CN102107277B - Process and equipment for preparing anisotropic rare-earth permanent-magnet powder and product prepared thereby - Google Patents
Process and equipment for preparing anisotropic rare-earth permanent-magnet powder and product prepared thereby Download PDFInfo
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- CN102107277B CN102107277B CN 200910244362 CN200910244362A CN102107277B CN 102107277 B CN102107277 B CN 102107277B CN 200910244362 CN200910244362 CN 200910244362 CN 200910244362 A CN200910244362 A CN 200910244362A CN 102107277 B CN102107277 B CN 102107277B
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Abstract
The invention relates to a process and equipment for preparing anisotropic rare-earth permanent-magnet powder and a product prepared thereby. The equipment for preparing the magnetic powder comprises three parts, namely a heating and magnetic field orientation system, a flow control system and a vacuum system. The preparation process comprises the following steps of: putting rare earth elements containing Sc and Y and rare earth alloy which takes boron and iron as principal components into the preparation equipment, and performing high-temperature hydrogen treatment at the temperature of between 650 and 900 DEG C under the hydrogen partial pressure of 10 to 90 kPa; and performing multi-step dehydrogenation at the temperature of between 750 and 950 DEG C under a certain magnetic field. Through the method, magnetic powder grains can be refined, and anisotropy and magnetic property are improved.
Description
Technical field
The present invention relates to a kind of preparation technology and device and product of anisotropy rare earth permanent magnet powder, be specifically related in the magnetic preparation process, apply magnetic field and improve the associated magnetic performances such as degree of anisotropy.
Technical background
NdFeB Bonded Magnets has excellent magnetic property, mechanical performance, good machinability, has very large application and development future, market demand phenomenal growth has been widely used in automobile, computer peripheral equipment, electronics, office automation and other electronic devices at present.Bonded rare earth permanent magnetic is mainly used in stator or the rotor magnet of various micromachines in information industry, information products require micromachine to export higher power when reducing volume, therefore require magnet to have higher magnetic property, less, more accurate size.Consider above factor, selecting on unique basis that reaches practical rare-earth iron-based permanent magnetism NdFeB that anisotropy permanent magnetism is an inevitable developing direction of bonded permanent magnet.The anisotropic magnetic powder, preparation method thereof is exactly the method by HDDR except the forge hot casting, and the method is the NdFeB virgin alloy to be heated to 750～950 ℃ carry out hydrogen abstraction reaction in hydrogen, makes principal phase Nd
2Fe
14Disproportionation occurs and decomposes in B, makes after this dehydrogenation program of disproportionation phase releasing hydrogen gas generation reverse transformation, obtains the tiny anisotropic magnetic powder of crystal grain.
The parameter of investigating anisotropic magnet powder mainly contains coercivity iHc, remanent magnetism Br and degree of anisotropy etc.Wherein iHc is relevant with the magnetic grain size, and the less degree of anisotropy of crystal grain is just larger; Remanent magnetism Br depends primarily on degree of anisotropy, and crystal orientation is more consistent, and namely degree of anisotropy is higher, and remanent magnetism Br is just larger, and end reaction is that magnetic energy product (BH) m is just larger.
Degree of anisotropy can represent with DOA (Degree Of Alignment), be formulated as:
DOA＝(Br
//-Br
⊥)Br
//
In the formula: Br
//Expression is parallel to the remanent magnetism that the magnetic field orientating direction obtains
Br
⊥The remanent magnetism that expression obtains perpendicular to the magnetic field orientating direction
Isotropic magnetic DOA=0, the sample DOA=1 that is orientated fully, DOA is larger, and the anisotropy of material is stronger, is impossible but in fact reach 1.Aspect the preparation method of anisotropic magnet powder, like to know that there has been patent application in the company such as steel processed.Mitsubishi has found that at first the HDDR method of NdFeB produces anisotropic magnet powder, its in 88106845.4 and 92113705.2 SEPARATE APPLICATION microstructure patent and technique patent; And like to know that steel processed has further developed HDDR technique, proposing RFeB in 01140696.8 patent is hydride (RFeBHx) and the R1 element (monomer of one or more compositions among Tb, Dy, Nd, the Pr, alloy, compound or consisting of spread powder) mix, the anisotropic magnet powder that counterdiffusion obtains high-coercive force is carried out in heat treatment; In 96103173.5, for the uppity problem of temperature in the HDDR technique, propose to carry out opposite reaction with a kind of compensative material and produce the heat that absorbs when identical heat balance rare earth magnet powders is inhaled the heat of hydrogen generation and dehydrogenation.99123355.7 effect and the multistep hydrogen treatment process of middle proposition Nb and Ga propose in 20048001073.7 and 200510070024.5 to increase after the stage in disproportionation and organize stabilization process, and prepare (R with this technique
1-xLa
x)
12-14Fe
BalB
9-10It is the high-temperature stability anisotropic powder; 200410085531.1 propose the technique that Anisotropy NdFeB Powder and SmFeN powder are mixed and made into the magnetic of high magnetic characteristics.
Aspect the anisotropic magnet powder Preparation equipment, like to know that steel processed applied for a kind of anisotropic magnet powder Preparation equipment in 96103173.5, synchronously carry out opposite reaction with a kind of compensative material and produce the heat that absorbs when identical heat comes the balanced heat that produces during owing to described rare earth magnet powders suction hydrogen and dehydrogenation.98125398.9 middle adding thermal compensation device and a bearing part, bearing part makes reaction raw materials move up and down to enhance productivity.Domestic patent 200710061622.5 has also proposed a kind of externally heating type rotating vacuum furnace, has guaranteed the uniformity of reaction and the accurate control of temperature.
Above-mentioned domestic and international patent or relevant anisotropic magnetic powder preparation technique patent, or relevant magnet prepares related magnetic preparation technology in the patent, or the preparation facilities of magnetic, the preparation technology that all to have related to some extent relevant rare earth R-T-B be anisotropic magnet powder.But all do not relate to and in preparation process, apply magnetic field and improve the anisotropy of magnetic and the crystalline form situation for preparing magnetic by this kind method.
In the multiple processing procedure of different magnetic materials, all observe the phenomenon that high-intensity magnetic field is induced texture structure, aspect preparing for anisotropic magnet powder, the present magnetic anisotropy for preparing by traditional process is all below 0.6, and the magnetic particle capability loss is more.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of high anisotropy magnetic, the device of implementing the method and anisotropic magnet powder for preparing according to this device of preparing.
Can be known by theory of magnetism, magnetic field is by making the material magnetization, change thermodynamics and kinetics condition in the material processed process, even directly affect the behaviors such as migration, coupling, complexing of material Atom, molecule or ion, can produce on tissue, the microstructure and performance of material impact profound, essence.Concerning magnetic material, because magnetocrystalline anisotropy, apply magnetic field and can in material, produce the grain-oriented magnetocrystalline anisotropy energy of dependence, thereby for crystal boundary migration provides additional driving force, in Fe base alloy, because＜001〉direction magnetic conductivity is maximum, so its magnetocrystalline anisotropy energy is minimum, be that the free energy that magnetic field causes increases minimum, thereby promote the grain growth of＜001〉crystal orientation parallel magnetic field direction, therefore can needed texture orientation.
Apparatus of the present invention and method make hydrogenization method prepare anisotropic magnet powder an induced by magnetic field in certain embodiments, because when the crystal of composition material had obvious magnetic anisotropy, crystal was different with the magnetized energy of different crystallographic axis parallel magnetic fields.The difference of this magnetic energy is the driving force that crystal is orientated in magnetic field, therefore can use the texturing of induced by magnetic field material structure.The NdFeB material is through behind the high temperature hydrogenation process, and disproportionation tissue is understood under magnetic fields along the minimum crystal orientation preferential growth of magnetic energy, thereby makes the tissue that finally prepares have better magnetic anisotropy.
The technique that application apparatus of the present invention are carried out anisotropic magnet powder comprises following several steps:
(1) at first contain the rare-earth element R that comprises Sc and Y, and iron, the elements such as boron are the alloy of main component, are 10～90kPa in the pressure size, temperature range is that 650～900 ℃ of high temperature that carried out 30 minutes to 3 hours are inhaled the hydrogen processing procedure;
(2) to the product through obtaining after the high temperature hydrogen treatment operation, be that 0.1～10kPa and treatment temperature T2 are under 750～950 ℃ the condition at the permanent magnetic field, the hydrogen dividing potential drop P2 that keep applying 0.05-10kOe, carry out dehydrogenation operation under the magnetic field that 0.1～3h processes;
(3) discharge with the hydrogen in the environment with through hydrogen residual in the product that obtains after the dehydrogenation operation processing under the magnetic field, and the vacuum of carrying out is forced the dehydrogenation operation;
(4) the pressure refrigerating work procedure that environment and product is carried out.
This kind anisotropy rare earth permanent magnet powder preparation technique, the permanent magnetic field magnitude range that applies in step (2) is preferably 0.1-3kOe, and the duration is 0.1～2.5h.
This kind anisotropy rare earth permanent magnet powder preparation technique, the hydrogen dividing potential drop P2 scope that keeps in step (2) is 2-6kPa.
This kind rare earth aeolotropic rare earth permanent magnet powder preparation technique before above-mentioned high temperature hydrogen treatment operation, comprises that also with R-Fe-B be the low temperature hydrogenation treatment process that alloy carried out 30 minutes to 3 hours under 50-500 ℃ of temperature.
Force to get rid of the hydrogen in the reaction environment, carry out carrying out water-cooled or air-cooled after vacuum forces dehydrogenation to be processed, obtain the Magnaglo of high anisotropy degree, the chemical expression of described high anisotropy rare earth permanent magnet powder be (R '
1-xNd
x)
zM
yFe
100-z-y-δB
δ, wherein, the content of each composition in the formula is in atm%, and R ' is one or more in all rare earth elements that comprises Sc and Y except Nd, x=0～1; M is one or more in the following metallic element: Zr, Hf, Mn, Ti, Si, V, Co, Ni, Cr, Mo, Al, Nb, Ga, In, Cu and Zn, y=0～2, z=11.5～14, δ=6～12.
R ' is preferably one or both in all rare earth elements that comprises Sc and Y except Nd, R ' more preferably in the rare earth element of Pr, Dy, Gd, Ho, Ce and La one or both.M be preferably in Zr, Hf, Mn, Ti, Si, V, Co, Ni, Cr, Mo, Al, Nb, Ga, In, Cu and the Zn metallic element a kind of, two or three.
M is one or more in the following metallic element: Zr, Hf, Mn, Ti, Si, V, Co, Ni, Cr, Mo, Al, Nb, Ga, In, Cu and Zn, M be preferably in Zr, Hf, Mn, Ti, Si, V, Co, Ni, Cr, Mo, Al, Nb, Ga, In, Cu and the Zn metallic element a kind of, two or three.
The virgin alloy that is prepared anisotropic magnet powder is polycrystalline cast ingot or the rapid hardening thin slice that contains column crystal, virgin alloy for have (R '
1-xNd
x)
zM
yFe
100-z-y-δB
δThe content of each composition in the formula is in atm%; the 0.3mm of ratio of components～0.9mm rapid hardening thin slice or common ingot casting; with alloy through 900 ℃～1170 ℃; the Ar gas of 5～25h protection heat treatment or do not process is eliminated thick with α-Fe a small amount of in the alloy and make the abundant alligatoring to 50 of main phase grain broad ways～250 μ m.
Equipment provided by the invention is mainly by the magnetic field orientating heating system, flow control system, and vacuum system three parts form; Heating and magnetic field orientating system are provided with high temperature resistant quartz ampoule (1) in body of heater (2), in the body of heater (2) and be provided with heating control apparatus (6) and thermocouple (5), outer wall at body of heater (2) is surrounded by water collar (4), around solenoid (3), solenoid power supply (7) connects solenoid (3) by magnetic field sensor (19) in water collar (4) outer peripheral; Water collar (4) connects water-cooling system by circulating water pipe (8); High temperature resistant quartz ampoule (1) is enclosed construction, and its entrance point is provided with the air inlet that is connected with air inlet pipe and the vacuum orifice that is connected with vacuum-pumping tube.
Flow control system is connected in series respectively pressure maintaining valve (9), Pressure gauge (13), flow stabilizing valve (10), flowmeter (12) and switch valve (11) by source of the gas and taps into afterwards tracheae and form.
Vacuum system is the import that is connected mechanical pump (18) by the outlet of diffusion pump (17), the outlet serial connection of mechanical pump (18) switching valve (14) of bleeding, and switch valve (15), vacuum meter (16), and be connected with vacuum-pumping tube.
The permanent magnetic field intensity that the solenoid of this apparatus characteristic (3) produces is regulated by solenoid power supply (7) in the 0.05-10kOe scope.
The environment facies of preparation anisotropic magnet powder of the present invention prepare environmental advantages to tradition:
1. has a magnetic field orientating device in the preparation facilities provided by the invention
Anisotropic magnet powder preparation facilities principal focal point concentrates on change temperature and pressure situation and obtains excellent anisotropic magnetic generally speaking, the method is induced crystal structure and forming core by applying magnetic field, the impact of the unmanageable temperature and pressure condition that weakened on magnetic particle capability.
2. preparation facilities provided by the invention has a flow control system
Preparation facilities provided by the invention has a flow control system, can be used by the trace of the flowmeter in the flow control system, flow stabilizing valve and vacuum system and the switching valve of bleeding in a large number, can accurately control reaction condition by experimental needs.
Description of drawings
Carry out multistep hydrogen in the situation of Fig. 1 magnetic field and process preparation anisotropic magnet powder schematic diagram.
The high temperature resistant quartz ampoule of being numbered among the figure: 1-, 2-heating furnace body, 3-solenoid, 4-water collar, 5-thermocouple, 6-heating control apparatus, 7-solenoid power supply, 8-circulating water pipe, 9-pressure maintaining valve, 10-flow stabilizing valve, 11-switch valve, 12-flowmeter, 13-Pressure gauge, 14-trace bleed in a large number switching valve, 15-switch valve, 16-vacuum meter, 17-diffusion pump, 18-mechanical pump, 19-magnetic field sensor.
Fig. 2 carries out the schematic diagram that magnetic field multistep hydrogen is processed the preparation anisotropic magnet powder, and wherein abscissa is the processing time, and ordinate is for processing hydrogen pressure and temperature.Time, temperature and hydrogen pressure scope that black matrix is partly processed for magnetic field, dotted line is cut apart magnetic field dehydrogenation and two stages of high temperature hydrogenation, and bullet is the end point of each stage of reaction.
The specific embodiment
The below is further described rare-earth magnetic of the present invention and preparation method thereof with example, will help to understand better characteristics and the advantage of middle rare earth magnetic of the present invention.Protection domain of the present invention is not limited by the following examples, and protection scope of the present invention is determined by claims.
(1) implements alloy
Choose rare earth alloy (R '
1-xNd
x)
zM
yFe
100-z-y-δB
δ(atm%) alloy cast ingot or rapid hardening thin slice, rare earth element mainly is comprised of Nd, in all Sc, Y and lanthanide, Nd
2Fe
14B each side magnetic property is the highest, but the adding of other rare earth elements is to Nd
4Fe
14The B coercivity, the aspect performances such as temperature stability are improved effect, add other rare earth elements on the basis of this patent rare earth Nd and carry out certain modification, wherein optimum element is Pr, Gd, Ho, Dy etc., wherein the adding of Gd, Ho has certain effect to improving temperature stability, and the adding of Dy can improve the coercivity of magnetic.
In addition, NdFeB is to be iron as main component in the alloy, and when all as 100atm%, ideal is to contain the R of 10～14atm% and the B of 6～12atm%, if Nd content is lower than 10atm%, α-Fe will separate out mutually, causes magnetic property to descend; If Nd content surpasses 14atm%, R
2Fe
14B will reduce mutually, equally also cause magnetic property to descend.On the other hand, if the content of B is lower than 6atm%, R
2Fe
17To separate out mutually, and cause magnetic property to descend, B content surpasses 12atm%, R
2Fe
14B reduces mutually, equally also causes magnetic property to descend.B content is higher than 10atm%, can suppress separating out of a-Fe.
The adding of transition element M is mainly the partial properties of improving magnetic, is the effective element that improves remanent magnetism such as Nb, and Ga has very important effect to the coercivity that improves magnetic, and wherein the content of Ga is preferably 0.01%～2at%, and optimum content is 0.1～0.6at%.If Ga contains quantity not sufficient 0.01%, the effect of modification will be can not get; On the other hand, the content of Ga surpasses 2at%, causes conversely the minimizing of iHc.The content of Nb is preferably 0.01%～1at%, and optimum content is 0.1～0.4at%, if Nb contain quantity not sufficient 0.01%, the effect of modification will be can not get, Nb content surpasses 1atm%, cause the passivation of high temperature disproportionated reaction, and compound interpolation Ga and Nb can improve magnetic coercivity and degree of anisotropy.
Generally speaking, among Zr, Hf, Mn, Ti, Si, V, Co, Ni, Cr, Mo, Al, Nb, Ga, In, Cu, the Zn one or more, the performances such as the anisotropy that improves magnetic and coercivity are played an important role, content preferably is controlled within the 2atm% scope, content is crossed the major general and is made DeGrain, content too much will the rare earth dephasign, causes magnetic property to descend.
Quartz ampoule 1 is put in the coarse crushing after annealing of above-mentioned alloy, seals quartz ampoule 1, as shown in Figure 1.The Main Function of annealing is dephasign content in the reduction alloy, homogenising tissue etc., and the crystal grain of growing up simultaneously has certain booster action to the HDDR process.
(2) preparation technology
Begin to open vacuum system after checking the gas circuit connection, as shown in Figure 1, open successively trace bleed in a large number switching valve 14, switch valve 15, vacuumize with diffusion pump 17 and mechanical pump 18, after the vacuum that vacuum meter 16 is surveyed reaches setting value, close vacuum system; Open air-channel system, open successively pressure maintaining valve 9, flow stabilizing valve 10, switch valve 11, be filled with hydrogen, wherein, flowmeter 12 can be surveyed the flow of the hydrogen that enters quartz ampoule 1, and Pressure gauge 13 can be surveyed the pressure that is filled with hydrogen.Carry out the processing of multistep hydrogen according to the technique that sets and carry out the preparation of anisotropic magnetic powder, wherein, control the pressure of the hydrogen of quartz ampoules 1 by pressure maintaining valve 9, flow stabilizing valve 10, switch valve 11; By the temperature in the heating control apparatus 6 control quartz ampoules 1; By magnetic field sensor 19 and electromagnet control device 7 control solenoids 3, with the intensity in the magnetic field in the control quartz ampoule 1; Water collar 4 connects water-cooling system by circulating water pipe 8, so that 2 coolings of control body of heater.
At first at 90～150kPa, the low temperature that carried out below 50-500 ℃ 30 minutes to 3 hours is inhaled hydrogen; Then at 10～90kPa, the high temperature that carried out 30 minutes to 3 hours under 650～900 ℃ of conditions is inhaled the hydrogen process; Under 0.05-10kOe magnetic field, carry out dehydrogenation processing under the magnetic field in 750～950 ℃ of scopes, then rapid cooling obtains high magnetic anisotropy, high performance magnetic after vacuum is forced dehydrogenation.
The effect that low temperature is inhaled hydrogen is mainly the hydrogen diffusion admittance of opening the high temperature disproportionation stage, makes the high temperature disproportionation more even.But concerning the RFeB alloy, it is not necessary operation that low temperature is inhaled hydrogen, and a small amount of raw material of processing also can carry out this operation simultaneously at hot stage, concerning the raw material of a large amount of processing, can carry out this low temperature hydrogenation process and carry out steady production.
High temperature is inhaled the hydrogen process at 10～90kPa, 650～900 ℃, carry out under 30 minutes to the 3 hours conditions, wherein hydrogen pressure is arranged on 10～90kPa scope, too high hydrogen pressure makes reaction speed too fast, is unfavorable for reacting evenly carrying out, when hydrogen pressure is lower than 10kPa, reaction does not reach thermodynamic power and learns condition, thereby makes reaction carry out difficulty.Temperature is in 650～900 ℃ of scopes, and temperature is below 650 ℃ the time, and reaction can not be carried out, and when surpassing 900 ℃, is difficult to separate out Fe from supersaturation Fe
2B, the simultaneous reactions excessive velocities is difficult to form needed tissue and structure, causes magnetic remanent magnetism to reduce.The time range of 30min～3h guarantees to react evenly carries out fully.
The magnetic field dehydrogenation again chemical combination the processing stage at 0.05～10kOe, carry out in 750～950 ℃ of scopes.Magnetic field greater than 10kOe is not only not obvious to improving the magnetic anisotropy, and is difficult to reach at equipment.Because dehydrogenation again chemical combination processing is the endothermic reaction, need to carry out under certain temperature range, temperature is lower than 750kPa makes the material dehydrogenation incomplete, also has the not disproportionation phase of complete reaction in the product, temperature is higher than 950 ℃ makes tiny grain growth behind the chemical combination again, reduces the magnetic coercivity.
Vacuum forces to adopt water-cooled or air-cooled after the dehydrogenation, makes material remain on the tiny crystal grain state of high temperature, avoids in cooling procedure crystal grain to grow up.
(3) equipment state
Use the device of preparation rare-earth magnetic under the magnetic field of the present invention as shown in Figure 1, high temperature resistant quartz ampoule 1 diameter is 5～20mm, length is 20～80mm, seals up quartz ampoule 1 after the alloy that needs to process of packing into, stays outlet and links to each other with vacuum system with flow control system.Heating furnace body 2 is in quartz ampoule 1 outside, and thermocouple 5 and links to each other with the heating control apparatus 6 of outside between heating furnace body 2 and quartz ampoule 1.Quartz ampoule 1, heating furnace body 2 are nested from inside to outside with outside electromagnet axis coinciding, and heating furnace body 2 and solenoid 3 are separated by heat-preservation cotton and water collar 4.The magnetic field that solenoid 3 produces is along quartz ampoule 1 axial direction, and magnetic field intensity can dynamically be controlled in the 0.05-10kOe scope by solenoid power supply 7.
Vacuum system adopts mechanical pump 17 and diffusion pump 18 to carry out compound vacuumizing, and flow control system adopts the flowmeter 12 of 0-80ml/min.The high vacuum of vacuum system reaches 2.5 * 10
-3Pa is by can also keeping the atmosphere that flows to the reaction quartz ampoule 1 interior hydrogen that slowly fills with being used of flowmeter 12.
Describe by the following examples this patent in detail.
Embodiment
(1) raw-material preparation
Be grouped into the one-tenth shown in the table 1; batch scale content of starting materials element or raw alloy; prepare and carry out induction melting or rapid hardening behind the material and get rid of band and obtain alloy; the annealing in process of then carrying out uniform temperature and time under the protection of argon gas makes alloy structure even, obtains particle diameter after the coarse crushing and is to carry out hydrogen in the corase meal access arrangement of 5-25mm and cause reaction treatment.In table 1, composition consists of atomic percent.
(2) preparation of anisotropic magnetic powder
After annealing and fragmentation, carry out the processing that hydrogen causes course of reaction according to the alloy of the composition proportion shown in the table 1.
Alloy is that the high temperature of processing under P1 and the treatment temperature T1 condition is inhaled the hydrogen operation keeping the hydrogen dividing potential drop;
Inhale the suction hydrogen product that obtains after the hydrogen operation is processed through high temperature, keep applying certain permanent magnetic field, the hydrogen dividing potential drop is under P2 and the treatment temperature T2 condition, dehydrogenation operation under the magnetic field of processing.
Discharge with the hydrogen in the environment with through hydrogen residual in the product that obtains after the dehydrogenation operation processing under the magnetic field, and the vacuum of carrying out is forced the dehydrogenation operation.
The pressure refrigerating work procedure that at last environment and product is carried out.
The condition that responds is as shown in table 2
So just prepare and have good anisotropic Magnaglo.
Gained magnetic powder particle size accounts for 90% of total amount between 25 μ m～1000 μ m.The magnetic crystalline form is mainly uniform column crystal, and column crystal volume ratio accounts for 90%, and grain size all below 300 μ m, is analyzed magnetic and magnet performance and seen Table 2.
Magnetic is estimated
Can find out by embodiment 1#-12#, the raising that every magnetic property and the degree of anisotropy by magnetic after the magnetic-field heat treatment all had a lot of degree, wherein degree of anisotropy is all more than 0.75.
Claims (9)
1. anisotropy rare earth permanent magnet powder preparation technique, it is characterized in that: this technique comprises following step:
(1) will contain the rare-earth element R that comprises Sc and Y and iron and boron is that the R-Fe-B of main component be alloy keeping hydrogen dividing potential drop P1 is that 10～90kPa and treatment temperature T1 are the high temperature hydrogen treatment operation of carrying out processing in 30 minutes to 3 hours under 650～900 ℃ the condition;
(2) to the product through obtaining after the high temperature hydrogen treatment operation, be that 0.1～10kPa and treatment temperature T2 are under 750～950 ℃ the condition at the permanent magnetic field, the hydrogen dividing potential drop P2 that keep applying 0.05-10kOe, carry out dehydrogenation operation under the magnetic field that 0.1～3h processes;
(3) discharge with the hydrogen in the environment with through hydrogen residual in the product that obtains after the dehydrogenation operation processing under the magnetic field, and the vacuum of carrying out is forced the dehydrogenation operation;
(4) the pressure refrigerating work procedure that environment and product is carried out.
2. according to anisotropy rare earth permanent magnet powder preparation technique claimed in claim 1, it is characterized in that: the permanent magnetic field magnitude range that applies in the step (2) is 0.1-3kOe, and the duration is 0.1～2.5h.
3. according to claims 1 described a kind of anisotropy rare earth permanent magnet powder preparation technique, it is characterized in that: the hydrogen dividing potential drop P2 scope that keeps in the step (2) is 2-6kPa.
4. according to rare earth aeolotropic rare earth permanent magnet powder preparation technique claimed in claim 1, it is characterized in that, before above-mentioned high temperature hydrogen treatment operation, comprise that also with R-Fe-B be the low temperature hydrogenation treatment process that alloy carried out 30 minutes to 3 hours under 50-500 ℃ of temperature.
5. employed equipment of anisotropy permanent magnetism powder preparation technique claimed in claim 1 is characterized in that: this equipment is by heating and magnetic field orientating system, and flow control system, vacuum system three parts form; Heating and magnetic field orientating system are provided with high temperature resistant quartz ampoule (1) in body of heater (2), heating control apparatus (6) and thermocouple (5), outer wall at body of heater (2) is surrounded by water collar (4), around solenoid (3), solenoid power supply (7) connects solenoid (3) by magnetic field sensor (19) in water collar (4) outer peripheral; Water collar (4) connects water-cooling system by circulating water pipe (8); High temperature resistant quartz ampoule (1) is enclosed construction, and its entrance point is provided with the air inlet that is connected with air inlet pipe and the vacuum orifice that is connected with vacuum-pumping tube.
6. according to equipment claimed in claim 5, it is characterized by and be: described flow control system is connected in series respectively pressure maintaining valve (9), Pressure gauge (13), flow stabilizing valve (10), flowmeter (11) and switch valve (12) by source of the gas and taps into afterwards tracheae and form.
7. according to equipment claimed in claim 5, it is characterized by and be: described vacuum system is the import that is connected mechanical pump (18) by the outlet of diffusion pump (17), the outlet of mechanical pump (18) is connected in series the switching valve (14) of bleeding, switch valve (15), vacuum meter (16), and be connected with vacuum-pumping tube.
8. according to equipment claimed in claim 5, it is characterized by and be: the permanent magnetic field intensity that solenoid (3) produces is regulated by solenoid power supply (7) in the 0.05-10kOe scope.
9. according to the anisotropy rare earth permanent magnet powder of preparation technology claimed in claim 1 preparation, it is characterized in that: the chemical expression of described anisotropy rare earth permanent magnet powder for (R '
1-xNd
x)
zM
yFe
100-z-y-δB
δ, wherein, the content of each composition in the formula is in atm%, and R ' is one or more in all rare earth elements that comprises Sc and Y except Nd, x=0.8～1; M is selected from the metallic element of Zr, Hf, Mn, Ti, Si, V, Co, Ni, Cr, Mo, Al, Nb, Ga, In, Cu and Zn one or more, y=0～2, z=11.5～14, δ=6～12; Described magnetic powder particle size accounts for 90% of total amount between 25 μ m～1000 μ m, the magnetic crystalline form is mainly uniform column crystal, and column crystal volume ratio accounts for 90%, and all below 300 μ m, the magnetic degree of anisotropy is more than 0.75 for grain size.
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| CN104342721A (en) * | 2014-10-28 | 2015-02-11 | 南京萨伯工业设计研究院有限公司 | Device and process for preparing rare-earth permanent-magnet material |
| CN108257751B (en) * | 2016-12-29 | 2021-02-19 | 北京中科三环高技术股份有限公司 | Alloy casting sheet for preparing fine-grain rare earth sintered magnet |
| CN108766701B (en) * | 2018-04-26 | 2020-08-21 | 安徽省瀚海新材料股份有限公司 | Crushing process of neodymium iron boron melt-spun piece |
| CN110767400B (en) * | 2019-11-06 | 2021-12-14 | 有研稀土新材料股份有限公司 | Rare earth anisotropic bonded magnetic powder, preparation method thereof and magnet |
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|---|---|---|---|---|
| JP2002025813A (en) * | 1999-06-28 | 2002-01-25 | Aichi Steel Works Ltd | Anisotropic rare earth magnet powder |
| CN101393791A (en) * | 2007-09-21 | 2009-03-25 | 有研稀土新材料股份有限公司 | Anisotropic magnetic powder and manufacturing method thereof |
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2009
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002025813A (en) * | 1999-06-28 | 2002-01-25 | Aichi Steel Works Ltd | Anisotropic rare earth magnet powder |
| CN101393791A (en) * | 2007-09-21 | 2009-03-25 | 有研稀土新材料股份有限公司 | Anisotropic magnetic powder and manufacturing method thereof |
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