CN103617854A - Neodymium iron boron magnetic material with high coercivity - Google Patents
Neodymium iron boron magnetic material with high coercivity Download PDFInfo
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Abstract
The invention relates to a neodymium iron boron magnetic material with the high coercivity. The neodymium iron boron magnetic material with the high coercivity is formed by a main-phase alloy and a secondary-phase alloy through mixing. The main-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 molybdenum and 0.1-0.4% of gallium. The secondary-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 praseodymium, 8.9-11.1% of terbium, and 0.8-1.2% of cobalt. The neodymium iron boron magnetic material prepared with the method has high intrinsic coercivity.
Description
Technical field
The present invention relates to a kind of magnetic material and production technology thereof, especially a kind of neodymium-iron-boron magnetic material and production technology thereof with high-coercive force.
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, to neodymium iron boron, the crystal structure in microstructure destroys serious tradition smelting process, thereby cause rich neodymium phase structure in neodymium iron boron to receive damage, the HCJ of neodymium iron boron is declined, make neodymium iron boron magnetic body easily demagnetize phenomenon and affect use.
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 make the HCJ of neodymium iron boron magnetic body be improved.
For solving the problems of the technologies described above, the present invention relates to a kind of neodymium-iron-boron magnetic material with high-coercive force, 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%, molybdenum 0.05～0.4%, gallium 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%, praseodymium 12.8～16.3%, terbium 8.9～11.1%, cobalt 0.8～1.2%.
In such scheme, the molybdenum in main-phase alloy can pass through crystal grain thinning, suppresses soft magnetism and separates out mutually, thereby improve magnet coercive force; And gallium also can significantly improve the coercive force of alloy, and gallium is more obvious at the Effect on Alloys containing cobalt.In auxiliary phase alloy, coercitive raising has good effect to magnet for terbium and praseodymium; Cobalt can all be replaced the iron atom in principal phase, because the exchange interaction of cobalt is stronger than iron, therefore it can significantly improve the Curie temperature of principal phase, thereby the temperature stability of magnet is strengthened to some extent, the HCJ of temperature stability and rare-earth permanent magnet is closely bound up, so improved the coercive force performance of neodymium iron boron magnetic body.
In the raw material of described main-phase alloy, the purity of iron, boron and gallium is all at least 99.9%, and the purity of neodymium and molybdenum is at least 99.8%; In the raw material of described auxiliary phase alloy, the purity of iron, boron and cobalt is at least 99.9%, and the purity of neodymium, praseodymium and terbium is at least 99.8%.
The above-mentioned production technology with the neodymium-iron-boron magnetic material of high-coercive force 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, and rich neodymium is conducive to the raising of magnet HCJ mutually.
In the production technology of the described neodymium-iron-boron magnetic material with high-coercive force, 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 molybdenum, boron, iron, neodymium, and gallium is positioned in the loading hopper of smelting furnace; The loading sequence of auxiliary phase alloy is followed successively by boron, iron, cobalt, terbium, neodymium, praseodymium;
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 18～25KW, until metal all melts in stove;
3) after metal in stove melts, add gallium; Temperature with 2300 to 2700 ℃ 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 20 to 32mm two-sided water-cooled jig, cooling water temperature is 15 to 30 ℃, and hydraulic pressure is 4MPa, and be 85 to 100 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 980 to 1230 ℃, and under this temperature environment, be incubated 6 to 8 hours;
7) make main-phase alloy ingot casting with stove cooling 50 to 75 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, and 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, thus the performance of harm neodymium-iron-boron magnetic material.
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, promote the magnet performance of ingot casting.
In the production technology of the described neodymium-iron-boron magnetic material with high-coercive force, 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 75 to 110 ℃, during hydrogen blasting furnace keep rotation;
4) above-mentioned steps continues, after 1.2 to 2.8 hours, to stop passing into hydrogen, and find time, hydrogen in stove is disclosed to heating, heating-up temperature is 520 to 750 ℃, and be 4.5 to 6.3 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 comprises a plurality of isolated main phase grains each other and forms, 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.Be attached to the quantity of principal phase crystal rich neodymium phase crystal around simultaneously, with and the uniformity that distributes be all conducive to the coercitive raising of magnet.
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) in the quick-fried technique of hydrogen, rich neodymium phase crystal is difficult for being damaged, and its distribution is simultaneously more even compared with prior art, thereby magnet HCJ is increased;
4) 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 described neodymium-iron-boron magnetic material with high-coercive force, 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 1.5 to 3 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 3 to 5 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;
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 55 to 80 minutes under the environment of 250 to 370 ℃, under the environment of 350 to 470 ℃, is incubated 55 to 80 minutes, under the environment of 550 to 670 ℃, be incubated 140 to 210 minutes;
6) the temperature high temperature sintering with 1050 to 1150 ℃ by the slug press through above-mentioned processing, sintering time is 180 to 300 minutes;
7) neodymium-iron-boron magnetic material after sintering is carried out to temper, first order tempering for to be incubated 95 to 120 minutes under the environment of 800～950 ℃, and second level tempering for to be incubated 155 to 190 minutes under the environment of 450～700 ℃.
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) after sintering, to magnet, adopt tempering process to process, can effectively improve magnet performance and magnet HCJ.
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 5～10KW; 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 molybdenum, gallium, terbium, the HCJ of neodymium-iron-boron magnetic material is increased, improved the NdFeB material feature of coercive force deficiency in the past; By adding cobalt, improve the temperature temperature of neodymium-iron-boron magnetic material simultaneously, and then indirectly promote the raising of HCJ;
2) adopt pairing gold legal system for neodymium-iron-boron magnetic material, it can obtain than the equal better magnetic material of the magnetic behavior of single alloyage and HCJ, and it has good corrosion resistance and lower final oxygen content 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, realizes densification sintering, and the rich neodymium crystal boundary that hands down distributes simultaneously, and principal phase particle is isolated mutually, plays the effect of exchange coupling, is conducive to the coercitive raising of magnet;
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.
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
A neodymium-iron-boron magnetic material with high-coercive force, 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%, molybdenum 0.1%, gallium 0.1%; Auxiliary phase alloy is equipped by weight percentage by following raw materials according: iron 53.8%, boron 1.2%, neodymium 19.5%, praseodymium 14.3%, terbium 10.2%, cobalt 1.0%.
In such scheme, the molybdenum in main-phase alloy can pass through crystal grain thinning, suppresses soft magnetism and separates out mutually, thereby improve magnet coercive force; And gallium also can significantly improve the coercive force of alloy, and gallium is more obvious at the Effect on Alloys containing cobalt.In auxiliary phase alloy, coercitive raising has good effect to magnet for terbium and praseodymium; Cobalt can all be replaced the iron atom in principal phase, because the exchange interaction of cobalt is stronger than iron, therefore it can significantly improve the Curie temperature of principal phase, thereby the temperature stability of magnet is strengthened to some extent, the HCJ of temperature stability and rare-earth permanent magnet is closely bound up, so improved the coercive force performance of neodymium iron boron magnetic body.
In the raw material of described main-phase alloy, the purity of iron, boron and gallium is 99.9%, and the purity of neodymium and molybdenum is 99.8%; In the raw material of described auxiliary phase alloy, the purity of iron, boron and cobalt is 99.9%, and the purity of neodymium, praseodymium and terbium is 99.8%.
The above-mentioned production technology with the neodymium-iron-boron magnetic material of high-coercive force 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, and rich neodymium is conducive to the raising of magnet HCJ mutually.
In the production technology of the described neodymium-iron-boron magnetic material with high-coercive force, 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 molybdenum, boron, iron, neodymium, and gallium is positioned in the loading hopper of smelting furnace; The loading sequence of auxiliary phase alloy is followed successively by boron, iron, cobalt, terbium, neodymium, praseodymium;
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 18KW, until metal all melts in stove;
3) after metal in stove melts, add gallium; With the temperature of 2300 ℃, 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 jig that cooling thickness is 20 mm, cooling water temperature is 30 ℃, 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 980 ℃ in stove, and is incubated 8 hours under this temperature environment;
7) make main-phase alloy ingot casting with stove cooling 50 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, and 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, thus the performance of harm neodymium-iron-boron magnetic material.
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, promote the magnet performance of ingot casting.
In the production technology of the described neodymium-iron-boron magnetic material with high-coercive force, 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 75 ℃, during hydrogen blasting furnace keep rotation;
4) above-mentioned steps continues, after 1.2 hours, to stop passing into hydrogen, and find time, and hydrogen in stove is disclosed to heating, and heating-up temperature is 520 ℃, and be 6.3 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 comprises a plurality of isolated main phase grains each other and forms, 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.Be attached to the quantity of principal phase crystal rich neodymium phase crystal around simultaneously, with and the uniformity that distributes be all conducive to the coercitive raising of magnet.
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) in the quick-fried technique of hydrogen, rich neodymium phase crystal is difficult for being damaged, and its distribution is simultaneously more even compared with prior art, thereby magnet HCJ is increased;
4) 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 described neodymium-iron-boron magnetic material with high-coercive force, 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 1.5 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 3 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;
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 80 minutes under the environment of 250 ℃, under the environment of 350 ℃, is incubated 80 minutes, under the environment of 550 ℃, be incubated 210 minutes;
6) the temperature high temperature sintering with 1050 ℃ by the slug press through above-mentioned processing, sintering time is 300 minutes;
7) neodymium-iron-boron magnetic material after sintering is carried out to temper, first order tempering for to be incubated 120 minutes under the environment of 800 ℃, and second level tempering for to be incubated 190 minutes under the environment of 450 ℃.
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) after sintering, to magnet, adopt tempering process to process, can effectively improve magnet performance and magnet HCJ.
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 5KW; 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 molybdenum, gallium, terbium, the HCJ of neodymium-iron-boron magnetic material is increased, improved the NdFeB material feature of coercive force deficiency in the past; By adding cobalt, improve the temperature temperature of neodymium-iron-boron magnetic material simultaneously, and then indirectly promote the raising of HCJ;
2) adopt pairing gold legal system for neodymium-iron-boron magnetic material, it can obtain than the equal better magnetic material of the magnetic behavior of single alloyage and HCJ, and it has good corrosion resistance and lower final oxygen content 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, realizes densification sintering, and the rich neodymium crystal boundary that hands down distributes simultaneously, and principal phase particle is isolated mutually, plays the effect of exchange coupling, is conducive to the coercitive raising of magnet;
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.
Embodiment 2
A neodymium-iron-boron magnetic material with high-coercive force, 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%, molybdenum 0.2%, gallium 0.2%; Auxiliary phase alloy is equipped by weight percentage by following raw materials according: iron 54.2%, boron 0.8%, neodymium 20.2%, praseodymium 13.4%, terbium 10.6%, cobalt 0.8%.
In such scheme, the molybdenum in main-phase alloy can pass through crystal grain thinning, suppresses soft magnetism and separates out mutually, thereby improve magnet coercive force; And gallium also can significantly improve the coercive force of alloy, and gallium is more obvious at the Effect on Alloys containing cobalt.In auxiliary phase alloy, coercitive raising has good effect to magnet for terbium and praseodymium; Cobalt can all be replaced the iron atom in principal phase, because the exchange interaction of cobalt is stronger than iron, therefore it can significantly improve the Curie temperature of principal phase, thereby the temperature stability of magnet is strengthened to some extent, the HCJ of temperature stability and rare-earth permanent magnet is closely bound up, so improved the coercive force performance of neodymium iron boron magnetic body.
In the raw material of described main-phase alloy, the purity of iron is 99.99%.The purity of boron and gallium is 99.9%, and the purity of neodymium and molybdenum 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 cobalt is 99.9%, and the purity of neodymium, praseodymium and terbium is 99.8%.
The above-mentioned production technology with the neodymium-iron-boron magnetic material of high-coercive force 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, and rich neodymium is conducive to the raising of magnet HCJ mutually.
In the production technology of the described neodymium-iron-boron magnetic material with high-coercive force, 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 molybdenum, boron, iron, neodymium, and gallium is positioned in the loading hopper of smelting furnace; The loading sequence of auxiliary phase alloy is followed successively by boron, iron, cobalt, terbium, neodymium, praseodymium;
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 25KW, until metal all melts in stove;
3) after metal in stove melts, add gallium; With the temperature of 2700 ℃, raw material in smelting furnace is heated, carry out sufficient electromagnetic agitation simultaneously;
4) utilize funnel by the molten steel two-sided water-cooled jig that to be poured into cooling thickness be 32mm, cooling water temperature is 15 ℃, and hydraulic pressure is 4MPa, and be 100 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 1230 ℃ in stove, and is incubated 6 hours under this temperature environment;
7) make main-phase alloy ingot casting with stove cooling 75 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, and 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, thus the performance of harm neodymium-iron-boron magnetic material.
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, promote the magnet performance of ingot casting.
In the production technology of the described neodymium-iron-boron magnetic material with high-coercive force, 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 110 ℃, during hydrogen blasting furnace keep rotation;
4) above-mentioned steps continues, after 2.8 hours, to stop passing into hydrogen, and find time, and hydrogen in stove is disclosed to heating, and heating-up temperature is 750 ℃, and be 4.5 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 comprises a plurality of isolated main phase grains each other and forms, 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.Be attached to the quantity of principal phase crystal rich neodymium phase crystal around simultaneously, with and the uniformity that distributes be all conducive to the coercitive raising of magnet.
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) in the quick-fried technique of hydrogen, rich neodymium phase crystal is difficult for being damaged, and its distribution is simultaneously more even compared with prior art, thereby magnet HCJ is increased;
4) 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 described neodymium-iron-boron magnetic material with high-coercive force, 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 3 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 5 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;
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 55 minutes under the environment of 370 ℃, under the environment of 470 ℃, is incubated 55 minutes, under the environment of 670 ℃, be incubated 140 minutes;
6) the temperature high temperature sintering with 1150 ℃ by the slug press through above-mentioned processing, sintering time is 180 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 155 minutes under the environment of 700 ℃.
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) after sintering, to magnet, adopt tempering process to process, can effectively improve magnet performance and magnet HCJ.
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 10KW; 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 molybdenum, gallium, terbium, the HCJ of neodymium-iron-boron magnetic material is increased, improved the NdFeB material feature of coercive force deficiency in the past; By adding cobalt, improve the temperature temperature of neodymium-iron-boron magnetic material simultaneously, and then indirectly promote the raising of HCJ;
2) adopt pairing gold legal system for neodymium-iron-boron magnetic material, it can obtain than the equal better magnetic material of the magnetic behavior of single alloyage and HCJ, and it has good corrosion resistance and lower final oxygen content 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, realizes densification sintering, and the rich neodymium crystal boundary that hands down distributes simultaneously, and principal phase particle is isolated mutually, plays the effect of exchange coupling, is conducive to the coercitive raising of magnet;
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.
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. a neodymium-iron-boron magnetic material with high-coercive force, is characterized in that, described in there is high-coercive force neodymium-iron-boron magnetic material by main-phase alloy and auxiliary phase alloy mixed configuration, formed; 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%, molybdenum 0.05～0.4%, gallium 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%, praseodymium 12.8～16.3%, terbium 8.9～11.1%, cobalt 0.8～1.2%.
2. according to the neodymium-iron-boron magnetic material with high-coercive force 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 gallium is all at least 99.9%, and the purity of neodymium and molybdenum is at least 99.8%; In the raw material of described auxiliary phase alloy, the purity of iron, boron and cobalt is at least 99.9%, and the purity of neodymium, praseodymium and terbium is at least 99.8%.
3. a production technology with the neodymium-iron-boron magnetic material of high-coercive force, is characterized in that, described in there is the neodymium-iron-boron magnetic material of high-coercive force production technology comprise 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;
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 molybdenum, boron, iron, neodymium, and gallium is positioned in the loading hopper of smelting furnace; The loading sequence of auxiliary phase alloy is followed successively by boron, iron, cobalt, terbium, neodymium, praseodymium;
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 18～25KW, until metal all melts in stove;
1.3) after metal in stove melts, add gallium; Temperature with 2300 to 2700 ℃ 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 20 to 32mm two-sided water-cooled jig, cooling water temperature is 15 to 30 ℃, and hydraulic pressure is 4MPa, and be 85 to 100 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 980 to 1230 ℃, and under this temperature environment, be incubated 6 to 8 hours;
1.7) make main-phase alloy ingot casting with stove cooling 50 to 75 minutes, its taking-up is naturally cooled to room temperature;
In the production technology of the described neodymium-iron-boron magnetic material with high-coercive force, 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 75 to 110 ℃, during hydrogen blasting furnace keep rotation;
2.4) above-mentioned steps continues, after 1.2 to 2.8 hours, to stop passing into hydrogen, and find time, hydrogen in stove is disclosed to heating, heating-up temperature is 520 to 750 ℃, and be 4.5 to 6.3 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 described neodymium-iron-boron magnetic material with high-coercive force, 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 1.5 to 3 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 3 to 5 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;
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 55 to 80 minutes under the environment of 250 to 370 ℃, under the environment of 350 to 470 ℃, is incubated 55 to 80 minutes, under the environment of 550 to 670 ℃, be incubated 140 to 210 minutes;
3.6) the temperature high temperature sintering with 1050 to 1150 ℃ by the slug press through above-mentioned processing, sintering time is 180 to 300 minutes;
3.7) neodymium-iron-boron magnetic material after sintering is carried out to temper, first order tempering for to be incubated 95 to 120 minutes under the environment of 800～950 ℃, and second level tempering for to be incubated 155 to 190 minutes under the environment of 450～700 ℃.
4. according to the production technology with the neodymium-iron-boron magnetic material of high-coercive force 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 neodymium-iron-boron magnetic material with high-coercive force described in any one 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 5～10KW; 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 neodymium-iron-boron magnetic material with high-coercive force 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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104399995A (en) * | 2014-12-05 | 2015-03-11 | 爱科科技有限公司 | Agent charging method for jet-mill-based powdering of sintered neodymium iron boron |
| CN106710765A (en) * | 2015-07-21 | 2017-05-24 | 宁波科田磁业有限公司 | High-coercivity sintered-neodymium-iron-boron magnetic body and preparing method thereof |
| CN112164571A (en) * | 2020-08-17 | 2021-01-01 | 包头韵升强磁材料有限公司 | Preparation method of sintered rare earth permanent magnet material |
| CN113314325A (en) * | 2021-04-24 | 2021-08-27 | 宁波大学 | Method for preparing high-performance neodymium iron boron |
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2013
- 2013-11-30 CN CN201310622022.7A patent/CN103617854A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104399995A (en) * | 2014-12-05 | 2015-03-11 | 爱科科技有限公司 | Agent charging method for jet-mill-based powdering of sintered neodymium iron boron |
| CN106710765A (en) * | 2015-07-21 | 2017-05-24 | 宁波科田磁业有限公司 | High-coercivity sintered-neodymium-iron-boron magnetic body and preparing method thereof |
| CN106710765B (en) * | 2015-07-21 | 2018-08-10 | 宁波科田磁业有限公司 | A kind of high-coercive force Sintered NdFeB magnet and preparation method thereof |
| CN112164571A (en) * | 2020-08-17 | 2021-01-01 | 包头韵升强磁材料有限公司 | Preparation method of sintered rare earth permanent magnet material |
| CN112164571B (en) * | 2020-08-17 | 2022-02-11 | 包头韵升强磁材料有限公司 | Preparation method of sintered rare earth permanent magnet material |
| CN113314325A (en) * | 2021-04-24 | 2021-08-27 | 宁波大学 | Method for preparing high-performance neodymium iron boron |
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Application publication date: 20140305 |