CN103680788A - Bonding rare-earth permanent-magnet alloy - Google Patents
Bonding rare-earth permanent-magnet alloy Download PDFInfo
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Abstract
The invention provides novel Nd-Fe-B system bonding rare-earth permanent-magnet alloy. The novel Nd-Fe-B system bonding rare-earth permanent-magnet alloy is characterized by comprising, by atomic percentage composition, 15.0-18.0 of Nd, 5.0-6.0 of B, 0.2-0.3 of Al, 7.0-10.0 of Co, 0.5-0.8 of Nb, 0.1-0.3 of Zr, 0.2-0.4 of Cu, 3.0-5.0 of Dy, the balance Fe and inevitable impurities. The novel Nd-Fe-B system bonding rare-earth permanent-magnet alloy has the advantage that a bonding alloy system is manufactured by an advanced injection forming method and is excellent in magnetic performance and corrosion resistance.
Description
Technical field
The present invention relates to the technical field of rare earth permanent-magnetic material, it is bonding rare earth permanent magnet material that a kind of Nd-Fe-B is particularly provided.
Background technology
Permanent magnetic material, as a kind of functional material being most widely used in modern industry and science and technology, mainly comprises Al-Ni-Co permanent magnet material, ferrite permanent-magnet materials, rare earth permanent-magnetic material and other permanent magnetic material etc.Wherein rare-earth permanent magnetic material is that the alloy that rare earth metal and transition metal form is made through certain technique, is the best class permanent magnetic material of current combination property.
And according to preparation method, Nd-Fe-Bo permanent magnet material can be divided into again sintered NdFeB and the large class of Agglutinate neodymium-iron-boron two.Wherein, although the magnetic property of sintered bond Nd-Fe-Bo permanent magnet material is very high, but coercive force etc. are on the low side, corrosion resistance is poor, particularly processing characteristics wretched insufficiency, also can produce in sintering process significantly and shrink, and causes its dimensional accuracy to guarantee, conventionally need the aftertreatment technologys such as grinding, it is very restricted in application.Binding Nd-Fe-B permanent magnetic material is by NdFeB magnetic powder and resin, the binding agents such as the macromolecular compounds such as plastics or low-melting-point metal evenly mix, then by compression, extrude or compound permanent magnetic material that the manufacturing process such as injection is made, compare with sintered Nd-Fe-B permanent magnetic material, although binding Nd-Fe-B permanent magnetic material magnetic property declines to some extent, but its stability is better, its magnet shape degree of freedom is good simultaneously, can make thin-walled, small-sized, the product that abnormity and dimensional accuracy are high, in addition its density is little, cost is low, the feature that material recovery recycling is good, development in recent years is very fast, be widely used in stereo set, computer, the every field such as mobile communications tool.
Yet the preparation of Agglutinate neodymium-iron-boron material also exists a lot of problems, first be exactly the contradiction existing between magnetic property and forming property, in order to improve as far as possible the magnetic property of material, wish to improve the NdFeB magnetic powder addition in composite permanent-magnetic material as far as possible, but too high useful load will inevitably reduce the mobility of magnetic and binder mixtures, and then worsen the performances such as follow-up mixing, shaping.Although adopted at present such as carry out the improvement methods such as couplant surface treatment for magnetic powder, the effect reaching is still unsatisfactory.In addition because Magnaglo surface activity is very high, there are a large amount of micro-cracks in broken, the quick-fried powder surface that causes of hydrogen in addition, makes powder very easily oxidized, thereby improved the viscosity of mixture and affect formability etc.
How can obtain a kind of forming property of existing excellence, have again the novel bonding Nd-Fe-Bo permanent magnet material of excellent magnetic energy simultaneously concurrently, be the main directions that people constantly pursue and study always.
Summary of the invention
Object of the present invention is to provide a kind of formability of novel existing excellence, and the Nd-Fe-B that has again excellent magnetic property is bonding rare earth permanent magnet material.
The Nd-Fe-B using in the present invention is that bonded rare earth permanent magnetic alloy powder has following composition: in atomic percentage conc, Nd15.0-18.0, B5.0-6.0, Al0.2-0.3, Co7.0-10.0, Nb0.5-0.8, Zr0.1-0.3, Cu0.2-0.4, Dy3.0-5.0, surplus is Fe and inevitable impurity.
Nd-Fe-B in the present invention is that the concrete preparation method of bonded rare earth permanent magnetic alloy is as follows:
1) melting, the alloy raw material being equipped with is put into vacuum induction melting furnace, smelting furnace is evacuated to 15-20Pa and the melting of heating until temperature starts to be filled with argon gas to pressure while being warming up to 1150 ℃ is 0.3-0.4MPa, be warming up to subsequently 1350-1400 ℃ of refining 5-10 minute, be incubated standing 1-1.5 minute;
2) cast, adopts the method for getting rid of Strip casting, and chill roll diameter is 500mm, controls cooling rate at 2.7m/s-3m/s, obtains the slab that thickness is 0.2-0.4mm;
3) Mechanical Crushing, obtains by Mechanical Crushing the meal that particle diameter is 100-200 μ m by slab;
4) hydrogen is quick-fried, the meal under the condition that is 1-2L/min at hydrogen flowing quantity, Mechanical Crushing being obtained is heated to 800-820 ℃, after insulation 5-10min, increase hydrogen flowing quantity to 3-4L/min and keep, inhale hydrogen 2-3h, arrange subsequently hydrogen and be filled with argon gas, when argon pressure reaches 0.8-1MPa, start to vacuumize dehydrogenation, during to vacuum degree 2-4Pa, dehydrogenation finishes;
5) grind, adopt airflow milling to grind, specifically add the zinc stearate of 0.10-0.13wt%, in nitrogen atmosphere, being crushed to average grain diameter is 30-50 μ m, obtains fine powder.
6) preliminary treatment, by fine powder with take after the polyamide-imide resin solution mixing and stirring that dimethylacetylamide is solvent, be heated to 150-180 ℃, solvent is volatilized and obtains cured film on magnetic surface.
7) mixing, by the magnetic after overlay film and polyamide binding agent and add auxiliary agent and mix, in twin shaft mixing roll, carry out mixingly, melting temperature is 200-220 ℃, mixing time 30-40min.
8) injection moulding, is preheating to 100-120 ℃ by mold temperature, injection temperature 240-260 ℃, and in the magnetic field intensity of 1800-2000kA/m,, the injection pressure hemostasis of 20-25MPa is shaped and pressurize, obtaining Nd-Fe-B of the present invention is bonded rare earth permanent magnetic alloy.
The invention has the advantages that: (1) appropriate design the composition of alloy, by rational proportion light, heavy rare earth, and the appropriateness of other alloying elements adds, and obtained the RE permanent magnetic alloy of optimal performance; (2) adopted suitable melting, disintegrating process to obtain bonding Magnaglo; (3) adopted suitable preliminary treatment, thermoplastic resin binder and interpolation auxiliary agent, and corresponding calendering process, obtained high charging ratio and there is the melt flow stream of excellent forming property; (4) adopted advanced injection molding process, the Nd-Fe-B that has prepared excellent performance is bonded rare earth permanent magnetic alloy.
Embodiment
Embodiment 1-4, and comparative example 1-3:
1) melting, the alloy raw material being equipped with by composition in table 1 is put into vacuum induction melting furnace, smelting furnace is evacuated to 18Pa and the melting of heating until temperature starts to be filled with argon gas to pressure while being warming up to 1150 ℃ is 0.4MPa, be warming up to subsequently 1380 ℃ of refinings 8 minutes, be incubated standing 1.5 minutes;
2) cast, adopts the method for getting rid of Strip casting, and chill roll diameter is 500mm, controls cooling rate at 2.8m/s, obtains the slab that thickness is 0.3mm;
3) Mechanical Crushing, obtains by Mechanical Crushing the meal that particle diameter is 150 μ m by slab;
4) hydrogen is quick-fried, the meal under the condition that is 1.5L/min at hydrogen flowing quantity, Mechanical Crushing being obtained is heated to 820 ℃, after insulation 8min, increase hydrogen flowing quantity to 4L/min and keep, inhale hydrogen 3h, arrange subsequently hydrogen and be filled with argon gas, when argon pressure reaches 0.9MPa, start to vacuumize dehydrogenation, during to vacuum degree 3Pa, dehydrogenation finishes;
5) grind, adopt airflow milling to grind, specifically add the zinc stearate of 0.12wt%, in nitrogen atmosphere, being crushed to average grain diameter is 40 μ m, obtains fine powder.
6) preliminary treatment, by fine powder with take after the polyamide-imide resin solution mixing and stirring that dimethylacetylamide is solvent, be heated to 150 ℃, solvent is volatilized and obtains cured film on magnetic surface; Wherein the mixing addition of polyamide-imide resin is 1 part with respect to magnetic powder 100 weight portions.
7) mixing, magnetic after overlay film is mixed with polyamide binding agent and interpolation auxiliary agent, in twin shaft mixing roll, carry out mixingly, melting temperature is 200 ℃, and mixing time is 30min, wherein, described polyamide is that molecular weight is 15000 nylon 6, and its addition is 3 parts with respect to the Magnaglo of 100 weight portions, and described interpolation auxiliary agent is 2,6-DI-tert-butylphenol compounds and active carbon, its addition is respectively 0.8 part and 1 part with respect to the Magnaglo of 100 weight portions.
8) injection moulding, mold temperature is preheating to 100 ℃, 240 ℃ of injection temperatures, in the magnetic field intensity of 1800kA/m,, the injection pressure hemostasis of 20MPa is shaped and pressurize, the Nd-Fe-B that obtains embodiment of the present invention 1-4 and comparative example 1-3 is bonded rare earth permanent magnetic alloy.
In described alloying element, Nd, Fe and B are the basic elements that forms neodymium iron boron principal phase, the content that must guarantee Nd surpasses 15.0, otherwise will be difficult to effectively form RE permanent magnetic alloy, yet its content can not be too high, otherwise will limit the interpolation quantity of other elements and affect the performance of alloy monolithic.B is also the basic composition element of principal phase, and its content should surpass 5.0, but too much interpolation can cause the deterioration of magnetic property.
Aluminium element can play significantly and improve coercitive effect, for the processing characteristics of improving alloy, play useful effect simultaneously, but excessive interpolation there is no benefit for coercitive raising, can cause on the contrary the remarkable decline of remanent magnetism, the Al in alloy system of the present invention should be in the scope of 0.2-0.3.
Cobalt element can obviously improve the Curie temperature of alloy system, but the interpolation of cobalt can obviously cause the decline of the performances such as remanent magnetism, coercive force, therefore must strictly control the addition of cobalt element, for it is played for the enough raising effects of Curie temperature, its addition at least should be 7.0, in order to limit the side effect of its interpolation, should control its content below 10.0 simultaneously.
Niobium and zirconium are all the elements of typical inhibiting grain growth, in alloy system, can play inhibiting grain growth, improve the effects such as squareness, its deficiency of adding content will affect magnetic and form anisotropy in dehydrogenation regrouping process, thus the remarkable deficiency of alloy system magnetic property after causing being shaped.
Copper can avoid principal phase for the excessively solid solution mutually of rich neodymium, thereby significantly improves coercive force, but the interpolation of too much copper can affect the level and smooth of main phase grain, thereby significantly falls low-alloyed magnetic property.In addition, copper can also play to a certain extent and suppress the effect that cobalt worsens magnetic property.
The interpolation of heavy rare earth element dysprosium can improve the coercive force of alloy system significantly, but its too much interpolation can worsen the performances such as remanent magnetism of alloy, and therefore limiting its addition is 3.0-5.0.
Table 1
RE permanent magnetic alloy system in the application, by the coordinative role between alloying element, has unforeseeablely obtained excellent comprehensive magnetic energy.
Embodiment 5-6, and comparative example 4-9, the chemical composition of alloy is identical with embodiment 2, mainly investigated the impact of preparation technology for alloy property, design parameter and test result are referring to table 2, wherein A represents the interpolation umber of polyamide-imides, B represents the interpolation umber of nylon 6/poly amide resin, C represents 2, the interpolation umber of 6-DI-tert-butylphenol compounds, D represents the interpolation umber of active carbon, E represent pretreated heating-up temperature (℃), F represent injection moulding temperature (℃), G represents the pressure (MPa) of injection moulding, H represents that temperature is 250 ℃, pressure is 100kgf/cm
2, the mixing constituent of magnetic that records of Φ 1mm * 7mm mouth mould fluidity of molten (g/10min), I is the remanent magnetism (T) of permanent magnetic material, J is that permanent magnetic material is soaked in the corrosion resistance test result after 24h in 5%NaCl salt solution (zero for no corrosion, * for there being obvious corrosion).
Table 2
Result by table 2 can find out, polyamide-imides overlay film has material impact for the mobility of magnetic/thermoplastic resin binder mixture, and this is mainly to come from intermiscibility good between polyamide-imides and polyamide thermoplastic resin; Meanwhile, polyamide-imides mechanical strength and heat resistance have also improved corrosion resistance and the antioxygenic property of material to a certain extent.For bringing into play above-mentioned effect, the addition of polyamide-imides at least should be 1.0 parts, thereby but too high addition can increase the viscosity of system on the contrary, reduces the mobility deterioration forming property of melt.
In addition the pretreated heating-up temperature of polyamide-imides overlay film also has material impact for the performance of overlay film, in order to guarantee the abundant volatilization dimethylacetylamide of solvent and to make polyamide-imides certain polymerization reaction occur and the overlay film that obtains hardening, to reach the object that mobility is provided, heating-up temperature should at least reach 150 ℃, but while surpassing 180 ℃, too high heating-up temperature has not had the effect further improving for fluidity of molten.
The addition of nylon 6/poly amide resin is limited in the scope of 3-5 part.If addition is less than 3 parts, by causing, the mixing resistance of mixed system is excessive, and mobility is too low, thereby make the difficulty that is shaped, conversely, if its addition is excessive, for example surpass 5 parts, do not reach the present invention improve Magnaglo useful load and improve magnetism of material can object.Meanwhile, in order to guarantee the mechanical strength of material, the number-average molecular weight that should limit nylon 6/poly amide resin is greater than 12000, but can not be too high, if surpass 18000, can cause the remarkable reduction of mobility, thereby worsens the forming property of system.
2,6-DI-tert-butylphenol compounds mainly plays two effects in system, the firstth, prevent the oxidation of mixing process and product, the secondth, the performance of raising injection moulding, for bringing into play above-mentioned effect, 2, the addition of 6-DI-tert-butylphenol compounds should at least reach 0.8 part, but can not be too high, too high meeting causes the mechanical property of formed product to worsen, and limits its addition for this reason and is less than 1 part.
Active carbon can effectively play heavy metal ion such as preventing Fe, Co and be oxidized, for bringing into play above-mentioned effect, preferably the addition of active carbon should be at least 1 part, but the mobility of the serious reduction system of too much active carbon addition meeting, also the fabrication strength of system can be affected, therefore its addition should be controlled below 1.4 parts.Meanwhile, in order to obtain the performance of enough Adsorption of Heavy Metal Ions, and avoid it for the anisotropic impact of magnetic, to reduce magnetic property, require the particle diameter of active carbon below 80 μ m.
Injection temperature and injection pressure have material impact for the final forming quality of material and magnetic property, injection temperature and injection pressure are too low, can cause illiquidity, the packed density of fluid too low, thereby worsen mechanical property and the magnetic property of moulding material, but excess Temperature, may cause resin glue to occur unnecessary crosslinked, and the cracking that causes moulding material, thereby affect the performance of material.
To sum up, reasonably combined by alloying element of the present invention, and suitable preparation technology, by injection molding process, prepared magnetic property and decay resistance all very excellent Nd-Fe-B be bonded rare earth permanent magnetic alloy.
Claims (2)
1. a novel Nd-Fe-B is bonded rare earth permanent magnetic alloy, it is characterized in that described Nd-Fe-B is that RE permanent magnetic alloy has following composition: in atomic percentage conc, Nd15.0-18.0, B5.0-6.0, Al0.2-0.3, Co7.0-10.0, Nb0.5-0.8, Zr0.1-0.3, Cu0.2-0.4, Dy3.0-5.0, surplus is Fe and inevitable impurity.
2. bonded rare earth permanent magnetic alloy according to claim 1, is characterized in that: the concrete preparation method of described bonded rare earth permanent magnetic alloy is as follows:
1) melting, the alloy raw material being equipped with is put into vacuum induction melting furnace, smelting furnace is evacuated to 15-20Pa and the melting of heating until temperature starts to be filled with argon gas to pressure while being warming up to 1150 ℃ is 0.3-0.4MPa, be warming up to subsequently 1350-1400 ℃ of refining 5-10 minute, be incubated standing 1-1.5 minute;
2) cast, adopts the method for getting rid of Strip casting, and chill roll diameter is 500mm, controls cooling rate at 2.7m/s-3m/s, obtains the slab that thickness is 0.2-0.4mm;
3) Mechanical Crushing, obtains by Mechanical Crushing the meal that particle diameter is 100-200 μ m by slab;
4) hydrogen is quick-fried, the meal under the condition that is 1-2L/min at hydrogen flowing quantity, Mechanical Crushing being obtained is heated to 800-820 ℃, after insulation 5-10min, increase hydrogen flowing quantity to 3-4L/min and keep, inhale hydrogen 2-3h, arrange subsequently hydrogen and be filled with argon gas, when argon pressure reaches 0.8-1MPa, start to vacuumize dehydrogenation, during to vacuum degree 2-4Pa, dehydrogenation finishes;
5) grind, adopt airflow milling to grind, specifically add the zinc stearate of 0.10-0.13wt%, in nitrogen atmosphere, being crushed to average grain diameter is 30-50 μ m, obtains fine powder.
6) preliminary treatment, by fine powder with take after the polyamide-imide resin solution mixing and stirring that dimethylacetylamide is solvent, be heated to 150-180 ℃, solvent is volatilized and obtains cured film on magnetic surface.
7) mixing, by the magnetic after overlay film and polyamide binding agent and add auxiliary agent and mix, in twin shaft mixing roll, carry out mixingly, melting temperature is 200-220 ℃, mixing time 30-40min.
8) injection moulding, is preheating to 100-120 ℃ by mold temperature, injection temperature 240-260 ℃, and in the magnetic field intensity of 1800-2000kA/m,, the injection pressure hemostasis of 20-25MPa is shaped and pressurize, obtaining Nd-Fe-B of the present invention is bonded rare earth permanent magnetic alloy.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62244105A (en) * | 1986-04-16 | 1987-10-24 | Hitachi Metals Ltd | Rare earth magnet |
| CN1359114A (en) * | 2000-11-28 | 2002-07-17 | 株式会社东金 | Magnetic core contaiing addrssive magnet with magnetic power with anti-oxidation metal coated on surface |
| CN101356593A (en) * | 2006-01-04 | 2009-01-28 | 住友电气工业株式会社 | Soft magnetic material, dust magnetic core, process for producing soft magnetic material and process for producing dust magnetic core |
| CN103056370A (en) * | 2012-12-31 | 2013-04-24 | 宁波中杭磁材有限公司 | Method of improving coercivity of sintering Nd-Fe-B magnetic material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62244105A (en) * | 1986-04-16 | 1987-10-24 | Hitachi Metals Ltd | Rare earth magnet |
| CN1359114A (en) * | 2000-11-28 | 2002-07-17 | 株式会社东金 | Magnetic core contaiing addrssive magnet with magnetic power with anti-oxidation metal coated on surface |
| CN101356593A (en) * | 2006-01-04 | 2009-01-28 | 住友电气工业株式会社 | Soft magnetic material, dust magnetic core, process for producing soft magnetic material and process for producing dust magnetic core |
| CN103056370A (en) * | 2012-12-31 | 2013-04-24 | 宁波中杭磁材有限公司 | Method of improving coercivity of sintering Nd-Fe-B magnetic material |
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Denomination of invention: A bonded rare earth permanent magnet alloy Effective date of registration: 20230515 Granted publication date: 20160302 Pledgee: China Construction Bank Corporation Fenghua sub branch Pledgor: NINGBO SONGKE MAGNETIC MATERIAL Co.,Ltd. Registration number: Y2023980040575 |