CN104637643B - Bayan Obo is total to association raw ore mischmetal permanent-magnet material and preparation method thereof - Google Patents
Bayan Obo is total to association raw ore mischmetal permanent-magnet material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to one kind being total to rare-earth permanent magnet and preparation method thereof made of association raw ore mischmetal Bayan Obo, and the ingredient of the rare-earth permanent magnet is shown below：MMxFeyAzB, 2≤x≤2.5,11≤y≤14,0≤z≤0.6, MM are that Bayan Obo is total to association raw ore mischmetal, and A is the auxiliary alloy of nanometer, including one or more in Nd, Pr, Al, Cu element.The rare-earth permanent magnet can utilize powder metallurgical technique, fast quenching hot pressing thermal deformation technique to realize.The present invention proposes that developing new type resource saving rare-earth permanent magnet using Bayan Obo raw ore mischmetal substitutes traditional rare-earth permanent magnet, has the advantages of cheap, to reduce environmental pollution, the magnetic energy product range of gained magnet can fill up the scope of application blank of ferrite, SmCo rare-earth permanent magnets well in 20 ~ 40MGOe.
Description
Technical field
It the present invention relates to the use of Bayan Obo and be total to association raw ore mischmetal and directly prepare rare earth permanent-magnetic material and its method,
Belong to rare earth permanent-magnetic material preparation field.
Background technology
Rare earth permanent-magnetic material is indispensable material in fields such as national security, information, the energy, environmental protection, and China is dilute
Native permanent-magnet material produces the first big country.Show that Nd-Fe-B permanent magnet is applied in tradition according to correlation report（Loud speaker, magnetic separation, permanent magnetism
Motor, VCM, MRI etc.）Market penetration rate is up to 50% or more, and demand is in the steady growth phase, and annual growth is 10% or so.China
Global rare earth resource big country, packet header baiyuneboite content of rare earth occupies first place in the world, be most important rare earth permanent magnet raw material and
Production base, the mine are the rare more metal intergrowth mineral beds in the world, have the characteristics that poor, thin, miscellaneous, and Bayan Obo is total to companion
Not only contain praseodymium, neodymium, lanthanum, cerium in raw raw ore mischmetal, contains the heavy rare earth elements such as dysprosium, terbium simultaneously, rare earth element is with total companion
Raw form coexists with iron, and finds the mine distributed mutually consistent appearance of praseodymium, neodymium, lanthanum, cerium mischmetal element.Traditional rare-earth permanent magnet disappears
A large amount of low abundance, resource scarcity praseodymium, neodymium, samarium, dysprosium, terbium rare earth element are consumed, high abundance lanthanum, Ce elements are not utilized effectively
And largely overstock, that causes rare earth resources utilizes imbalance.And original technique do not account for rare earth element total association it is natural
Be formulated attribute, excessively pursue the purity of raw material, adopt-select in rare earth-separating-purifying-smelting process in cause serious ecological environment
Pollution and the wasting of resources.
Invention content
According to an aspect of the present invention, the present invention provides one kind and being directly total to association raw ore mischmetal system using Bayan Obo
Standby rare earth permanent-magnetic material and its method.
According to another aspect of the present invention, the auxiliary alloying pellet of nanometer is added in the present invention in rare-earth permanent magnet, reaches raising
While magnet performance, the purpose of metal praseodymium neodymium usage amount is significantly reduced.
One kind being total to rare-earth permanent magnet made of association raw ore mischmetal Bayan Obo, which is characterized in that the rare earth
The ingredient of permanent magnet is shown below：MMxFeyAzB, wherein 2≤x≤2.5,11≤y≤14,0≤z≤0.6, MM are white clouds Hubei Province
Rich association raw ore mischmetal altogether, Fe are ferro element, and A is the auxiliary alloy of nanometer, including one kind or several in Nd, Pr, Al, Cu element
Kind, B is boron element.
Preferably, the Bayan Obo is total to the natural constituent of association raw ore mischmetal and includes by weight percentage
Following rare earth composition：La:10%-30%、Ce:20%-60%、Pr:5%-10%、Nd:5%-15%、Sm:0-0.05%、Gd:0-0.04%、
Tb:0-0.01%、Dy:0-0.01%、Y:0-0.01%。
According to the present invention, it is by using novel choosing to baiyuneboite that Bayan Obo, which is total to association raw ore norium,
Mine method --- X-fluorescence sorts, and carries out separating-purifying as needed, directly smelts and obtains, wherein Bayan Obo is total to association raw ore
Norium includes natural constituent as shown in Table 1.It is important to note that the raw material white clouds used in the present invention
Pile of stones, earth or grass, which is total in association raw ore mischmetal, not only contains praseodymium, neodymium, lanthanum, cerium, while also containing the heavy rare earth elements such as dysprosium, terbium, rare earth
Element is coexisted in the form of total association with iron, and finds the mine distributed mutually consistent appearance of praseodymium, neodymium, lanthanum, cerium mischmetal element, rare earth element
Total association natural formula attribute to improve material comprehensive performance play the role of it is vital.
1. Bayan Obo of table is total to association raw ore mischmetal constituent
A kind of preparation method being total to rare-earth permanent magnet made of association raw ore mischmetal Bayan Obo, feature exist
In first to be directly total to association raw ore mischmetal MM preparations MM using Bayan OboxFeyB powder, then with the auxiliary alloying pellet of nanometer
It is prepared by mixing into MMxFeyAzB rare earth permanent-magnetic materials.
Preferably, the preparation method includes powder metallurgic method, hot pressing thermal deformation technique.
Wherein, powder metallurgic method has following steps：
（1）Feedstock processing：Raw material is surface-treated, ready raw material is mechanically removed into surface oxidation
Layer, wherein the raw material, which includes Bayan Obo, is total to association raw ore mischmetal MM；
（2）Dispensing：By step（1）Treated raw material mixed ingredients according to a certain percentage；It, first will be golden in process for preparation
The oxide and impurity of metal surface remove；
（3）It smelts：Dispensing is carried out in vaccum sensitive stove to be smelted into MMxFeyB ingot castings；Or by dispensing in vacuum induction speed
MM of the thickness between 0.1-1mm is made in solidifying stovexFeyB alloy sheets control it and form column crystal；
（4）Powder processed：, air-flow milling quick-fried using hydrogen, by MMxFeyB alloys are milled into the fine powder of 2.5 ~ 5 microns of sizes；
（5）Mixed powder：The auxiliary alloying pellet of nanometer is added to the MM preparedxFeyIn B powder, mixed in vacuum environment
Uniformly；
（6）Die mould：By step（5）The powder being mixed is pressed into certain shape, pressure 3T/cm in magnetic field2, magnetic field
H >15000 oersteds；
（7）Sintering：It is higher than 10 in vacuum degree-3It, will be by step in the vacuum environment of Pa（6）Obtained green compact is placed on hot place
It is sintered in reason stove, the sintering process is：It first is heated to keeping the temperature 1.5 ~ 2.5 hours at 560 ~ 630 DEG C by room temperature, then be risen
Temperature is warming up at 1050 ~ 1060 DEG C to keeping the temperature 2.5 ~ 3.5 hours at 860 ~ 930 DEG C and keeps the temperature 1.5 ~ 2.5 hours later, finally with
Stove takes out after being cooled to room temperature；
（8）Post isothermal treatment：It is higher than 10 in vacuum degree-3In the vacuum environment of Pa, by step（7）Obtained sintered body is by room
Temperature is increased to 870-890 DEG C, keeps the temperature 80-240 minutes, is cooled to room temperature later, then raises the temperature to 470-560 DEG C again,
After heat preservation 80-240 minutes, then it is cooled to room temperature；
（9）Magnetic-field heat treatment：It will be through step（8）It is 1.5-15T's that magnet after Post isothermal treatment, which is placed on magnetic field intensity,
Heat-treatment furnace is tempered in vacuum environment in 1000 ~ 1100 DEG C of temperature ranges.
Preferably, step（6）Middle magnetic field orientating is one of following method with forming method：Parallel punching block pressure, vertical steel
Molding, parallel punching block pressure and isostatic pressed, vertical steel molding and isostatic pressed.
Wherein, hot pressing thermal deformation technique has following steps：
（1）Dispensing：It is equipped with and is by weight percentage：MM：26-50%, Fe：49.5-72%, B：The master alloying of 0.5-2% is former
Material, wherein MM is that Bayan Obo is total to association raw ore mischmetal；
（2）Fast quenching：It will（1）In master alloying raw material melting fast quenching, by master alloying raw material be heated to after 1200 ~ 1250 DEG C with
The speed of quenching of 10-80m/s carries out fast quenching, and nozzle is round or elongated aperture, nozzle distance chill roll 2mm-10mm, gained fast quenching
Band vacuum heat -2 hours 1 minute at 300-1000 DEG C；
（3）Powder processed：It will（2）In master alloying rapid tempering belt ball milling obtain MM after 0.5-4 hoursxFeyB master alloying powder；It will be auxiliary
Alloy raw material Pr, Nd, PrNd, PrCu, NdCu and AlCu be quick-fried through hydrogen, after airflow milling, high-energy ball milling, and it is 10- to be milled into grain size
The auxiliary alloying pellet of nanometer that grain size is 10-500nm, auxiliary alloy is made through vaporization condensation process in the auxiliary alloying pellet of nanometer of 500nm
The mass percent of Cu is 1%-90% in raw material PrCu, NdCu and AlCu；
（4）Mixed powder：It will（3）Middle master alloying powder obtains mixed powder after being mixed with the auxiliary alloying pellet of nanometer, wherein nanometer
The mixed powder ratio of auxiliary alloying pellet is mass percent 0-8%；
（5）Hot pressing：It will（4）In mixed powder carry out hot pressing, the heat pressing process is：Hot pressing is vacuum environment,
Vacuum degree is higher than 10-3Pa, 500-800 DEG C of hot pressing temperature, hot pressing pressure 100-500MPa, 10-80 DEG C of heating rate/min；Hot pressing
In the process, the density of pressurize 1.5 ~ 2.5 minutes after magnet temperature reaches default hot pressing temperature, gained hot-pressed magnets is 7-
7.60g/cm3；
（6）Thermal deformation：It will（5）In hot-pressed magnets carry out thermal deformation, the thermal deformation technique is：Thermal deformation process is true
Altitude, vacuum degree are higher than 10-3Pa, 850-1050 DEG C of heat distortion temperature, thermal deformation pressure 700-1000MPa, thermal deformation rate
For 12-15mm/s, 10-80 DEG C of heating rate/min；In thermal deformation process, wait for that magnet pressure reaches default thermal deformation pressure
40 ~ 60s of pressurize afterwards；The density of gained heat distortion magnet is 7-7.68g/cm3。
It is mixed the invention has the advantages that a kind of utilization of present invention offer is directly total to association raw ore using Bayan Obo
It closes rare earth and prepares rare earth permanent-magnetic material and its method.The new rare-earth permanent magnetic material has cheap, reduces environmental pollution, magnetic
Energy product range can fill up ferrite, SmCo rare-earth permanent magnet scope of application blank well in 20 ~ 40MGOe.
Specific implementation mode：
One kind being total to rare-earth permanent magnet made of association raw ore mischmetal Bayan Obo, which is characterized in that the rare earth
The ingredient of permanent magnet is shown below：MMxFeyAzB, wherein 2≤x≤2.5,11≤y≤14,0≤z≤0.6, MM are white clouds Hubei Province
Rich association raw ore mischmetal altogether, Fe are ferro element, and A is the auxiliary alloy of nanometer, including one kind or several in Nd, Pr, Al, Cu element
Kind, B is boron element.
Preferably, the Bayan Obo is total to the natural constituent of association raw ore mischmetal and includes by weight percentage
Following rare earth composition：La:10%-30%、Ce:20%-60%、Pr:5%-10%、Nd:5%-15%、Sm:0-0.05%、Gd:0-0.04%、
Tb:0-0.01%、Dy:0-0.01%、Y:0-0.01%。
A kind of preparation method being total to rare-earth permanent magnet made of association raw ore mischmetal Bayan Obo, feature exist
In first to be directly total to association raw ore mischmetal MM preparations MM using Bayan OboxFeyB powder, then with the auxiliary alloying pellet of nanometer
It is prepared by mixing into MMxFeyAzB rare earth permanent-magnetic materials.
Preferably, the preparation method includes powder metallurgic method, hot pressing thermal deformation technique.
Wherein, powder metallurgic method has following steps：
（1）Feedstock processing：Raw material is surface-treated, ready raw material is mechanically removed into surface oxidation
Layer, wherein the raw material, which includes Bayan Obo, is total to association raw ore mischmetal MM；
（2）Dispensing：By step（1）Treated raw material mixed ingredients according to a certain percentage；It, first will be golden in process for preparation
The oxide and impurity of metal surface remove；
（3）It smelts：Dispensing is carried out in vaccum sensitive stove to be smelted into MMxFeyB ingot castings；Or by dispensing in vacuum induction speed
MM of the thickness between 0.1-1mm is made in solidifying stovexFeyB alloy sheets control it and form column crystal；
（4）Powder processed：, air-flow milling quick-fried using hydrogen, by MMxFeyB alloys are milled into the fine powder of 2.5 ~ 5 microns of sizes；
（5）Mixed powder：The auxiliary alloying pellet of nanometer is added to the MM preparedxFeyIn B powder, mixed in vacuum environment
Uniformly；
（6）Die mould：By step（5）The powder being mixed is pressed into certain shape, pressure 3T/cm in magnetic field2, magnetic field
H >15000 oersteds；
（7）Sintering：It is higher than 10 in vacuum degree-3It, will be by step in the vacuum environment of Pa（6）Obtained green compact is placed on hot place
It is sintered in reason stove, the sintering process is：It first is heated to keeping the temperature 1.5 ~ 2.5 hours at 560 ~ 630 DEG C by room temperature, then be risen
Temperature is warming up at 1050 ~ 1060 DEG C to keeping the temperature 2.5 ~ 3.5 hours at 860 ~ 930 DEG C and keeps the temperature 1.5 ~ 2.5 hours later, finally with
Stove takes out after being cooled to room temperature；
（8）Post isothermal treatment：It is higher than 10 in vacuum degree-3In the vacuum environment of Pa, by step（7）Obtained sintered body is by room
Temperature is increased to 870-890 DEG C, keeps the temperature 80-240 minutes, is cooled to room temperature later, then raises the temperature to 470-560 DEG C again,
After heat preservation 80-240 minutes, then it is cooled to room temperature；
（9）Magnetic-field heat treatment：It will be through step（8）It is 1.5-15T's that magnet after Post isothermal treatment, which is placed on magnetic field intensity,
Heat-treatment furnace is tempered in vacuum environment in 1000 ~ 1100 DEG C of temperature ranges.
Preferably, step（6）Middle magnetic field orientating is one of following method with forming method：Parallel punching block pressure, vertical steel
Molding, parallel punching block pressure and isostatic pressed, vertical steel molding and isostatic pressed.
Wherein, hot pressing thermal deformation technique has following steps：
（1）Dispensing：It is equipped with and is by weight percentage：MM：26-50%, Fe：49.5-72%, B：The master alloying of 0.5-2% is former
Material, wherein MM is that Bayan Obo is total to association raw ore mischmetal；
（2）Fast quenching：It will（1）In master alloying raw material melting fast quenching, by master alloying raw material be heated to after 1200 ~ 1250 DEG C with
The speed of quenching of 10-80m/s carries out fast quenching, and nozzle is round or elongated aperture, nozzle distance chill roll 2mm-10mm, gained fast quenching
Band vacuum heat -2 hours 1 minute at 300-1000 DEG C；
（3）Powder processed：It will（2）In master alloying rapid tempering belt ball milling obtain MM after 0.5-4 hoursxFeyB master alloying powder；It will be auxiliary
Alloy raw material Pr, Nd, PrNd, PrCu, NdCu and AlCu be quick-fried through hydrogen, after airflow milling, high-energy ball milling, and it is 10- to be milled into grain size
The auxiliary alloying pellet of nanometer that grain size is 10-500nm, auxiliary alloy is made through vaporization condensation process in the auxiliary alloying pellet of nanometer of 500nm
The mass percent of Cu is 1%-90% in raw material PrCu, NdCu and AlCu；
（4）Mixed powder：It will（3）Middle master alloying powder obtains mixed powder after being mixed with the auxiliary alloying pellet of nanometer, wherein nanometer
The mixed powder ratio of auxiliary alloying pellet is mass percent 0-8%；
（5）Hot pressing：It will（4）In mixed powder carry out hot pressing, the heat pressing process is：Hot pressing is vacuum environment,
Vacuum degree is higher than 10-3Pa, 500-800 DEG C of hot pressing temperature, hot pressing pressure 100-500MPa, 10-80 DEG C of heating rate/min；Hot pressing
In the process, the density of pressurize 1.5 ~ 2.5 minutes after magnet temperature reaches default hot pressing temperature, gained hot-pressed magnets is 7-
7.60g/cm3；
（6）Thermal deformation：It will（5）In hot-pressed magnets carry out thermal deformation, the thermal deformation technique is：Thermal deformation process is true
Altitude, vacuum degree are higher than 10-3Pa, 850-1050 DEG C of heat distortion temperature, thermal deformation pressure 700-1000MPa, thermal deformation rate
For 12-15mm/s, 10-80 DEG C of heating rate/min；In thermal deformation process, wait for that magnet pressure reaches default thermal deformation pressure
40 ~ 60s of pressurize afterwards；The density of gained heat distortion magnet is 7-7.68g/cm3。
Rare earth permanent-magnetic material provided by the present invention and preparation method thereof has the following advantages：
（1）Directly being total to association raw ore mischmetal using Bayan Obo prepares sintered rare-earth permanent magnetic material, can significantly subtract
Few Rare Earth Separation step and reduction separation requirement, environmental protection while advantageously reducing material production cost；
（2）Since Bayan Obo is total to the total concomitant characteristics of association raw ore mischmetal, it is mixed to be total to association raw ore with Bayan Obo
The mischmetal that the magnet performance prepared by rare earth is higher than independent addition pure rare earth element or manually prepares in proportion is closed to be given birth to
The magnet of production；
（3）Bayan Obo is total to association raw ore mischmetal other than containing a large amount of La, Ce, Pr, Nd, also Dy, Tb
The equal other elements such as heavy rare earth elements and Al, these elements are all beneficial to improve magnetism of material energy, are common artificial mixing
Advantage not available for rare earth；
（4）Permanent-magnet material directly is prepared using mischmetal, hardly results in the higher product of performance, previous preparation method is
Replace part praseodymium neodymium alloy to reach the product for preparing and can use using mischmetal, and adds the auxiliary alloy of nanometer in the present invention
Particle can effectively improve the Grain-Boundary Phase of material, while significantly reducing praseodymium neodymium usage amount, moreover it is possible to significantly improve the property of material
Energy；
（5）The new rare-earth permanent magnetic material is conducive to improve the utilization rate of the high abundances rare earths such as La, Ce, reduces Pr, Nd valence
The dynamic influence greatly to the price of rare earth permanent-magnetic material of lattice wave, is conducive to the popularization and application of rare earth permanent-magnetic material；
（6）The new rare-earth permanent magnetic material magnetic energy product coverage is wide, can effectively make up ferrite and SmCo permanent magnetism
Using deficiency；
（7）There is a large amount of La, Ce element since Bayan Obo is total in association raw ore mischmetal, can effectively reduce burning
Junction temperature and time, into the production cost of a reduction material.
Embodiment 1：
It is a kind of to be total to the sintered rare-earth permanent magnetic material that association raw ore mischmetal is directly prepared using Bayan Obo.
Dispensing is as follows by table 2：
Table 2
| Ingredient | Bayan Obo is total to association raw ore mischmetal | Fe | B |
| Weight percent | 35 | 64 | 1 |
Using powder metallurgical technique, by containing the raw material centainly matched such as：Bayan Obo be total to association raw ore mischmetal,
Then ferro-boron etc. is smelted by induction melting furnace is crushed the powder for being made 3~5 μm at alloy steel ingot, and add NdCu thereto
The auxiliary alloying pellet of nanometer, the additive amount of wherein NdCu nanometer auxiliary alloying pellet by the weight of alloy steel ingot for 100% in terms of its weight hundred
Divide than as shown in table 3, and the compression moulding in magnetic field, the densified sintering product after molding in vacuum freezing of a furnace are simultaneously tempered.Gained rare earth
The results are shown in Table 3 for the magnetism testing of permanent-magnet material.
Table 3
| The additive amount of PrCu | Br(kGs) | Hcj(kOe) | BHmax(MGOe) |
| 0 | 10.33 | 4.69 | 10.92 |
| 4% | 11.23 | 7.02 | 18.37 |
| 8% | 11.65 | 10.87 | 23.75 |
From the table 3 of embodiment 1 as can be seen that Bayan Obo is total to association raw ore mischmetal and easily aoxidizes, to be difficult
To the product that can be applied, then after adding a small amount of auxiliary alloying pellet of PdCu nanometers, the performance of material significantly improves.In material
While capable of being applied, lanthanum, cerium utilization rate also dramatically increase.
Embodiment 2
Table 4
| Method | Br(kGs) | Hcj(kOe) | BHmax(MGOe) |
| Raw ore mischmetal | 11.23 | 7.02 | 18.37 |
| Common mischmetal | 10.65 | 5.87 | 15.38 |
From the table 4 of embodiment 2 as can be seen that in the case of formula is identical with process conditions, common mischmetal is used
Performance will be well below the performance for using Bayan Obo to be total to association raw ore mischmetal.
Embodiment 3
Table 5
| Method | Ce contents | La contents | Br(kGs) | Hcj(kOe) | BHmax(MGOe) |
| Individually addition La | 0.9% | 11.1 | 8.91 | 25 | |
| Individually addition Ce | 35% | 11.36 | 6.47 | 25.94 | |
| Bayan Obo is total to association raw ore mischmetal magnet | 18.75% | 9.06% | 11.33 | 8.69 | 25.92 |
From the table 5 of embodiment 3 as can be seen that similar in magnet performance, Bayan Obo is total to the mixing of association raw ore
The utilization rate of lanthanum is independent add lanthanum 10 times in rare earth, can effective solution high abundance rare earth problem of complex utilization.And it uses
The performance of common mischmetal will be well below the performance for using Bayan Obo to be total to association raw ore mischmetal.
Embodiment 4
It is a kind of to be total to the hot-pressing thermal deformable rare earth permanent-magnet material that association raw ore mischmetal is directly prepared, institute using Bayan Obo
The preparation method for stating rare earth permanent-magnetic material is as follows：
（1）Dispensing：It is equipped with and is by weight percentage：MM：31%, Fe：68%, B：1% master alloying raw material, wherein MM is
Bayan Obo is total to association raw ore mischmetal；
（2）Fast quenching：It will（1）In master alloying raw material melting fast quenching, master alloying raw material is heated to after 1250 DEG C with 30m/s
Quench speed carry out fast quenching, nozzle is circular aperture, nozzle distance chill roll 8mm, gained rapid tempering belt vacuum heat at 500 DEG C
5 minutes；
（3）Powder processed：It will（2）In master alloying rapid tempering belt ball milling obtain MM after 1.5 hoursxFeyB master alloying powder；By auxiliary conjunction
The auxiliary alloying pellet of nanometer that grain size is 100nm is made through vaporization condensation process by golden raw material A lCu, the matter of Cu in auxiliary alloy raw material AlCu
It is 50% to measure percentage；
（4）Mixed powder：It will（3）Middle master alloying powder obtains mixed powder after being mixed with the auxiliary alloying pellet of nanometer, wherein nanometer
The mixed powder ratio of auxiliary alloying pellet is mass percent 5%；
（5）Hot pressing：It will（4）In mixed powder carry out hot pressing, the heat pressing process is：Hot pressing is vacuum environment,
Vacuum degree is higher than 10-3Pa, 600 DEG C, hot pressing pressure 500MPa of hot pressing temperature, 60 DEG C/min of heating rate；In hot pressing, magnetic is waited for
Temperature reaches pressurize 2 minutes after default hot pressing temperature, and the density of gained hot-pressed magnets is 7.58g/cm3；
（6）Thermal deformation：It will（5）In hot-pressed magnets carry out thermal deformation, the thermal deformation technique is：Thermal deformation process is true
Altitude, vacuum degree are higher than 10-3Pa, 900 DEG C of heat distortion temperature, thermal deformation pressure 800MPa, thermal deformation rate are 13mm/s, are risen
60 DEG C/min of warm rate；In thermal deformation process, the pressurize 60s after magnet pressure reaches default thermal deformation pressure；Gained heat
The density for deforming magnet is 7.65g/cm3。
The magnetism testing result of gained hot pressing heat distortion magnet is as shown in table 6 below.
Table 6
| The additive amount of AlCu | Br(kGs) | Hcj(kOe) | BHmax(MGOe) |
| 5% | 10.42 | 12.89 | 26.37 |
Claims (1)
1. a kind of being total to the method that association raw ore mischmetal prepares rare-earth permanent magnet by Bayan Obo, which is characterized in that described dilute
The ingredient of native permanent magnet is shown below：MMxFeyAzB, wherein 2≤x≤2.5,11≤y≤14,0≤z≤0.6, MM are white clouds
Pile of stones, earth or grass is total to association raw ore mischmetal, and Fe is ferro element, and A is the auxiliary alloy of nanometer, including Nd, Pr, Al, Cu element, and B is boron member
Element；It includes following rare earth composition that the Bayan Obo, which is total to the natural constituent of association raw ore mischmetal by weight percentage,：
La:10%-30%, Ce:20%-60%, Pr:5%-10%, Nd:5%-15%, Sm:0-0.05%, Gd:0-0.04%, Tb:
0-0.01%, Dy:0-0.01%, Y:0-0.01%；It is to pass through dialogue that the Bayan Obo, which is total to association raw ore norium,
Cloud oborite using X-fluorescence sort, carry out analysis purification as needed, directly smelt and obtain, wherein not only containing praseodymium, neodymium, lanthanum,
Cerium, while also containing dysprosium, terbium heavy rare earth element；
The preparation method comprises the following steps：
(1) dispensing：It is equipped with and is by weight percentage：MM：26-50%, Fe：49.5-72%, B：The master alloying of 0.5-2% is former
Material, wherein MM is that Bayan Obo is total to association raw ore mischmetal；
(2) fast quenching：By the master alloying raw material melting fast quenching in (1), master alloying raw material is heated to after 1200~1250 DEG C with 10-
The speed of quenching of 80m/s carries out fast quenching, and nozzle is round or elongated aperture, nozzle distance chill roll 2mm-10mm, gained rapid tempering belt
Vacuum heat -2 hours 1 minute at 300-1000 DEG C；
(3) powder processed：Master alloying rapid tempering belt ball milling in (2) is obtained into MM after 0.5-4 hoursxFeyB master alloying powder；By auxiliary alloy
Raw material Pr, Nd, PrNd, PrCu, NdCu and AlCu be quick-fried through hydrogen, after airflow milling, high-energy ball milling, and it is 10-500nm's to be milled into grain size
The auxiliary alloying pellet of nanometer that grain size is 10-500nm, auxiliary alloy raw material is made through vaporization condensation process in the auxiliary alloying pellet of nanometer
The mass percent of Cu is 1%-90% in PrCu, NdCu and AlCu；The grain size of the auxiliary alloying pellet of nanometer is 10nm-
500nm；
(4) powder is mixed：Mixed powder is obtained after master alloying powder in (3) is mixed with the auxiliary alloying pellet of nanometer, wherein the auxiliary conjunction of nanometer
The mixed powder ratio of gold particle is mass percent 0-8%；
(5) hot pressing：Mixed powder in (4) is subjected to hot pressing, the heat pressing process is：Hot pressing is vacuum environment, vacuum
Degree is higher than 10-3Pa, 500-800 DEG C of hot pressing temperature, hot pressing pressure 100-500MPa, 10-80 DEG C of heating rate/min；Hot pressing
In, the density of the pressurize 1.5~2.5 minutes after magnet temperature reaches default hot pressing temperature, gained hot-pressed magnets is 7-7.60g/
cm3；
(6) thermal deformation：Hot-pressed magnets in (5) are subjected to thermal deformation, the thermal deformation technique is：Thermal deformation process is vacuum ring
Border, vacuum degree are higher than 10-3Pa, 900-1050 DEG C of heat distortion temperature, thermal deformation pressure 700-1000MPa, thermal deformation rate are 12-
15mm/s, 10-80 DEG C of heating rate/min；In thermal deformation process, protected after magnet pressure reaches default thermal deformation pressure
Press 40~60s；The density of gained heat distortion magnet is 7-7.68g/cm3。
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| CN105321646A (en) * | 2015-11-25 | 2016-02-10 | 中国科学院宁波材料技术与工程研究所 | Nanocrystalline thermal deformation rare-earth permanent magnet with high coercivity and preparation method of nanocrystalline thermal deformation rare-earth permanent magnet |
| CN107578869B (en) * | 2016-07-05 | 2020-03-17 | 中国科学院物理研究所 | Mixed rare earth-iron-based permanent magnet material and preparation method and application thereof |
| CN106210997A (en) * | 2016-08-26 | 2016-12-07 | 广东欧珀移动通信有限公司 | A kind of speaker and terminal |
| CN106548843A (en) * | 2016-10-17 | 2017-03-29 | 中国科学院宁波材料技术与工程研究所 | Rare earth permanent-magnetic material and preparation method thereof |
| CN106782971A (en) * | 2016-12-05 | 2017-05-31 | 湖南航天磁电有限责任公司 | A kind of NdFeB material and preparation method thereof |
| CN108666127A (en) * | 2018-06-04 | 2018-10-16 | 安徽天宇磁业股份有限公司 | Based on energy-saving and environment-friendly permanent magnet processing technology |
| CN109550945B (en) * | 2018-12-28 | 2021-05-28 | 内蒙古科技大学 | Permanent magnet material prepared from bayan obo associated raw ore mixed rare earth and preparation method thereof |
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| CN101958171A (en) * | 2010-04-14 | 2011-01-26 | 无锡南理工科技发展有限公司 | Method for preparing corrosion-resistant sintered neodymium iron boron (NdFeB) magnet |
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| CN103123838B (en) * | 2013-01-30 | 2015-06-03 | 浙江大学 | Rare earth permanent magnet produced by applying abundant rare earth MM and preparation method thereof |
| CN103151161B (en) * | 2013-03-22 | 2015-08-12 | 四川大学 | The directed broken method preparing anisotropy NdFeB magnetic powder of heat distortion magnet |
| CN103834863B (en) * | 2014-03-31 | 2015-11-11 | 内蒙古科技大学 | The method of Nd-Fe-Bo permanent magnet material is manufactured with common association mishmetal |
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| CN101958171A (en) * | 2010-04-14 | 2011-01-26 | 无锡南理工科技发展有限公司 | Method for preparing corrosion-resistant sintered neodymium iron boron (NdFeB) magnet |
| CN103426624A (en) * | 2013-08-14 | 2013-12-04 | 林建强 | Production method for neodymium-iron-boron permanent magnet |
| CN103928204A (en) * | 2014-04-10 | 2014-07-16 | 重庆科技学院 | Low-rare earth content anisotropy nanocrystalline NdFeB compact magnet and preparation method thereof |
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