CN104575901A - Neodymium iron boron magnet added with terbium powder and preparation method thereof - Google Patents
Neodymium iron boron magnet added with terbium powder and preparation method thereof Download PDFInfo
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Abstract
The invention specifically relates to neodymium iron boron magnet added with terbium powder and a preparation method thereof, belonging to the technical field of magnetic material. The composition and mass percentage of the neodymium iron boron magnet are as follows: 28.40-28.8% of PrNd, 2.70-2.90% of Gd, 0.95-0.98% of B, 0.70-0.78% of Al, 0.22-0.25% of Cu and 0.10-0.30% of Tb, and the remaining is Fe. The invention further provides a method for preparing the neodymium iron boron magnet, comprising the following steps of: firstly compounding; then smelting, casting in a manner of scale to obtain melt-spinning sheets; and then hydrogen-smashing, airflow-grinding, spark plasma sintering and second temper heat treating to obtain neodymium iron boron magnet end products. The neodymium iron boron magnet of the invention has relatively high coercive force, residual magnetism and magnetic energy product simultaneously, good corrosion resistance and good mechanical property. The preparation method is simple and practicable.
Description
Technical field
The present invention relates to a kind of neodymium iron boron magnetic body, be specifically related to a kind ofly add neodymium iron boron magnetic body of terbium powder and preparation method thereof, belong to technical field of magnetic materials.
Background technology
Neodymium iron boron magnetic body is as rare earth permanent-magnetic material of new generation, and having the features such as high remanent magnetism, high-coercive force and high energy product, is the permanent magnetic material that in the world today, comprehensive magnetic can be the strongest.Along with the development of electronic information, automobile and machinery manufacturing industry, neodymium iron boron magnetic body also obtains fast development, particularly now the environmental consciousness of people is more and more stronger, and the demand of Nd-Fe-B permanent magnet for the high combination property that can be used for the energy-conservation field of Environment Protection such as electric automobile, wind-powered electricity generation constantly increases.
Neodymium iron boron magnetic body can be divided into Sintered NdFeB magnet and Agglutinate neodymium-iron-boron magnet, and Sintered NdFeB magnet is the best permanent magnetic material of current magnetic property, is most widely used.But for sintered Nd-Fe-B permanent magnet, the defects such as it also exists, and decay resistance is poor, mechanical property is good not.At present, the research for the combination property improving Sintered NdFeB magnet also gets more and more, but while improving these performances, often to the remanent magnetism of neodymium iron boron magnetic body and the negative effect of magnetic energy product also larger.
The preparation method of heavy rare earth hydride nano-particle doped sintered NdFeB permanent magnet is disclosed in Chinese invention patent application file (publication number: CN101521069A), its technical process is first adopt rapid hardening thin slice technique and the quick-fried legal system of hydrogen for NdFeB powder, prepare hydrogenation terbium or hydrogenation dysprosium nanometer powder with physics gas deposition technique again, carry out after then both being mixed suppressing, sinter and heat treatment obtains magnet.Prepare compared with NdFeB magnet prepares sintered NdFeB magnet with conventional art by the method, improve coercive force to a certain extent, and reduce the usage ratio of heavy rare earth terbium or dysprosium.But the carryover effect preparing NdFeB magnet by the method is that coercive force raising is not obvious, and remanent magnetism and magnetic energy product reduce obviously.And this application file does not embody to some extent for the aspect such as corrosion resistance and mechanical property improving sintered NdFeB magnet.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, provide one to have higher coercivity, remanent magnetism and magnetic energy product simultaneously, and the neodymium iron boron magnetic body of good corrosion resistance.
Object of the present invention realizes by following technical proposal: a kind of neodymium iron boron magnetic body adding terbium powder, its constituent and mass percent are: PrNd:28.40%-28.80%, Gd:2.70%-2.90%, B:0.95%-0.98%, Al:0.70%-0.78%, Cu:0.22%-0.25%, Tb:0.10%-0.30%, and surplus is Fe.
Compared to prior art, the present invention is by adding Tb powder, and part replaces Nd, the growth suppressing crystal grain and refinement main phase grain to improve coercive force and the temperature stability of NdFeB magnet; And the adding of Al, Cu and rare-earth Gd, the effect played in magnet by them, not only effectively can improve the coercive force of NdFeB magnet, and can improve the corrosion resistance of NdFeB magnet.
In neodymium iron boron magnetic body, improve the magnetic properties such as the coercive force of magnet usually through interpolation rare earth element as Gd, Dy, Ho, Tb, Ce etc.Rare earth Gd and Tb is added in neodymium iron boron magnetic body of the present invention, because they are heavy rare earth, the saturated pole intensity of the compound that they are formed in NdFeB magnet is lower, but there is high anisotropy field, and there is temperature compensation function, therefore can obtain the NdFeB magnet with high-coercive force and high-temperature stability.In neodymium iron boron magnetic body, the coercive force of Gd by suppressing the generation of harmful phase α-Fe to carry out magnet, but too much Gd can enter principal phase, reduces the coercive force of magnet on the contrary, therefore in the present invention controls Gd at 2.70%-2.90%.In addition, in neodymium iron boron magnetic body, conventional Dy or Tb comes partly to replace Nd to improve anisotropy and the coercive force of magnet, but reach identical action effect, the consumption of Dy will much larger than the consumption of Tb, therefore consider from the angle economized on resources with economic benefit, add the Tb of 0.10%-0.30% in the present invention, carry out refinement main phase grain by it and make it be evenly distributed, and then effectively improve the coercive force of NdFeB magnet.
In neodymium iron boron magnetic body of the present invention, with PrNd alloy, B and Fe for primary raw material, in order to obtain the NdFeB magnet of more high combination property, compositely add Al and Cu, their energy are most of or enter Grain-Boundary Phase completely, make Grain-Boundary Phase have better magnetic decoupling effect, effectively improve the coercive force of NdFeB magnet, and improve the decay resistance of NdFeB magnet, also can improve the mechanical property such as bending strength, toughness of NdFeB magnet simultaneously.Al has special wettability on the one hand, good wetting action is played on the border of crystal grain, Al can form the new rich neodymium phase containing Al on the border of crystal grain on the other hand, the border of crystal grain is made to become more clear, thus effectively reduce the demagnetizing effect of intercrystalline exchange coupling, not only substantially increase the coercive force of magnet, and reduce the remanent magnetism of NdFeB magnet and the negative effect of magnetic energy product.And Cu not only can enter principal phase, respectively improve its coercive force to different field property by the single shaft improving NdFeB magnet, but also can the specific area of crystal grain be increased crystal grain thinning, thus make rich neodymium Entropy density deviation more even, be more conducive to improving its coercive force.In addition, difference due to the chemical composition of each phase of magnet can cause its electrochemical potentials different, these can contact with each other in the environment of higher temperature and humidity thus composition corrodes micro cell and accelerated corrosion between phase, Al and Cu adds, and effectively can prevent the generation of this corrosion phenomenon.But the addition prevented in order to Al and Cu is too much, and can reduce the magnetic property of NdFeB magnet on the contrary, the addition of Al and Cu controls at 0.70%-0.78% and 0.22%-0.25% by the present invention respectively.
In neodymium iron boron magnetic body of the present invention, with PrNd alloy, B and Fe for primary raw material, add Tb powder, and compositely add heavy rare earth Gd and there is Al and Cu of decay resistance improving magnet, by they synergies in NdFeB magnet, obtain coercive force, remanent magnetism and magnetic energy product all higher, the NdFeB magnet that good corrosion resistance, mechanical property are good.
Further, as preferably, component and the mass percent of the neodymium iron boron magnetic body of described interpolation terbium powder are: PrNd:28.60%, Gd:2.80%, B:0.97%, Al:0.74%, Cu:0.23%, Tb:0.20%, surplus is Fe.
The present invention also provides a kind of method preparing the neodymium iron boron magnetic body of above-mentioned interpolation terbium powder, and described preparation method comprises the steps:
S1, batching and melting: prepare burden according to the constituent of above-mentioned neodymium iron boron magnetic body and mass percent, be evacuated down to 10 after then sending into vacuum rapid hardening smelting furnace
-3pa-10
-2pa, stops vacuumizing and being filled with after argon gas reaches 0.045-0.050MPa and carries out melting, carry out after furnace charge melts completely scale casting obtain thickness be 0.20-0.50mm get rid of strap;
Broken and the airflow milling process of S2, hydrogen: the above-mentioned strap that gets rid of is obtained through hydrogen break process the flour that average grain diameter is 10.0 μm-12.0 μm, then adds Tb powder and antioxidant and carries out airflow milling and obtain the fine powder that average grain diameter is 3.0 μm-4.0 μm;
S3, compacting and sintering: in above-mentioned fine powder, add lubricant, by the pulsed magnetic field of 3.0T-4.0T, the pressure orientation of 200-210MPa compressing under the protective atmosphere of nitrogen, then obtain neodymium iron boron magnetic body blank through discharge plasma sintering process;
S4, tempering heat treatment: above-mentioned neodymium iron boron magnetic body blank is carried out second annealing heat treatment and obtains neodymium iron boron magnetic body finished product; Wherein the temperature of first order tempering heat treatment is 870-900 DEG C, and temperature retention time is 2.5-3.5h, and the temperature of second level tempering heat treatment is 550-600 DEG C, and temperature retention time is 3.0-4.0h.
In the preparation method of the neodymium iron boron magnetic body of above-mentioned interpolation terbium powder, ferro-boron, industrial aluminium ingot, ingot iron and cathode copper that the gadolinium-iron alloy that the praseodymium neodymium alloy of to be Pr content the be 22%-28% of the furnace charge described in step S1, Gd content are 60%-65%, B content are 15%-20%.
In the preparation method of the neodymium iron boron magnetic body of above-mentioned interpolation terbium powder, the chill roll rotating speed in the process of the scale casting described in step S1 is 2.60m/s-2.70m/s.In traditional water-cooled copper mold casting ingot process, because cooling rate can not suppress peritectic reaction comparatively slowly, make in ingot casting, to there is more α-Fe phase, thus cause the ratio of principal phase to reduce, rich neodymium Entropy density deviation is uneven, is unfavorable for the generation of the bad phenomenon such as the raising of the magnetic property of NdFeB magnet.Therefore, in order to effectively prevent the generation of above-mentioned bad phenomenon, having abandoned traditional handicraft in the preparation method of neodymium iron boron magnetic body of the present invention and having adopted rapid casting casting ingot process to obtain getting rid of strap.And in rapid casting casting ingot process, the chill roll rotating speed in scale casting cycle for final magnet magnetic property particularly remanent magnetism have a great impact.If the rotating speed of chill roll is too low, get rid of composition generation segregation in strap crystalline structure, after part α-Fe separates out mutually, unnecessary rich neodymium phase and other non-magnetic phase can be formed, cause volume shared by principal phase to reduce, thus reduce remanent magnetism; If the rotating speed of chill roll is too high, then can form a large amount of polycrystalline particle after obtained powder, thus reduce remanent magnetism.Therefore, in order to obtain the NdFeB magnet of high magnetic characteristics, the chill roll rotating speed in scale casting cycle controls in suitable scope by the present invention.In addition, after furnace charge is put into vacuum rapid hardening smelting furnace, want first power transmission to carry out preheating before carrying out melting, to get rid of the adsorbed gas, organic substance etc. of furnace charge, thus make finally to obtain high-quality NdFeB magnet.
In the preparation method of the neodymium iron boron magnetic body of above-mentioned interpolation terbium powder, in the hydrogen break process described in step S2, the heating-up temperature of dehydrogenation reaction is 460-560 DEG C, and heating time is 200-230min.Compared with Mechanical Crushing flouring technology, hydrogen decrepitation can keep the integrality of crystal grain by the ratio reducing transgranular fracture in pulverizing process, and can suppress the abnormal growth of crystal grain in sintering process, thus effectively improves the combination property of magnet.For hydrogen decrepitation, its cardinal principle is rich neodymium phase and Nd
2fe
14b phase successively inhales hydrogen, causes volumetric expansion, and due to the difference of both expansion rates, cause producing internal stress at crystal grain intersection, along crystal boundary, alloy is then preferential occurs that crackle is broken for single crystal grain through External Force Acting.Hydrogen break process in the preparation method of neodymium iron boron magnetic body of the present invention comprises inhales hydrogen and dehydrogenation two processes, namely first to proceed in reaction vessel and pass into hydrogen and make it inhale hydrogen by getting rid of strap to 0.20-0.22MPa (pressure is the pressure under normal temperature state), until the stove heating of after no longer inhaling hydrogen, reactor being put into 460-560 DEG C is carried out dehydrogenation reaction and vacuumizes, stop after keeping 200-230min heating and being filled with argon gas, circulating water is adopted to reactor, cooling water temperature is 60-90 DEG C, obtains flour after being cooled to room temperature.
In the preparation method of the neodymium iron boron magnetic body of above-mentioned interpolation terbium powder, in step S2 after hydrogen break process, add the Tb powder of 0.10%-0.30% and the antioxidant of 0.035-0.040% in flour after, carry out airflow milling again.Tb can better mix with obtained flour in the form of a powder, and what the effect of Tb in NdFeB magnet was played is more abundant, effectively suppresses the growth of crystal grain, improves the coercive force etc. of final obtained NdFeB magnet.And adding of antioxidant, make the NdFeB magnet obtained have better non-oxidizability.Wherein, described antioxidant be triethanolamine borate, N-dodecyl bi-quaternary ammonium salt, tristerin one or more.
In the preparation method of the neodymium iron boron magnetic body of above-mentioned interpolation terbium powder, in order to reduce the friction between powder particle, preventing powder particle from reuniting thus improving the mobility of powder, after airflow milling, adding lubricant carry out orientation compacting again.But the addition of lubricant can not be too much, otherwise causing being difficult to deviate to reduce on the contrary magnet remanent magnetism and magnetic energy product completely when sintering, therefore in the present invention, the addition of lubricant being controlled at 0.020%-0.030%.Wherein, described lubricant is one or more in fat alcohol polyethylene ether, olein and lauryl sodium sulfate.In orientation and after pressing process, the present invention adopts discharge plasma sintering process to obtain neodymium iron boron magnetic body blank, wherein sintering atmosphere is vacuum degree is 0.01Pa-0.02Pa or argon gas atmosphere, sintering pressure is 30-40MPa, sintering temperature is 650-800 DEG C, heating rate is 150-180 DEG C/min, and temperature retention time is 5-10min.Discharge plasma sintering process is the pressure sintering method utilizing DC pulse resistance sintering; it can carry out in vacuum or protective atmosphere; have that programming rate is fast, sintering time is short, sintering temperature is low, uniform crystal particles, be conducive to controlling the fine structure of sintered body, and simple to operate, safe and reliable, energy savings, low cost and other advantages.In the preparation method of neodymium iron boron magnetic body of the present invention, sintering temperature, sintering pressure, heating rate and the temperature retention time quality to obtained NdFeB magnet has material impact, and the unreasonable of these parameters arranges the quality that all can reduce final NdFeB magnet.Programming rate is too fast, sintering temperature is too high, makes grain growth speed fast and causes crystal grain abnormal large, reducing the performance of magnet, otherwise then do not reach the quality requirement of magnet; Sintering pressure increases in right amount effectively can suppress growing up and reducing sintering temperature of crystal grain, but sintering pressure is excessive, can make on the contrary to reduce density and these beneficial effects; Temperature retention time is long, crystal grain can be made during this period of time sharply to grow up, reduce magnetic property, temperature retention time is too short, and the density of magnet can be caused to reduce, and therefore sintering temperature, sintering pressure, heating rate and temperature retention time all control in suitable scope by the present invention.In addition, in the preparation method of neodymium iron boron magnetic body of the present invention, after sintering second annealing heat treatment and surface treatment are carried out to magnet, make final neodymium iron boron magnetic body have better combination property.Wherein, surface treatment is the common surface treatment process in this area.
Compared with prior art, the present invention has following beneficial effect:
1) the present invention adds the neodymium iron boron magnetic body of terbium powder, on the basis being primary raw material with PrNd alloy, B and Fe, compositely add terbium powder, Gd and Al, Cu, by their reasonable disposition in NdFeB magnet and synergy, the NdFeB magnet obtained is made to have good corrosion resistance and mechanical property while having higher coercive force, remanent magnetism and magnetic energy product.
2) the present invention adds preparation method's simple possible of the neodymium iron boron magnetic body of terbium powder, and raw material is simple and easy to get, and by the reasonable set of each technological parameter, the good combination property of the NdFeB magnet obtained, production cost is lower.
Embodiment
Be below specific embodiments of the invention, technical scheme of the present invention is further described, but the present invention is not limited to these embodiments.
Table 1: embodiment 1-3 is for the preparation of the constituent of neodymium iron boron magnetic body and the mass percent of adding terbium powder
Embodiment 1
Batching and melting: prepare burden according to the constituent of neodymium iron boron magnetic body described in table 1 embodiment 1 and mass percent, then send into vacuum rapid hardening smelting furnace and power transmission preheating, be then evacuated down to 10
-3paPa, stops vacuumizing and being filled with after high-purity argon gas (content>=99.99%) reaches 0.045MPa and carries out melting, and after furnace charge melts completely, that carries out scale casting with the chill roll rotating speed of 2.60m/s to obtain average thickness be 0.20mm gets rid of strap; Ferro-boron, industrial aluminium ingot, ingot iron and cathode copper that the gadolinium-iron alloy that the praseodymium neodymium alloy of wherein said furnace charge to be Pr content be 22%-28%, Gd content are 60%-65%, B content are 15%-20%.
Hydrogen fragmentation and airflow milling process: the above-mentioned strap that gets rid of is obtained through hydrogen break process the flour that average grain diameter is 10.0 μm, then add Tb powder and 0.035% N-dodecyl bi-quaternary ammonium salt carry out airflow milling and obtain the fine powder that average grain diameter is 3.0 μm, stir 1.5-3.0h with mixer;
Wherein, hydrogen break process comprises inhales hydrogen and dehydrogenation two processes, namely first to proceed in reaction vessel and pass into high-purity hydrogen (content >=99.99%) and make it inhale hydrogen by getting rid of strap to 0.20MPa (pressure is the pressure under normal temperature state), until the stove heating of after no longer inhaling hydrogen, reactor being put into 460 DEG C is carried out dehydrogenation reaction and vacuumizes, stop after keeping 200min heating and being filled with argon gas, circulating water is adopted to reactor, cooling water temperature is 60 DEG C, obtains flour after being cooled to room temperature.
Compacting and sintering: in above-mentioned fine powder, add the olein of 0.020%, by the pulsed magnetic field of 3.0T, the pressure orientation of 200MPa compressing under the protective atmosphere of nitrogen, then obtain neodymium iron boron magnetic body blank through discharge plasma sintering process; Wherein in discharge plasma sintering process, sintering atmosphere is argon gas atmosphere, and sintering pressure is 30MPa, and sintering temperature is 650 DEG C, and heating rate is 150 DEG C/min, and temperature retention time is 5min.
Tempering heat treatment: above-mentioned neodymium iron boron magnetic body blank is carried out second annealing heat treatment and surface treatment obtains neodymium iron boron magnetic body finished product; Wherein the temperature of first order tempering heat treatment is 870 DEG C, and temperature retention time is 2.5h, and the temperature of second level tempering heat treatment is 550 DEG C, and temperature retention time is 3.0h.
Embodiment 2
Batching and melting: prepare burden according to the constituent of neodymium iron boron magnetic body described in table 1 embodiment 2 and mass percent, then send into vacuum rapid hardening smelting furnace and power transmission preheating, be then evacuated down to 6 × 10
-3pa, stops vacuumizing and being filled with after high-purity argon gas (content>=99.99%) reaches 0.048MPa and carries out melting, and after furnace charge melts completely, that carries out scale casting with the chill roll rotating speed of 2.65m/s to obtain average thickness be 0.40mm gets rid of strap; Ferro-boron, industrial aluminium ingot, ingot iron and cathode copper that the gadolinium-iron alloy that the praseodymium neodymium alloy of wherein said furnace charge to be Pr content be 22%-28%, Gd content are 60%-65%, B content are 15%-20%.
Hydrogen fragmentation and airflow milling process: the above-mentioned strap that gets rid of is obtained through hydrogen break process the flour that average grain diameter is 11.0 μm, then add Tb powder and the triethanolamine borate of 0.020% and the tristerin of 0.020% to carry out airflow milling and obtain the fine powder that average grain diameter is 4.0 μm, stir 2.5h with mixer;
Wherein, hydrogen break process comprises inhales hydrogen and dehydrogenation two processes, namely first to proceed in reaction vessel and pass into high-purity hydrogen (content >=99.99%) and make it inhale hydrogen by getting rid of strap to 0.21MPa (pressure is the pressure under normal temperature state), until the stove heating of after no longer inhaling hydrogen, reactor being put into 500 DEG C is carried out dehydrogenation reaction and vacuumizes, stop after keeping 210min heating and being filled with argon gas, circulating water is adopted to reactor, cooling water temperature is 75 DEG C, obtains flour after being cooled to room temperature.
Compacting and sintering: in above-mentioned fine powder, add the fat alcohol polyethylene ether of 0.025%, by the pulsed magnetic field of 3.5T, the pressure orientation of 205MPa compressing under the protective atmosphere of nitrogen, then obtain neodymium iron boron magnetic body blank through discharge plasma sintering process; Wherein in discharge plasma sintering process, sintering atmosphere is vacuum degree is 0.01Pa atmosphere, and sintering pressure is 35MPa, and sintering temperature is 720 DEG C, and heating rate is 160 DEG C/min, and temperature retention time is 8min.
Tempering heat treatment: above-mentioned neodymium iron boron magnetic body blank is carried out second annealing heat treatment and surface treatment obtains neodymium iron boron magnetic body finished product; Wherein the temperature of first order tempering heat treatment is 880 DEG C, and temperature retention time is 3.0h, and the temperature of second level tempering heat treatment is 580 DEG C, and temperature retention time is 3.5h.
Embodiment 3
Batching and melting: prepare burden according to the constituent of neodymium iron boron magnetic body described in table 1 embodiment 3 and mass percent, then send into vacuum rapid hardening smelting furnace and power transmission preheating, be then evacuated down to 10
-2pa, stops vacuumizing and being filled with after high-purity argon gas (content>=99.99%) reaches 0.050MPa and carries out melting, and after furnace charge melts completely, that carries out scale casting with the chill roll rotating speed of 2.70m/s to obtain average thickness be 0.50mm gets rid of strap; Ferro-boron, industrial aluminium ingot, ingot iron and cathode copper that the gadolinium-iron alloy that the praseodymium neodymium alloy of wherein said furnace charge to be Pr content be 22%-28%, Gd content are 60%-65%, B content are 15%-20%.
Hydrogen fragmentation and airflow milling process: the above-mentioned strap that gets rid of is obtained through hydrogen break process the flour that average grain diameter is 12.0 μm, then add Tb powder and 0.035% tristerin carry out airflow milling and obtain the fine powder that average grain diameter is 4.0 μm, stir 3.0h with mixer;
Wherein, hydrogen break process comprises inhales hydrogen and dehydrogenation two processes, namely first to proceed in reaction vessel and pass into high-purity hydrogen (content >=99.99%) and make it inhale hydrogen by getting rid of strap to 0.22MPa (pressure is the pressure under normal temperature state), until the stove heating of after no longer inhaling hydrogen, reactor being put into 540 DEG C is carried out dehydrogenation reaction and vacuumizes, stop after keeping 230min heating and being filled with argon gas, circulating water is adopted to reactor, cooling water temperature is 85 DEG C, obtains flour after being cooled to room temperature.
Compacting and sintering: in above-mentioned fine powder, add the fat alcohol polyethylene ether of 0.015% and the lauryl sodium sulfate of 0.015%, by the pulsed magnetic field of 4.0T, the pressure orientation of 210MPa compressing under the protective atmosphere of nitrogen, then obtain neodymium iron boron magnetic body blank through discharge plasma sintering process; Wherein in discharge plasma sintering process, sintering atmosphere is argon gas atmosphere, and sintering pressure is 40MPa, and sintering temperature is 760 DEG C, and heating rate is 170 DEG C/min, and temperature retention time is 6min.
Tempering heat treatment: above-mentioned neodymium iron boron magnetic body blank is carried out second annealing heat treatment and surface treatment obtains neodymium iron boron magnetic body finished product; Wherein the temperature of first order tempering heat treatment is 900 DEG C, and temperature retention time is 3.5h, and the temperature of second level tempering heat treatment is 600 DEG C, and temperature retention time is 4.0h.
Neodymium iron boron magnetic body obtained in embodiment 1-3 is carried out performance test, and with do not add terbium powder, the performance of the neodymium iron boron magnetic body that other conditions are identical and obtained with embodiment 1-3 compares, and result is as shown in table 2.
The neodymium iron boron magnetic body that table 2: embodiment of the present invention 1-3 obtains and the performance comparison result of neodymium iron boron magnetic body of not adding terbium powder
Comparative example 1-3 for not add terbium powder, the neodymium iron boron magnetic body that other conditions are identical and obtained with embodiment 1-3.
In sum, the neodymium iron boron magnetic body that the present invention adds terbium powder adopts rational chemical composition, by adding of Tb powder and Al, Cu etc., synergy is produced between each composition, the neodymium iron boron magnetic body obtained is not compared with adding the neodymium iron boron magnetic body of terbium powder, and its coercive force significantly improves, and then magnetic property is more stable for demagnetization curve rectangular degree height, remanent magnetism and magnetic energy product decline not obvious, and the good combination property such as corrosion resistance, mechanical property.
Specific embodiment described herein is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment, but can't depart from spirit of the present invention or surmount the scope that appended claims defines.
Claims (9)
1. one kind is added the neodymium iron boron magnetic body of terbium powder, it is characterized in that, the constituent of described neodymium iron boron magnetic body and mass percent are: PrNd:28.40%-28.80%, Gd:2.70%-2.90%, B:0.95%-0.98%, Al:0.70%-0.78%, Cu:0.22%-0.25%, Tb:0.10%-0.30%, and surplus is Fe.
2. the neodymium iron boron magnetic body of interpolation terbium powder according to claim 1, it is characterized in that, the component of described neodymium iron boron magnetic body and mass percent are: PrNd:28.60%, Gd:2.80%, B:0.97%, Al:0.74%, Cu:0.23%, Tb:0.20%, and surplus is Fe.
3. the preparation method adding the neodymium iron boron magnetic body of terbium powder as claimed in claim 1, it is characterized in that, described preparation method comprises the steps:
S1, batching and melting: prepare burden according to the constituent of neodymium iron boron magnetic body described in claim 1 and mass percent, be evacuated down to 10 after then sending into vacuum rapid hardening smelting furnace
-3pa-10
-2pa, stops vacuumizing and being filled with after argon gas reaches 0.045-0.050MPa and carries out melting, carry out after furnace charge melts completely scale casting obtain thickness be 0.20-0.50mm get rid of strap;
Broken and the airflow milling process of S2, hydrogen: the above-mentioned strap that gets rid of is obtained through hydrogen break process the flour that average grain diameter is 10.0 μm-12.0 μm, then adds Tb powder and antioxidant and carries out airflow milling and obtain the fine powder that average grain diameter is 3.0 μm-4.0 μm;
S3, compacting and sintering: in above-mentioned fine powder, add lubricant, by the pulsed magnetic field of 3.0T-4.0T, the pressure orientation of 200-210MPa compressing under the protective atmosphere of nitrogen, then obtain neodymium iron boron magnetic body blank through discharge plasma sintering process;
S4, tempering heat treatment: above-mentioned neodymium iron boron magnetic body blank is carried out second annealing heat treatment and obtains neodymium iron boron magnetic body finished product; Wherein the temperature of first order tempering heat treatment is 870-900 DEG C, and temperature retention time is 2.5-3.5h, and the temperature of second level tempering heat treatment is 550-600 DEG C, and temperature retention time is 3.0-4.0h.
4. the preparation method of the neodymium iron boron magnetic body of interpolation terbium powder according to claim 3, it is characterized in that, ferro-boron, industrial aluminium ingot, ingot iron and cathode copper that the gadolinium-iron alloy that the praseodymium neodymium alloy of to be Pr content the be 22%-28% of the furnace charge described in step S1, Gd content are 60%-65%, B content are 15%-20%.
5. the preparation method of the neodymium iron boron magnetic body of interpolation terbium powder according to claim 3, is characterized in that, the chill roll rotating speed in the process of the scale casting described in step S1 is 2.60m/s-2.70m/s.
6. the preparation method of the neodymium iron boron magnetic body of interpolation terbium powder according to claim 3, is characterized in that, in the hydrogen break process described in step S2, the heating-up temperature of dehydrogenation reaction is 460-560 DEG C, and heating time is 200-230min.
7. the preparation method of the neodymium iron boron magnetic body of interpolation terbium powder according to claim 3, is characterized in that, the addition of the antioxidant described in step S2 is 0.035%-0.040%.
8. the preparation method of the neodymium iron boron magnetic body of interpolation terbium powder according to claim 3, is characterized in that, the addition of the lubricant described in step S3 is 0.020%-0.030%.
9. the preparation method of the neodymium iron boron magnetic body of interpolation terbium powder according to claim 3, it is characterized in that, in discharge plasma sintering process described in step S3, sintering atmosphere is vacuum degree is 0.01Pa-0.02Pa or argon gas atmosphere, sintering pressure is 30-40MPa, sintering temperature is 650-800 DEG C, heating rate is 150-180 DEG C/min, and temperature retention time is 5-10min.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105903950A (en) * | 2016-05-23 | 2016-08-31 | 苏州思创源博电子科技有限公司 | Preparation method of nanometer neodymium iron boron magnetic material |
| CN106128668A (en) * | 2016-08-15 | 2016-11-16 | 深圳市威富多媒体有限公司 | A kind of preparation method of Nanocomposite rare earth permanent-magnetic material |
| CN106328367A (en) * | 2016-08-31 | 2017-01-11 | 烟台正海磁性材料股份有限公司 | Preparing method of R-Fe-B line sintering magnet |
| CN106409495A (en) * | 2015-06-24 | 2017-02-15 | 株式会社捷太格特 | Manufacturing method for magnet and magnet |
| WO2019056643A1 (en) * | 2017-09-20 | 2019-03-28 | 江民德 | Method for producing neodymium-iron-boron composite magnetic material |
| CN110233039A (en) * | 2018-03-05 | 2019-09-13 | 宁波招宝磁业有限公司 | A kind of method that terbium powder prepares high-performance neodymium-iron-boron magnet |
| CN110534280A (en) * | 2019-09-23 | 2019-12-03 | 广西科技大学 | A kind of preparation method of the performance Nd Fe B sintered magnet based on crystal boundary addition |
| CN111968850A (en) * | 2020-07-15 | 2020-11-20 | 西安工程大学 | Method for preparing high-coercivity neodymium-iron-boron permanent magnet material by discharge plasma sintering |
| WO2023207019A1 (en) * | 2022-04-29 | 2023-11-02 | 福建省长汀金龙稀土有限公司 | Neodymium-iron-boron magnet material, preparation therefor, and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002030378A (en) * | 2000-07-17 | 2002-01-31 | Sumitomo Special Metals Co Ltd | Method for producing iron-based permanent magnet alloy by control of crystallization heat generating temperature |
| CN103258634A (en) * | 2013-05-30 | 2013-08-21 | 烟台正海磁性材料股份有限公司 | Method for preparing high-performance R-Fe-B system sintering magnetic body |
| CN103956244A (en) * | 2014-05-14 | 2014-07-30 | 辽宁五寰科技发展有限公司 | Preparation method for high-coercivity sintered neodymium-iron-boron |
-
2014
- 2014-11-26 CN CN201410695601.9A patent/CN104575901A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002030378A (en) * | 2000-07-17 | 2002-01-31 | Sumitomo Special Metals Co Ltd | Method for producing iron-based permanent magnet alloy by control of crystallization heat generating temperature |
| CN103258634A (en) * | 2013-05-30 | 2013-08-21 | 烟台正海磁性材料股份有限公司 | Method for preparing high-performance R-Fe-B system sintering magnetic body |
| CN103956244A (en) * | 2014-05-14 | 2014-07-30 | 辽宁五寰科技发展有限公司 | Preparation method for high-coercivity sintered neodymium-iron-boron |
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| CN106409495A (en) * | 2015-06-24 | 2017-02-15 | 株式会社捷太格特 | Manufacturing method for magnet and magnet |
| CN105903950A (en) * | 2016-05-23 | 2016-08-31 | 苏州思创源博电子科技有限公司 | Preparation method of nanometer neodymium iron boron magnetic material |
| CN106128668A (en) * | 2016-08-15 | 2016-11-16 | 深圳市威富多媒体有限公司 | A kind of preparation method of Nanocomposite rare earth permanent-magnetic material |
| CN106328367A (en) * | 2016-08-31 | 2017-01-11 | 烟台正海磁性材料股份有限公司 | Preparing method of R-Fe-B line sintering magnet |
| CN106328367B (en) * | 2016-08-31 | 2017-11-24 | 烟台正海磁性材料股份有限公司 | A kind of preparation method of R Fe B based sintered magnets |
| WO2019056643A1 (en) * | 2017-09-20 | 2019-03-28 | 江民德 | Method for producing neodymium-iron-boron composite magnetic material |
| CN110233039A (en) * | 2018-03-05 | 2019-09-13 | 宁波招宝磁业有限公司 | A kind of method that terbium powder prepares high-performance neodymium-iron-boron magnet |
| CN110534280A (en) * | 2019-09-23 | 2019-12-03 | 广西科技大学 | A kind of preparation method of the performance Nd Fe B sintered magnet based on crystal boundary addition |
| CN111968850A (en) * | 2020-07-15 | 2020-11-20 | 西安工程大学 | Method for preparing high-coercivity neodymium-iron-boron permanent magnet material by discharge plasma sintering |
| WO2023207019A1 (en) * | 2022-04-29 | 2023-11-02 | 福建省长汀金龙稀土有限公司 | Neodymium-iron-boron magnet material, preparation therefor, and application thereof |
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