carbon dioxide etc. in the interior raw material of stove and air to react; Secondly because argon gas is inert gas, it can play a protective role; Meanwhile, passing into of argon gas makes stove internal gas pressure be less than atmospheric pressure, and the fusing point of raw material in stove is decreased, and reduced process time;
4) main-phase alloy ingot casting is carried out to high annealing, can eliminate its inner α-Fe phase, promoted magnet performance and the temperature stability of ingot casting.
In the production technology of the neodymium-iron-boron magnetic material that described temperature stability is good, main-phase alloy ingot casting and auxiliary phase alloy ingot casting carry out respectively the quick-fried operation of hydrogen and are:
1) the main-phase alloy ingot casting of annealed processing and auxiliary phase alloy ingot casting are broken into respectively to fritter, make it large as far as possible at the basic material loading piece that can put into hydrogen blasting furnace, and it is inserted respectively to hydrogen blasting furnace and carry out the quick-fried processing of hydrogen;
2) hydrogen blasting furnace is vacuumized after processing, complete backward its inside and pass into high-purity hydrogen, Hydrogen Vapor Pressure remains on 2MPa;
3) treat that temperature starts to raise in hydrogen blasting furnace, to water spray in stove, to reduce temperature in stove, make temperature in hydrogen blasting furnace remain on 120 ℃, during hydrogen blasting furnace keep rotation;
4) above-mentioned steps continues, after 2 hours, to stop passing into hydrogen, and find time, and hydrogen in stove is disclosed to heating, and heating-up temperature is 780 ℃, and be 5 hours heating time, makes main-phase alloy and auxiliary phase alloy ingot casting all after hydrogen is quick-fried, become alloy powder;
5) end to be heated, adopts powder in water quench stove, and cooling water temperature is 15 ℃.
Neodymium-iron-boron magnetic material is comprised of a plurality of isolated main phase grains each other, and described crystal grain has sharp-pointed corner angle or the polyhedral at outstanding position for occupying, and corner angle or outstanding position can produce magnetic field.So the quantity of main phase grain increase the performance that is all conducive to neodymium-iron-boron magnetic material with the minimizing at its corner angle or outstanding position.
Adopt above-mentioned processing step, tool has the following advantages:
1) main-phase alloy ingot casting and auxiliary phase alloy ingot casting are broken into respectively to the maximum fragment that can pack hydrogen blasting furnace into, can reduce the infringement of Mechanical Crushing to ingot structure, thereby avoid wherein main phase grain to be damaged;
2) adopt the quick-fried technique of hydrogen, alloy cast ingot in the quick-fried process of hydrogen by along brilliant and transgranular fracture and fragmentation can reduce the infringement to ingot casting crystal grain in pulverizing process, thereby make the proportion increase of single crystal grain in magnetic, it is conducive to improve the degree of orientation of magnetic, improves the magnetic property of sintered magnet;
3) the quick-fried gained powder of hydrogen fragility is large, can save the abrasive dust time of follow-up airflow milling operation; The quick-fried technique of hydrogen can be improved the pattern of powder simultaneously, powder particle shape is more approaching circle or oval-shaped polyhedron, and the quick-fried particle size distribution of improving of hydrogen, reduces excessive and meticulous powder, thereby make its more easily processing in the operations such as follow-up moulding and sintering, be heated more even.
In the production technology of the neodymium-iron-boron magnetic material that described temperature stability is good, main-phase alloy powder and auxiliary phase alloy powder mixed processes, and the grinding of the mixed-powder of main-phase alloy and auxiliary phase alloy, moulding, sintering and heat treatment step are:
1) main-phase alloy and auxiliary phase alloy powder are sieved respectively, sieve out coarse granules more than 8 orders, to it, adopt mechanical mill broken, after fragmentation, it is mixed with fine powder, utilize batch mixer to mix 2.5 hours;
2) main-phase alloy mixing and auxiliary phase alloy powder are inserted to Gas grinding machine and carry out fine grinding, in grinder, Control for Oxygen Content is at 15ppm;
3) main-phase alloy powder and auxiliary mixed powder for alloy are made respectively after the fine powder of 4 μ m, by 90～98:10～2 proportioning, mixed, add after the antioxidant of 1 ‰ weight ratios and the mixture of lubricant simultaneously, mixed 2.5 hours; Described lubricant is mixed and is equipped by weight percentage by following raw materials according: 12 parts of industrial lubricants, 5 parts of Sodium Benzoates, 4 parts of vegetable oil acids, 4 parts of nitrite, 75 parts, water;
4) adopt Magnetic field press to carry out vertical mold pressing to said mixture, forming magnetic field Wei1.8 tesla, briquetting pressure is 3MPa, adopts afterwards isostatic pressing machine, and the mixture of processing through mold pressing is waited to static pressure, obtains slug press, isostatic pressure is 10MPa;
5) above-mentioned slug press is incubated to 45 minutes under the environment of 400 ℃, under the environment of 500 ℃, is incubated 45 minutes, under the environment of 700 ℃, be incubated 145 minutes;
6) the temperature high temperature sintering with 1250 ℃ by the slug press through above-mentioned processing, sintering time is 167 minutes;
7) neodymium-iron-boron magnetic material after sintering is carried out to temper, first order tempering for to be incubated 95 minutes under the environment of 950 ℃, and second level tempering for to be incubated 165 minutes under the environment of 680 ℃.
In the quick-fried operation of hydrogen, the residual certain hydrogen of meeting in alloy powder, it not only can cause the cracking of product in sintering process, and can make product partially hard, and follow-up plating afterwards easy electrodeposited coating comes off, therefore tackle it, arranges hydrogen technique.
Adopt above-mentioned processing step, tool has the following advantages:
1) meal after hydrogen is quick-fried is mixed into row airflow milling with fine powder again after machine mill, and it can make alloy powder volume less, and more even, makes in subsequent forming operation powder bonding more even;
2) in sintering circuit, blank is carried out to the insulation under various temperature, it can realize row's hydrogen of blank, thereby avoids because hydrogen is got rid of the clean product generation the problems referred to above that cause;
3) lubricating oil that adopts above-mentioned formula to make, compares conventional diesel fuel lubricity oil, has cooling, corrosion-resistant effect, and its volatility is little simultaneously, and environment is not polluted;
4) after sintering, to magnet, adopt tempering process to process, can effectively improve magnet performance.
As a modification of the present invention, after being equipped with, the raw material of described main-phase alloy and auxiliary phase alloy all needs to cut off and the work of polishing, and it can be so that raw metal be convenient to weighing, and can reduce impurity.
As a modification of the present invention, vacuumizing in the smelting procedure of described main-phase alloy and auxiliary phase alloy is treated to: adopt vacuum pump to vacuumize processing to smelting furnace, in stove, vacuum degree reaches 2.5 * 10
-2after Pa, induction coil power transmission, carries out preheating to raw material in smelting furnace, and heating power is 12KW; Stable after changing until vacuum degree in smelting furnace, stop vacuumizing; Vacuumizing in the high annealing operation of main-phase alloy is treated to: in heating process, guarantee that vacuum degree reaches 2.5 * 10
-2pa, guarantees that in insulating process vacuum degree reaches 5.0 * 10
-2pa; Vacuumizing in the quick-fried operation of hydrogen of main-phase alloy and auxiliary phase alloy ingot casting is treated to: adopt vacuum pump to vacuumize processing to hydrogen blasting furnace, after 40 minutes duration, stop vacuumizing, and pass into nitrogen in hydrogen blasting furnace, and again vacuumize, until in hydrogen blasting furnace, vacuum degree reaches 0.2Pa.
As another kind of improvement of the present invention, described in vacuumize that to process the vacuum furnace adopting be oil-sealed rotary pump, Roots vacuum pump and three grades of pumped vacuum systems of diffusion vacuum pump.
Than prior art, tool of the present invention has the following advantages:
1) by adding the elements such as gadolinium, zirconium, samarium, the temperature stability of neodymium iron boron magnetic body is promoted to some extent, make its temperature fluctuation in the use procedure of smelting process and neodymium iron boron magnetic body more stable, thereby be beneficial to processing and use;
2) adopt pairing gold legal system for neodymium-iron-boron magnetic material, it can obtain the magnetic material higher than the magnetic property of single alloyage, and it has good corrosion resistance and stability simultaneously;
3) by main-phase alloy and auxiliary phase alloy, smelt respectively and mixed sintering, avoid main-phase alloy in smelting process, to have that α-Fe is mutually rare to be gone out, can make simultaneously rich neodymium in auxiliary phase alloy be uniformly distributed mutually with main-phase alloy in principal phase around, effectively improved the magnetic behavior of neodymium-iron-boron magnetic material;
4) the rich neodymium in auxiliary phase alloy can be realized liquid-phase sintering mutually in sintering process, realize densification sintering, simultaneously the rich neodymium crystal boundary that hands down distributes, and principal phase particle is isolated mutually, play the effect of exchange coupling, be conducive to the raising of magnet coercive force and temperature stability;
5) by techniques such as the quick-fried powder process of hydrogen, in neodymium-iron-boron magnetic material production process, avoid its performance impaired, make its product compare existing product and all make moderate progress in magnet performance and coercive force performance, promote the improvement of magnet temperature stability.
All the other feature & benefits of the present embodiment are identical with embodiment 1, and embodiment 1 is preferred version of the present invention.
The disclosed technological means of the present invention program is not limited only to the disclosed technological means of above-mentioned execution mode, also comprises the technical scheme being comprised of above technical characterictic combination in any.
Claims (6)
1. the good neodymium-iron-boron magnetic material of temperature stability, is characterized in that, the good neodymium-iron-boron magnetic material of described temperature stability is formed by main-phase alloy and auxiliary phase alloy mixed configuration; Described main-phase alloy is configured and forms by weight percentage by following raw materials according: iron 64.5～68.5%, boron 1.0～1.2%, neodymium 30.2～34.3%, gadolinium 0.05～0.4%, aluminium 0.1～0.4%; Auxiliary phase alloy is equipped by weight percentage by following raw materials according: iron 50.8～54.2%, boron 0.8～1.2%, neodymium 18.9～21.1%, zirconium 12.8～16.3%, samarium 8.9～11.1%, copper 0.8～1.2%.
2. according to the good neodymium-iron-boron magnetic material of the temperature stability described in claim 1 or 2, it is characterized in that, in the raw material of described main-phase alloy, the purity of iron, boron and aluminium is all at least 99.9%, and the purity of neodymium and gadolinium is at least 99.8%; In the raw material of described auxiliary phase alloy, the purity of iron, boron and copper is at least 99.9%, and the purity of neodymium, zirconium and samarium is at least 99.8%.
3. a production technology for the good neodymium-iron-boron magnetic material of temperature stability, is characterized in that, the production technology of the neodymium-iron-boron magnetic material that described temperature stability is good comprises following processing step:
To main-phase alloy and auxiliary phase alloy prepare burden respectively, smelting and ingot casting operation, obtain main-phase alloy ingot casting and auxiliary phase alloy ingot casting;
1) main-phase alloy ingot casting is carried out to high annealing operation;
2) main-phase alloy ingot casting and auxiliary phase alloy ingot casting are carried out respectively to the quick-fried operation of hydrogen, obtain main-phase alloy powder and auxiliary phase alloy powder;
3) main-phase alloy powder is mixed according to a certain percentage with auxiliary phase alloy powder;
4) to the mixed-powder of main-phase alloy and auxiliary phase alloy grind, moulding, sintering and heat treatment step;
Wherein the row batching of main-phase alloy and auxiliary phase alloy, smelting and ingot casting operation, and the high annealing operation of main-phase alloy ingot casting is:
1.1) according to the percentage by weight of main-phase alloy and auxiliary phase alloy, get appropriate raw material, packed in the crucible of vacuum induction smelting furnace, wherein the loading sequence of main-phase alloy is followed successively by boron, iron, gadolinium, neodymium, and metallic aluminium is positioned in the loading hopper of smelting furnace; The loading sequence of auxiliary phase alloy is followed successively by boron, zirconium, iron, samarium, copper, samarium, neodymium;
1.2) smelting furnace is vacuumized to processing, and raw material in stove is carried out to preheating, complete in backward smelting furnace and be filled with high purity argon, make the relative atmospheric pressure of argon pressure in stove be-0.5Mpa; Smelting furnace heating power is promoted to 18～27KW, until metal all melts in stove;
1.3) after metal in stove melts, add metallic aluminium; Temperature with 1600 to 1900 ℃ heats raw material in smelting furnace, carries out sufficient electromagnetic agitation simultaneously;
1.4) utilizing funnel that molten steel is poured into cooling thickness is that in 15 to 30mm two-sided water cooled copper mould, cooling water temperature is 15 to 30 ℃, and hydraulic pressure is 4MPa, and be 65 to 85 minutes cooling time;
1.5) open smelting furnace, take out ingot casting, its surface finish is smooth, and encapsulation is preserved;
1.6) alloy cast ingot after processing is placed in high vacuum sintering furnace, and it is vacuumized to processing, after completing, alloy cast ingot in sintering furnace is carried out to annealing in process, be heated, programming rate is 5 ℃/min, until in stove, temperature reaches 900 to 1050 ℃, and under this temperature environment, be incubated 6 to 8 hours;
1.7) make main-phase alloy ingot casting with stove cooling 55 to 70 minutes, its taking-up is naturally cooled to room temperature;
In the production technology of the neodymium-iron-boron magnetic material that described temperature stability is good, main-phase alloy ingot casting and auxiliary phase alloy ingot casting carry out respectively the quick-fried operation of hydrogen and are:
2.1) the main-phase alloy ingot casting of annealed processing and auxiliary phase alloy ingot casting are broken into respectively to fritter, make it large as far as possible at the basic material loading piece that can put into hydrogen blasting furnace, and it is inserted respectively to hydrogen blasting furnace and carry out the quick-fried processing of hydrogen;
2.2) hydrogen blasting furnace is vacuumized after processing, complete backward its inside and pass into high-purity hydrogen, Hydrogen Vapor Pressure remains on 2MPa;
2.3) treat that temperature starts to raise in hydrogen blasting furnace, to water spray in stove, to reduce temperature in stove, make temperature in hydrogen blasting furnace remain on 80 to 120 ℃, during hydrogen blasting furnace keep rotation;
2.4) above-mentioned steps continues, after 1 to 2 hour, to stop passing into hydrogen, and find time, and hydrogen in stove is disclosed to heating, and heating-up temperature is 450 to 780 ℃, and be 5 to 7 hours heating time, makes main-phase alloy and auxiliary phase alloy ingot casting all after hydrogen is quick-fried, become alloy powder;
2.5) end to be heated, adopts powder in water quench stove, and cooling water temperature is 15 to 30 ℃;
Main-phase alloy powder and auxiliary phase alloy powder mixed processes in the production technology of the neodymium-iron-boron magnetic material that described temperature stability is good, and the grinding of the mixed-powder of main-phase alloy and auxiliary phase alloy, moulding, sintering and heat treatment step are:
3.1) main-phase alloy and auxiliary phase alloy powder are sieved respectively, sieve out coarse granules more than 8 orders, to it, adopt mechanical mill broken, after fragmentation, it is mixed with fine powder, utilize batch mixer to mix 1.2 to 2.5 hours;
3.2) main-phase alloy mixing and auxiliary phase alloy powder are inserted to Gas grinding machine and carry out fine grinding, in grinder, Control for Oxygen Content is at 15ppm;
3.3) main-phase alloy powder and auxiliary mixed powder for alloy are made respectively after the fine powder of 2 to 4 μ m, by 90～98:10～2 proportioning, mixed, add after the antioxidant of 1 ‰ weight ratios and the mixture of lubricant simultaneously, mixed 1.5 to 2.5 hours; Described lubricant is mixed and is equipped by weight percentage by following raw materials according: 1～12 part of industrial lubricants, 0.3～5 part of Sodium Benzoate, 0.5～6 part of vegetable oil acid, 0.2～6 part of nitrite, 25～85 parts, water;
3.4) adopt Magnetic field press to carry out vertical mold pressing to said mixture, forming magnetic field Wei1.8 tesla, briquetting pressure is 3MPa, adopts afterwards isostatic pressing machine, and the mixture of processing through mold pressing is waited to static pressure, obtains slug press, isostatic pressure is 10MPa;
3.5) above-mentioned slug press is incubated to 45 to 68 minutes under the environment of 310 to 400 ℃, under the environment of 410 to 500 ℃, is incubated 45 to 68 minutes, under the environment of 610 to 700 ℃, be incubated 145 to 230 minutes;
3.6) the temperature high temperature sintering with 1080 to 1250 ℃ by the slug press through above-mentioned processing, sintering time is 167 to 256 minutes;
3.7) neodymium-iron-boron magnetic material after sintering is carried out to temper, first order tempering for to be incubated 95 to 145 minutes under the environment of 780～950 ℃, and second level tempering for to be incubated 165 to 195 minutes under the environment of 530～680 ℃.
4. according to the production technology of the good neodymium-iron-boron magnetic material of temperature stability claimed in claim 3, it is characterized in that, the raw material of described main-phase alloy and auxiliary phase alloy all needs to cut off and polishing after being equipped with.
5. according to the production technology of the good neodymium-iron-boron magnetic material of the temperature stability described in claim 3 or 4, it is characterized in that, vacuumizing in the smelting procedure of described main-phase alloy and auxiliary phase alloy is treated to: adopt vacuum pump to vacuumize processing to smelting furnace, in stove, vacuum degree reaches 2.5 * 10
-2after Pa, induction coil power transmission, carries out preheating to raw material in smelting furnace, and heating power is 8～12KW; Stable after changing until vacuum degree in smelting furnace, stop vacuumizing; Vacuumizing in the high annealing operation of main-phase alloy is treated to: in heating process, guarantee that vacuum degree reaches 2.5 * 10
-2pa, guarantees that in insulating process vacuum degree reaches 5.0 * 10
-2pa; Vacuumizing in the quick-fried operation of hydrogen of main-phase alloy and auxiliary phase alloy ingot casting is treated to: adopt vacuum pump to vacuumize processing to hydrogen blasting furnace, after 25 to 40 minutes duration, stop vacuumizing, and pass into nitrogen in hydrogen blasting furnace, and again vacuumize, until in hydrogen blasting furnace, vacuum degree reaches 0.2Pa.
6. according to the production technology of the good neodymium-iron-boron magnetic material of the temperature stability described in claim 3 or 4, it is characterized in that, described in to vacuumize the vacuum furnace process adopting be oil-sealed rotary pump, Roots vacuum pump and three grades of pumped vacuum systems of diffusion vacuum pump.
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