CN104851542B - Method for preparing Ce-doped permanent magnetic material - Google Patents
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Abstract
The invention discloses a method for preparing a Ce-doped permanent magnetic material. The Ce-doped permanent magnetic material is composed of (CexNd1-x)a(Fe1-y-zZnySiz)100-a-b-cBbNbc, wherein x=0.56-0.75, y=0.20-0.22, z=0.03-0.05, a=25-28, b=1.5-1.8, and c=2-5. The Ce-doped permanent magnetic material prepared by the method is low in raw material cost, good in magnetic performance and high in resistivity.
Description
Art
The present invention relates to a kind of preparation method of the permanent-magnet material of cerium dopping.
Background technology
Magnetic material has the function of mutual to mechanical energy (information) and electromagnetic energy (information) phase transformation, extensively should at present
For the high-new skill such as computer, the network information, communication, Aero-Space, traffic, office automation, household electrical appliances, health and health care
Art field, and have become as one of important substance basis of new and high technology, new industry and social progress.In recent years, rare earth is forever
The application of magnet, makes the permasyn morot (pmsm) that structure is simple, power factor is high, starting torque is big progressively in each industry
Field substitutes traditional electrical excitation motor, and this also makes energy-saving electric machine manufacturing industry for the rush of demand of permanent-magnet material.
From ndfeb permanent-magnet material after in nineteen eighty-three, first time is reported, to the research of its magnetic property and preparation technology just
A large amount of development gets up, and ndfeb permanent-magnet material is magnetic permanent-magnet material the strongest so far, is with fastest developing speed on our times,
The best permanent-magnet material of market prospects.But, because the few price of metal nd reserves is high, bring to the application of ndfeb permanent-magnet material
Huge challenge.Therefore, it is necessary to adapt to the rare present situation of rare earth resources, explore novel magnetic materials, optimize magnet composition
On the basis of preparation technology, prepare cheap permanent-magnet material, reduce the purpose of the cost of raw material.Rare earth metal
Though cerium reserves larger, there is no big use, so price is cheaply a lot of with respect to praseodymium neodymium.
But, ce-fe-b permanent-magnet material is also conductor, in order to not cause irreversible heat to move back in the motor course of work
Magnetic, it is ensured that original magnetic flux, fundamentally solves the problems, such as the hot demagnetization of motor rare-earth permanent magnet it is necessary to reduce permanent magnet electricity
The eddy-current loss of machine.
Content of the invention
The present invention provides a kind of preparation method of the permanent-magnet material of cerium dopping, using the permanent-magnet material of the method preparation, tool
There is relatively low cost of material, and possess preferable magnetic property and higher resistivity.
To achieve these goals, the preparation method of the permanent-magnet material of a kind of cerium dopping that the present invention provides, this permanent magnetism material
Material possesses following alloying component: (cexnd1-x)a(fe1-y-zznysiz)100-a-b-cbbnbc, wherein x=0.56-0.75, y=0.20-
0.22, z=0.03-0.05, a=25-28, b=1.5-1.8, c=2-5, the method comprises the steps:
(1) foundry alloy preparation
By raw materials such as ce, nd, fe, zn, si, b, nb according to said ratio after the completion of, put into electric arc furnaces copper crucible (water simultaneously
Cold) in, close electric arc furnace cavity and be evacuated to 10-4-10-5Mbar, continuous gas washing 2-3 time, each gas washing is filled with high-purity ar air pressure
Power is 500-600mbar, and gas washing completes to be re-filled with high-purity ar gas 600-700mbar in rear chamber, continuous electricity consumption in fusion process
Arc agitation aluminium alloy, so as to abundant melt uniformly, is closed electric current after aluminium alloy cooling, is turned over alloy pig up and down with manipulator
Turn, repeat the above steps, melt back 5-6 time altogether, after cooling, obtain mother alloy ingot；
(2) rapid-hardening flake preparation
Ingot casting is placed in vacuum intermediate-frequency rapid hardening induction furnace, vacuumizes, be passed through argon gas, make ar pressure in stove reach-
Carry out melting after 0.05--0.06mpa, impose electromagnetic agitation refining after raw material all melt, subsequently molten steel is poured into line
Speed is in the water-cooled copper roller of 3-5m/s, prepares the rapid-hardening flake that average thickness is 0.2-0.3mm；
(3) base and orientation
Above-mentioned rapid-hardening flake is 1-3 μm through the micron powder particle diameter that hydrogen crushes and air-flow is milled into, then using fluorination
Dysprosium nano powder is the 3-6wt% of airflow milling raw material powder as solid surfactant, its additional proportion, is obtained by high-energy ball milling
There is the flaky powder of surface fluorination dysprosium insulating coating, High Energy Ball Milling Time wherein used is 3-4 hour, ratio of grinding media to material 10-15: 1,
Ball-milling medium is ethylene glycol；
Under argon gas protection atmosphere, by mixing magnetic oriented moulding in magnetic field intensity is for the magnetic field of 1.7-2.1t, then enter
Row isostatic cool pressing, makes blank, and isostatic pressed size is 280-320mpa；
(4) sinter
Molded blank is entered sintering furnace in argon gas protection down be sintered, first 600-750 is warming up to 5-10 DEG C/min
DEG C, it is incubated 3-4h, then 1000-1030 DEG C of sintering 4-5h is warming up to 10-15 DEG C/min, after being cooled to room temperature, carries out secondary
Temper, that is, respectively at 790-830 DEG C and 450-480 DEG C of tempering heat treatment 1-2h, obtains product.
Preferably, also include the step to rapid-hardening flake annealing after step (2), particularly as follows: after waiting copper roller cooling
Take out rapid-hardening flake, rapid-hardening flake is loaded in the quartz ampoule of an end closure, by vacuum sealing tube system gas washing, take out true after the completion of gas washing
The other end of quartz ampoule is closed after entering high-purity ar gas by empty refilling, opens 400 DEG C -750 DEG C of induction annealing stove design temperature, sensing
Frequency is 0.5-10khz, and heat treatment time is 10-20 minute；Afterwards quartz ampoule is pushed in core magnetic field annealing furnace, design temperature
400 DEG C -750 DEG C, magnetic field intensity be 1.5-3.7t, heat treatment time be 3-10 minute.
The Nd-Fe-B permanent magnet of present invention preparation, replaces nd by choosing cheap, resourceful ce, and combines conjunction
Golden component and the optimization of technological parameter, are prepared for ce based permanent magnetic material, its process is simple, and controllability is high, and raw material is cheap and easy to get, become
This is cheap, and obtained ce based permanent magnetic material is after making annealing treatment, and magnetic property is further substantially improved, for example fast quenching
Band coercivity improves nearly 2koe, and magnetic energy product improves 3mgoe；The high silicon of doped resistor rate on magnetic material surface in the material
Cover dysprosium fluoride to improve the internal resistance of material, improve the magnetic energy product of magnet using secondary pressed compact technique, finally in sintering process
Using double tempering technique, further increase the coercivity of material.
Specific embodiment
Embodiment one
The present embodiment permanent-magnet material possesses following alloying component: (ce0.56nd0.44)25(fe0.77zn0.2si0.03)71.5b1.5nb2.
By raw materials such as ce, nd, fe, zn, si, b, nb according to said ratio after the completion of, put into electric arc furnaces copper crucible (water simultaneously
Cold) in, close electric arc furnace cavity and be evacuated to 10-4-10-5Mbar, continuous gas washing 2 times, each gas washing is filled with high-purity ar atmospheric pressure
For 500mbar, gas washing completes to be re-filled with high-purity ar gas 600mbar in rear chamber, constantly stirs alloy with electric arc in fusion process
Liquid, so as to abundant melt uniformly, is closed electric current after aluminium alloy cooling, is spun upside down alloy pig with manipulator, repeat above-mentioned
Step, melt back 5 times altogether, obtain mother alloy ingot after cooling.
Ingot casting is placed in vacuum intermediate-frequency rapid hardening induction furnace, vacuumizes, be passed through argon gas, make ar pressure in stove reach-
Carry out melting after 0.05mpa, impose electromagnetic agitation refining after raw material all melt, subsequently molten steel being poured into linear velocity is
In the water-cooled copper roller of 3m/s, prepare the rapid-hardening flake that average thickness is 0.2-0.3mm.
Take out rapid-hardening flake after waiting copper roller cooling, rapid-hardening flake is loaded in the quartz ampoule of an end closure, by vacuum sealing tube
System gas washing, vacuumizes after the completion of gas washing and after being re-filled with high-purity ar gas closes the other end of quartz ampoule.Open induction annealing stove
400 DEG C of design temperature, induction frequencies are 1khz, and heat treatment time is 10 minutes；Afterwards quartz ampoule is pushed in core magnetic field annealing furnace,
400 DEG C DEG C of design temperature, magnetic field intensity are 1.5t, and heat treatment time is 3 minutes.
Above-mentioned rapid-hardening flake is 1-3 μm through the micron powder particle diameter that hydrogen crushes and air-flow is milled into, then using fluorination
As solid surfactant, its additional proportion is the 3wt% of airflow milling raw material powder to dysprosium nano powder, obtains tool by high-energy ball milling
There is the flaky powder of surface fluorination dysprosium insulating coating, High Energy Ball Milling Time wherein used is 3 hours, ratio of grinding media to material 10: 1, and ball milling is situated between
Matter is ethylene glycol；Under argon gas protection atmosphere, by mixing magnetic oriented moulding in magnetic field intensity is for the magnetic field of 1.7t, then carry out
Isostatic cool pressing, makes blank, and isostatic pressed size is 280mpa.
Molded blank is entered sintering furnace in argon gas protection down be sintered, be first warming up to 600 DEG C with 5 DEG C/min, insulation
3h, is then warming up to 1000 DEG C of sintering 4-5h with 10 DEG C/min, after being cooled to room temperature, carries out double tempering process, exist respectively
790 DEG C and 450 DEG C of tempering heat treatment 1h, obtain product.
Embodiment two
The present embodiment permanent-magnet material possesses following alloying component: (ce0.75nd0.25)28(fe0.73zn0.22si0.05)63.2b1.8nb5.
By raw materials such as ce, nd, fe, zn, si, b, nb according to said ratio after the completion of, put into electric arc furnaces copper crucible (water simultaneously
Cold) in, close electric arc furnace cavity and be evacuated to 10-5Mbar, continuous gas washing 3 times, each gas washing is filled with high-purity ar atmospheric pressure and is
600mbar, gas washing completes to be re-filled with high-purity ar gas 700mbar in rear chamber, constantly stirs aluminium alloy with electric arc in fusion process,
So that it is fully melted uniformly, close electric current after aluminium alloy cooling, with manipulator, alloy pig is spun upside down, repeat above-mentioned step
Suddenly, melt back 6 times altogether, obtain mother alloy ingot after cooling.
Ingot casting is placed in vacuum intermediate-frequency rapid hardening induction furnace, vacuumizes, be passed through argon gas, make ar pressure in stove reach-
Carry out melting after 0.06mpa, impose electromagnetic agitation refining after raw material all melt, subsequently molten steel being poured into linear velocity is
In the water-cooled copper roller of 5m/s, prepare the rapid-hardening flake that average thickness is 0.2-0.3mm.
Take out rapid-hardening flake after waiting copper roller cooling, rapid-hardening flake is loaded in the quartz ampoule of an end closure, by vacuum sealing tube
System gas washing, vacuumizes after the completion of gas washing and after being re-filled with high-purity ar gas closes the other end of quartz ampoule.Open induction annealing stove
750 DEG C of design temperature, induction frequencies are 10khz, and heat treatment time is 20 minutes；Afterwards quartz ampoule is pushed core magnetic field annealing furnace
In, 750 DEG C of design temperature, magnetic field intensity are 3.7t, and heat treatment time is 10 minutes.
Above-mentioned rapid-hardening flake is 1-3 μm through the micron powder particle diameter that hydrogen crushes and air-flow is milled into, then using fluorination
As solid surfactant, its additional proportion is the 6wt% of airflow milling raw material powder to dysprosium nano powder, obtains tool by high-energy ball milling
There is the flaky powder of surface fluorination dysprosium insulating coating, High Energy Ball Milling Time wherein used is 4 hours, ratio of grinding media to material 15: 1, and ball milling is situated between
Matter is ethylene glycol；Under argon gas protection atmosphere, by mixing magnetic oriented moulding in magnetic field intensity is for the magnetic field of 2.1t, then carry out
Isostatic cool pressing, makes blank, and isostatic pressed size is 320mpa.
Molded blank is entered sintering furnace in argon gas protection down be sintered, be first warming up to 750 DEG C with 10 DEG C/min, insulation
4h, is then warming up to 1030 DEG C of sintering 5h with 15 DEG C/min, after being cooled to room temperature, carries out double tempering process, that is, respectively 830
DEG C and 480 DEG C of tempering heat treatment 2h, obtain product.
Comparative example
Using rapid hardening rejection tablet vacuum induction melting furnace, by NdFeB material (prnd)29.95(fealcu)68.98b1.07In argon gas
Under protection, melting at a temperature of 1480 ~ 1550 DEG C, the molten steel of fusing is cast on the cooling copper rod of rotation, prepare 0.3 ~
The Nd Fe B alloys thin slice of 0.5mm thickness；Using hydrogen broken furnace, depress in 0.1mpa hydrogen and inhale hydrogen, 550 DEG C of temperature dehydrogenations, crush
Become 130 μm of Nd Fe B alloys powder；Above powder is broken into the Nd-Fe-B powder of 4 μm of particle mean size further across airflow milling
End；5 μm of lanthanum cerium alloy powder are added to 3) described in powder in, mix powder 3 hours using three-dimensional material mixer it is ensured that two kinds of powder
End uniformly mixes；Wherein, in lanthanum cerium alloy powder lanthanum cerium weight than for 64.7:35.3, the adding proportion of lanthanum cerium alloy powder is
The 1.52% of Nd Fe B alloys powder weight；Using Magnetic field press, by the powder that mixes be orientated under the magnetic field of 1.7t
Type, then through isostatic cool pressing, pressure is 200mpa, obtaining density is 4.68g/cm3Pressed compact；Shaping pressed compact is placed in vacuum burn
In freezing of a furnace, in 1075 DEG C of sintered heat insulatings 3 hours, in 890 DEG C of one-levels tempering insulations 2 hours, it is incubated 3 in 560 DEG C of second annealings little
When, obtaining final nominal composition is (prnd)29.95(fealcu)68.98b1.07Sintered magnet.
The permanent magnet of embodiment 1-2 to same shape and size and comparative example carries out magnetism testing and internal resistance is surveyed
Examination, is tested at 25 DEG C, measurement maximum magnetic energy product (bh)maxAnd coercivity.Test result shows: the maximum magnetic flux of embodiment 1-2
Energy product relatively example improves 20-25%, and coercivity relatively example improves more than 20%, and internal resistance improves more than 40%.
Above content is to further describe it is impossible to assert with reference to specific preferred embodiment is made for the present invention
Being embodied as of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of present inventive concept, make some equivalent substitutes or obvious modification, and performance or purposes are identical, all should
It is considered as belonging to protection scope of the present invention.
Claims (1)
1. a kind of preparation method of the permanent-magnet material of cerium dopping, this permanent-magnet material possesses following alloying component: (cexnd1-x)a
(fe1-y-zznysiz)100-a-b-cbbnbc, wherein x=0.56-0.75, y=0.20-0.22, z=0.03-0.05, a=25-28, b=
1.5-1.8, c=2-5, the method comprises the steps:
(1) foundry alloy preparation
After the completion of ce, nd, fe, zn, si, b, nb raw material proportioning, put in electric arc furnaces copper crucible simultaneously, close electric arc furnace cavity
It is evacuated to 10-4-10-5Mbar, continuous gas washing 2-3 time, it is 500-600mbar that each gas washing is filled with high-purity ar atmospheric pressure, gas washing
Complete in rear chamber, to be re-filled with high-purity ar gas 600-700mbar, constantly stir aluminium alloy with electric arc in fusion process so as to fully
Fusing uniformly, is closed electric current after aluminium alloy cooling, is spun upside down alloy pig with manipulator, repeat the above steps, altogether instead
Remelt refines 5-6 time, obtains mother alloy ingot after cooling；
(2) rapid-hardening flake preparation
Ingot casting is placed in vacuum intermediate-frequency rapid hardening induction furnace, vacuumizes, be passed through argon gas, make ar pressure in stove reach -0.05--
Carry out melting after 0.06mpa, impose electromagnetic agitation refining after raw material all melt, subsequently melt is poured into linear velocity
For in the water-cooled copper roller of 3-5m/s, preparing the rapid-hardening flake that average thickness is 0.2-0.3mm；
(3) base and orientation
Above-mentioned rapid-hardening flake is 1-3 μm through the micron powder particle diameter that hydrogen crushes and air-flow is milled into, then is received using dysprosium fluoride
As solid surfactant, its additional proportion is the 3-6wt% of airflow milling raw material powder to ground rice, is obtained by high-energy ball milling and has
The flaky powder of surface fluorination dysprosium insulating coating, High Energy Ball Milling Time wherein used is 3-4 hour, ratio of grinding media to material 10-15: 1, ball milling
Medium is ethylene glycol；
Under argon gas protection atmosphere, by mixing magnetic oriented moulding in magnetic field intensity is for the magnetic field of 1.7-2.1t, then carry out cold
Isostatic pressed, makes blank, and isostatic pressed size is 280-320mpa；
(4) sinter
Molded blank is entered sintering furnace in argon gas protection down be sintered, be first warming up to 600-750 DEG C with 5-10 DEG C/min, protect
Warm 3-4h, is then warming up to 1000-1030 DEG C of sintering 4-5h with 10-15 DEG C/min, after being cooled to room temperature, carries out at double tempering
Reason, that is, respectively at 790-830 DEG C and 450-480 DEG C of tempering heat treatment 1-2h, obtains product；
Wherein, also include the step to rapid-hardening flake annealing after step (2), particularly as follows: taking out speed after waiting copper roller cooling
Solidifying piece, rapid-hardening flake is loaded in the quartz ampoule of an end closure, by vacuum sealing tube system gas washing, vacuumizes and fill after the completion of gas washing
After entering high-purity ar gas, the other end of quartz ampoule is closed, open 400 DEG C -750 DEG C of induction annealing stove design temperature, induction frequencies are
0.5-10khz, heat treatment time is 10-20 minute；Afterwards quartz ampoule is pushed in core magnetic field annealing furnace, 400 DEG C of design temperature-
750 DEG C, magnetic field intensity be 1.5-3.7t, heat treatment time be 3-10 minute.
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| CN105931783A (en) * | 2016-06-27 | 2016-09-07 | 无锡新大力电机有限公司 | Preparation method for gadolinium-doped permanent magnet material |
| CN110323053B (en) * | 2018-03-30 | 2022-07-19 | 福建省长汀金龙稀土有限公司 | R-Fe-B sintered magnet and preparation method thereof |
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| JPS63255902A (en) * | 1987-04-13 | 1988-10-24 | Hitachi Metals Ltd | R-b-fe sintered magnet and manufacture thereof |
| CN103320665A (en) * | 2013-06-26 | 2013-09-25 | 沈冬杰 | Preparation method of samarium cobalt-based permanent magnet material |
| CN103474225A (en) * | 2013-07-20 | 2013-12-25 | 南通万宝实业有限公司 | Preparation method of neodymium-iron-boron magnet doped with dysprosium and cerium |
| CN104593666A (en) * | 2015-01-09 | 2015-05-06 | 梁玲 | Preparation method of lanthanum-doped iron-cobalt-base soft magnetic material |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2753431B2 (en) * | 1992-10-28 | 1998-05-20 | ゼネラル・モーターズ・コーポレーション | Sintered permanent magnet |
| CN104103393A (en) * | 2014-06-03 | 2014-10-15 | 宁波镨鸣磁业有限公司 | High-temperature resistance low-cost high-performance yttrium praseodymium cobalt iron boron sintered rare earth permanent magnet and multi-alloy preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63255902A (en) * | 1987-04-13 | 1988-10-24 | Hitachi Metals Ltd | R-b-fe sintered magnet and manufacture thereof |
| CN103320665A (en) * | 2013-06-26 | 2013-09-25 | 沈冬杰 | Preparation method of samarium cobalt-based permanent magnet material |
| CN103474225A (en) * | 2013-07-20 | 2013-12-25 | 南通万宝实业有限公司 | Preparation method of neodymium-iron-boron magnet doped with dysprosium and cerium |
| CN104593666A (en) * | 2015-01-09 | 2015-05-06 | 梁玲 | Preparation method of lanthanum-doped iron-cobalt-base soft magnetic material |
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