CN103779061B - High corrosion resistance Re-(Fe, TM)-B magnet and preparation method thereof - Google Patents
High corrosion resistance Re-(Fe, TM)-B magnet and preparation method thereof Download PDFInfo
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- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0273—Imparting anisotropy
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- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
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Abstract
The open high corrosion resistance Re-(Fe of the present invention, TM)-B magnet preparation method: 1) by Re-(Fe, TM) after-B system magnet material melting, carry out coarse crushing, broken in carrying out, obtain the dusty material of average grain diameter 0.5mm, wherein Re is selected from Pr-Nd, Nd, Dy, Tb, Gd, Ho or its mixing, and TM is selected from Al, Nb, Cu, Ga, Co, Zr or its mixing; 2) step 1 gained dusty material is ground to the little 5 μ m of dusty material average grain diameter through airflow milling one step; 3) by step 2 gained dusty material after pressing under magnetic field, vacuum-sintering, Ageing Treatment, obtain required product; Wherein step 1 and step 2 gained dusty material carries out mixing treatment dusty material mixed before being for further processing; Wherein underway broken, airflow milling grind and mixing treatment in dusty material, add metal or the metal oxide that particle mean size is less than 80 μ m when one or more operation.
Description
Technical field
The invention belongs to rare earth permanent-magnetic material field. Relate generally to the preparation of Re-(Fe, TM)-B sintered magnetMethod.
Background technology
Along with the continuous expansion of rare earth permanent-magnetic material application, client to the requirement of rare earth permanent magnet product alsoIn continuous raising. Such as wind-driven generator, electric motor of automobile, elevator motor, compressor electric motor, nuclear-magnetismResonance, voice coil motor, instrument and meter, sensor application, all to Re-(Fe, TM)-B magnetCorrosion resistance has proposed very high requirement.
Usually, conventionally use without coating magnet long-time continuous under high temperature, high pressure, high humidity environment conditionPlace, the loss in weight producing in per surface area reflects the corrosion resistance of magnet quantitatively.
At present, improve the corrosion resistance of Re-(Fe, TM)-B magnet, mainly contain two kinds of methods, one is logicalCross surface treatment (as plating, electrophoresis, coating) technology and improve the corrosion resistance of magnet appearance, but existingThere is process for treating surface often to have the shortcoming that cost is high, contaminated environment large, affect magnet magnetic property. AnotherPlant is to improve Re-(Fe, TM)-intrinsic corrosion resistance of B magnet own. For example, Chinese invention patent application "Plant highly corrosion resistant Re-(Fe, TM)-B series magnet and preparation method thereof " (CN200910116871.9) provideA kind of before sintering, be the method for magnet processing protective layer, specific practice is before sintering, by cylinderBe placed in alloy molten solution and carry out high temperature sintering, make alloy atom form Hou Du Wei≤2 μ at peripheryThe overcoat of m, and have part of atoms to penetrate into magnet inside, this method no doubt can improve magnetCorrosion resistance, but because the method has the process of twice sintering, than the more than once sintering of conventional methodProcess, will improve the cost of sintering workshop section; And can only usually improve corrosion resistance by elemental metals unit,Improve the price of cost of raw material elemental metals higher than the price of metal oxide. Due to sintering Re-Fe-BThe corrosion behavior of magnet shows as Grain-Boundary Phase and preferentially corrodes, therefore, and can be by improving the anticorrosive of Grain-Boundary PhaseProperty improves the corrosion resistance of magnet. In the prior art, normally in smelt stage, add one or manyPlant microalloying element, in magnet structure, form one or more and there is better anti-corruptionLose the crystal-boundary phase alloy of performance, can improve the corrosion resistance of Grain-Boundary Phase, thereby magnet is anticorrosiveProperty is improved. But the shortcoming of this process is part microalloying element directly enters principal phaseNd2Fe14B crystal grain inside, has reduced the magnetic property of magnet, has also reduced microalloying element and has changed simultaneouslyThe effect of kind magnet corrosion resistance.
Summary of the invention
The present invention is intended to solve the existing problem of prior art, provides a kind of preparation cost cheap and anti-corruptionRe-(Fe, TM)-B magnet of erosion performance and preparation method thereof.
Preparation method provided by the present invention comprises following processing step:
1) by carrying out coarse crushing after the melting of Re-(Fe, TM)-B system magnet material, then further enterBroken in row, obtain the dusty material of average grain diameter 0.5mm, wherein Re be selected from Pr-Nd,Nd, Dy, Tb, Gd, Ho or its mix, TM be selected from Al, Nb, Cu, Ga, Co,Zr or its mixing;
2) step 1 gained dusty material is further ground to dusty material average grain diameter through airflow milling little5μm；
3) by step 2 gained dusty material after pressing under magnetic field, vacuum-sintering, Ageing Treatment, obtainRequired product;
Wherein, the pulverizing of step 1 and step 2 or grinding gained dusty material, be for further processingBefore, carry out mixing treatment, dusty material is mixed;
Wherein, underway broken, airflow milling grind and mixing treatment operation in when one or more operation,Be less than 80 μ m(and be about 200 orders to adding particle mean size in dusty material) metal (as Cu powder, CoPowder, Nb powder, Al powder, liquid Ga, or its mixture) or metal oxide (Dy2O3、Tb4O7，Or its mixture), after interpolation, stir. Wherein, preferably add elemental metals.
While wherein adding metal or metal oxide, it need fill nitrogen before being added in closed containerDeoxygenation, deoxygenation process generally will be carried out 5-20 minute, the concrete time according to addition number determine,Additive is fewer, and the deoxygenation time is shorter; After deoxygenation finishes, will be added thing is added into and in powder, carries out evenlyBatch mixing, the wherein content of the weight based on powder and former composition middle rare earth, addition < 2%(powder of additivePowder material gross mass), and make mass ratio Re:(Fe, TM): the ratio of B=2:14:1 is added,Re represents rare earth, and TM represents the non-rare earth metals such as Al, Nb, Cu, Ga, Co, Zr, and B represents boron.
The present invention also provides prepared Re-(Fe, the TM)-B magnet of method thus.
The inventor surprisingly finds, thus the corrosion resistance of prepared Re-(Fe, the TM)-B magnet of methodEnhancing, be mainly due to add powder magnetic powder particle surface uniform distribute, in the time of vacuum-sintering,Microalloying element only and magnetic powder particle or main phase grain Nd2Fe14B spreads on top layer, forms a kind ofOr the multiple crystal-boundary phase alloy with good corrosion, thereby improve the corrosion resistance of magnet, simultaneouslyAvoid again microalloying element to enter the inner infringement of magnetic crystal grain magnet magnetic property.
The object of the invention is in lower-cost situation, in when broken, airflow milling or batch mixing, pass throughAdd micro-metal simple-substance element or metal oxide, make its major part enter rich Nd mutually in, form newGrain-Boundary Phase, thereby farthest bring into play trace meter simple substance element or metal oxide to magnet intrinsicThe improvement effect of corrosion resistance, reaches client's actual operation requirements, simultaneously by it to magnet magnetic propertyInfringement drops to minimum.
Detailed description of the invention
Embodiment 1:
Be (NdPr) at design mix31.5Fe64.73Al0.5Nb0.5Co1.0Zr0.25B1.02(mass percent)In formula, in order to improve coercivity, have two kinds of methods, one is with conventional method preparation, in meltingIn journey, add 0.5%Cu, be called magnet 1; Another kind is with method provided by the present invention preparation, inBefore broken rear airflow milling, 200 objects, 0.5%Cu powder are added, be called magnet 2. Two kinds of alloys warp respectivelyMelting, thick broken, in carry out after broken, airflow milling, batch mixing, pressing under magnetic field, vacuum-sintering, Ageing TreatmentMagnetic property is measured (test method: blank is measured with magnetization characteristic automatic measuring instrument standard: ChinaPeople's republic's national standard (GB/T13650-2000)-sintered Nd-Fe-B permanent magnetic material) and weightless testTest. Test result is in table 1:
Table 1: the magnetic property of magnet and weightless test
Weightless test condition: place continuously 240 little under 120 DEG C, 100% humidity, 2 atmospheric environmentTime; Sample size: φ 10*10 cylinder.
From table, result can be found out: no matter magnetic property or corrosion resistance is all superior than magnet 1 of magnet 2.
Embodiment 2:
Be (NdPr) at design mix30.5Dy0.5Fe65.78Al0.45Cu0.1Co1.0Zr0.25B1.02(mass percent)In formula, in order to improve coercivity, there are two kinds of methods, a kind of with conventional method preparation, be in meltingIn journey, add 0.4%Ga, be called magnet 3; Another kind is with method preparation provided by the present invention, at gasAfter stream mill, before batch mixing, 0.4% Liquid metal Ga is added, be called magnet 4. Two kinds of alloys respectively through melting,Thick broken, in carry out magnetic property after broken, airflow milling, batch mixing, pressing under magnetic field, vacuum-sintering, Ageing TreatmentMeasure and weightless test test. Test result sees the following form 2:
Table 2: the magnetic property of magnet and weightless test
Weightless test condition: place continuously 240 little under 120 DEG C, 100% humidity, 2 atmospheric environmentTime; Sample size: φ 10*10 cylinder.
From table 2, result can be found out: no matter magnetic property or corrosion resistance of magnet 4, and all than magnet 3Superior.
Embodiment 3:Relating to composition for (NdPr)25Tb1Fe66.19Al0.30Cu0.25Co1.0Zr0.25B1.01(mass percent)In formula, in order to improve coercivity, have two kinds of methods, one is in fusion process, to add elemental metalsElement 5%Dy, becomes magnet 5; Another kind adds elemental metals element 3.2% in fusion processDy, the Dy of interpolation metal oxide 1.8% before airflow milling batch mixing2O3, become magnet 6. Two kinds of alloys divideNot through melting, thick broken, in after broken, airflow milling, batch mixing, pressing under magnetic field, vacuum-sintering, Ageing TreatmentCarry out magnetic property measurement and volume zero-G test test. Test result sees the following form 3:
Table 3: the magnetic property of magnet and weightless test
Weightless test condition: place continuously 480 little under 120 DEG C, 100% humidity, 2 atmospheric environmentTime; Sample size:Cylinder.
From table 3, result can be found out: no matter magnetic property or corrosion resistance of magnet 6, and all than magnet 5Superior.
In when broken, airflow milling, batch mixing, by adding trace meter simple substance element, metal oxide etc.,Not only can increase the magnetic property of magnet, the corrosion resistance of enhancing magnet, and on production cost, alsoReduce to some extent compared with surface treatment, and environmentally friendly.
Disclosed is above only several specific embodiment of the present invention, and still, the present invention is not limited thereto,The changes that any person skilled in the art can think of all should fall into protection scope of the present invention.
Claims (6)
1. a high corrosion resistance Re-(Fe, TM)-B magnet preparation method comprises following processing step:
1) by carrying out coarse crushing after the melting of Re-(Fe, TM)-B system magnet material, then further enterBroken in row, obtain the dusty material of average grain diameter 0.5mm, wherein Re be selected from Pr-Nd,The mixture of any two or more compositions in Dy, Tb or Pr-Nd, Dy, Tb, TMBe selected from Al, Nb, Cu, Ga, Co, Zr or Al, Nb, Cu, Ga, Co, ZrIn the mixture of any two or more compositions;
2) step 1 gained dusty material is further ground to dusty material average grain diameter through airflow milling little5μm；
3) by step 2 gained dusty material after pressing under magnetic field, vacuum-sintering, Ageing Treatment, obtainRequired product;
Wherein, step 1 and step 2 gained dusty material, before being for further processing, carry out batch mixingProcess, dusty material is mixed;
Wherein, underway broken, airflow milling grind and mixing treatment in when one or more operation, toIn dusty material, add metal or metal oxide that particle mean size is less than 80 μ m; The metal that wherein addedBe selected from the mixed of any two or more compositions in Co, Nb, Al powder, Ga or Co, Nb, Al powder, GaCompound, wherein said metal oxide is selected from Dy2O3、Tb4O7Or its mixture, after interpolation, stir;While wherein adding metal or metal oxide, in the mass percent of dusty material, addition < 2%.
2. the method for claim 1, what wherein added is metal simple-substance.
3. the method for claim 1, the metal that wherein added or metal oxide are being added itBefore in closed container, carry out the processing of filling with inert gas deoxygenation.
4. method as claimed in claim 3, wherein said deoxygenation process will be carried out more than 5 minutes.
5. method according to claim 1, the addition that wherein adds metal or metal oxide makesObtaining mass ratio in end product is Re:(Fe, TM): B=2:14:1, wherein Re represents rare earth element,TM represents the Al of institute, Nb, Cu, Ga, Co, the non-rare earth metal of Zr, and B represents boron.
6. Re-(Fe, TM)-B magnet, it is made by arbitrary described method in claim 1-5.
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| CN201210393641.9A CN103779061B (en) | 2012-10-17 | 2012-10-17 | High corrosion resistance Re-(Fe, TM)-B magnet and preparation method thereof |
| PCT/CN2013/074081 WO2014059772A1 (en) | 2012-10-17 | 2013-04-11 | High corrosion-resistant re-(fe, tm)-b magnet and preparing method thereof |
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| CN201210393641.9A CN103779061B (en) | 2012-10-17 | 2012-10-17 | High corrosion resistance Re-(Fe, TM)-B magnet and preparation method thereof |
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| CN104064301B (en) * | 2014-07-10 | 2017-02-15 | 北京京磁电工科技有限公司 | NdFeB magnet and preparation method thereof |
| CN104493168A (en) * | 2014-12-27 | 2015-04-08 | 株洲茂翔硬质合金有限公司 | Preparation method for metal ceramic products |
| CN108269665A (en) * | 2017-12-27 | 2018-07-10 | 宁波招宝磁业有限公司 | A kind of neodymium iron boron magnetic body and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101055779A (en) * | 2007-03-08 | 2007-10-17 | 上海交通大学 | Method for grain boundary adulterated by oxide or nitride to improve the NdFeB permanent magnetic material performance |
| CN102543342A (en) * | 2011-12-31 | 2012-07-04 | 北京工业大学 | Sintered neodymium-iron-boron-based permanent magnet material with high coercive force and high corrosion resistance, prepared by doping copper nano-particles, and preparation method thereof |
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| JPS6393105A (en) * | 1986-10-08 | 1988-04-23 | Fuji Elelctrochem Co Ltd | Manufacture of isotropic bonded magnet |
| JP2001006911A (en) * | 1999-06-21 | 2001-01-12 | Shin Etsu Chem Co Ltd | Manufacture of rare earth permanent magnet |
| CN100394518C (en) * | 2006-08-04 | 2008-06-11 | 北京工业大学 | Method for preparing high coercive force sintering rare-earth-iron-p permanent magnetic material |
| CN101315825B (en) * | 2007-05-31 | 2012-07-18 | 北京中科三环高技术股份有限公司 | Fire resistant permanent magnet alloy and manufacturing method thereof |
| CN101562067A (en) * | 2008-04-18 | 2009-10-21 | 沈阳中北通磁科技有限公司 | Manufacture method of corrosion-resistant R-Fe-B rare-earth permanent magnet |
| CN102543343B (en) * | 2011-12-31 | 2015-10-14 | 北京工业大学 | The high-coercive force of aluminum nanoparticles doping preparation and high-corrosion resistance Sintered Nd-Fe-B based permanent magnetic material and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101055779A (en) * | 2007-03-08 | 2007-10-17 | 上海交通大学 | Method for grain boundary adulterated by oxide or nitride to improve the NdFeB permanent magnetic material performance |
| CN102543342A (en) * | 2011-12-31 | 2012-07-04 | 北京工业大学 | Sintered neodymium-iron-boron-based permanent magnet material with high coercive force and high corrosion resistance, prepared by doping copper nano-particles, and preparation method thereof |
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