CN105118655A - Method for preparing high-coercivity magnet by modifying nano zinc powder crystal boundary - Google Patents
Method for preparing high-coercivity magnet by modifying nano zinc powder crystal boundary Download PDFInfo
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- CN105118655A CN105118655A CN201510589785.5A CN201510589785A CN105118655A CN 105118655 A CN105118655 A CN 105118655A CN 201510589785 A CN201510589785 A CN 201510589785A CN 105118655 A CN105118655 A CN 105118655A
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Abstract
The invention discloses a method for preparing a high-coercivity magnet by modifying the nano zinc powder crystal boundary. The method includes the steps that 20% of Nd, 5.5% of Pr, 1.5% of Gd, 3.5% of Ho, 64.65% of Fe, 1% of B, 1% of Nb, 2% of Co, 0.7% of Al and 0.15% of Cu, by mass, are used for preparing raw materials, smelting is conducted, smelted alloy liquid is evenly stirred to be poured onto a rotating water-cooling copper bar, and an alloy sheet with the thickness being 0.2-0.5 mm is formed after fast cooling; the NdFeB alloy sheet is crushed into NdFeB alloy particles of 120-200 microns; the particles are further crushed into NdFeB alloy powder of 2.5-3.0 microns through an airflow mill; zinc slabs are machined into extremely-fine nanoscale metal powder of over 1500 meshes through a series of processes; the nano zinc powder is added into the NdFeB alloy powder according to a certain proportion to be evenly mixed; the mixed powder is formed in a forming press, and is further densified through isostatic cool pressing; after formed primary blank is sintered, a sintered permanent magnet is obtained.
Description
Technical field
The invention belongs to technical field of magnetic materials, be specifically related to a kind of crystal boundary modified method preparing high-coercivity magnet of nano zinc powder.
Background technology
Sintered NdFeB magnet has superior magnetic property, in each field of modern science and technology, as the aspects such as wind power generation, nulcear magnetic resonance (NMR), auto industry, computer, Aero-Space, household electrical appliance obtain extensive use.Along with the development of industry, the requirement of industry to magnet magnetic property is more and more higher.
The development of NdFeB mainly comes from the high energy product of material, but the actual HCJ of magnet is but often the 1/3-1/30 of theoretical value, and the working temperature and the stability which results in material are relatively low, constrain further developing and applying of NdFeB.For addressing this problem, the coercive force of NdFeB must be improved.Improve in current industrial production, improve magnet coercitive approach and mainly contain and add useful alloying element and optimize the preparation technologies such as melting, powder process, shaping, sintering.Add alloying element and can be divided into two large classes, the first kind be by add heavy rare earth element Dy, Tb come alternative Hard Magnetic mutually in Nd, the coercive force of material can be promoted significantly, but the method is with the magnetic energy product of expendable material for cost, and expensive Dy, Tb increase the production cost of magnet significantly simultaneously.Equations of The Second Kind is that doping adds non-thulium in magnet, comprises low-melting-point metal Al, Ga, Cu, Sn etc. and refractory metal Nb, Zr, Ti etc.Low-melting-point metal can improve the wetability of rich-Nd phase, and high-melting-point element effectively can suppress growing up of crystal grain in sintering process, finally effectively can improve the coercive force of magnet, but the non magnetic Br and (BH) that reduce magnet of meeting of these Element generations
max.In addition, the method for adding alloying element also has various ways, both can add in the batching before melting, and can be mixed in proportion by the alloy powder of required interpolation again before airflow milling powder with magnetic.
Summary of the invention
The object of the present invention is to provide a kind of crystal boundary modified method preparing high-coercivity magnet of nano zinc powder.
For achieving the above object, the present invention adopts following technical scheme:
The crystal boundary modified method preparing high-coercivity magnet of nano zinc powder, concrete steps are as follows:
(1) prepare following alloy raw material by mass fraction: 20%Nd, 5.5%Pr, 1.5%Gd, 3.5%Ho, 64.65%Fe, 1%B, 1%Nb, 2%Co, 0.7%Al, 0.15%Cu, utilize vacuum induction rapid hardening slab stove that raw material metal good for proportioning is carried out melting at 1200-1400 DEG C of temperature; Before melting, furnace chamber first vacuumizes, then is filled with protective gas high-purity argon gas; Aluminium alloy after raw material fusing is even through electromagnetic agitation, is poured on the water-cooled copper rod of rotation, and alloy solution cools fast and forms thickness under the cooling rate of 102-104 DEG C/s is the alloy sheet of 0.2-0.5mm;
(2) utilize hydrogen crushing furnace, under 0.1MPa hydrogen-pressure, inhale hydrogen, dehydrogenation at 550 DEG C of temperature, Nd Fe B alloys thin slice is broken into the Nd Fe B alloys particle of 120-200 μm;
(3) particle step (2) obtained is broken into the Nd Fe B alloys powder of 2.5-3.0 μm further across airflow milling;
(4) by spelter order through melting, dust, wet ball mill, annealing, smart ball milling, the operation such as polishing process the imperceptible nano level metal powder of more than 1500 orders;
(5) nano zinc powder of preparation is joined by a certain percentage in the obtained Nd Fe B alloys powder of step (3), and utilize three-dimensional mixer, powder is fully mixed;
(6) utilize Magnetic field press, by powder oriented moulding under the magnetic field of 1.8T in step (5), then through isostatic cool pressing, pressure is 200MPa, and the first base density obtained is 4.5-5.0g/cm
3;
(7) pressed compact is placed in vacuum sintering furnace, at 1060-1100 DEG C of sintered heat insulating 3-4 hour; One-level temperature is 850-950 DEG C, insulation 1-2 hour; Second annealing temperature is 450-600 DEG C, insulation 3-4 hour; Final acquisition sintered permanent magnet.
In described step (1), smelting temperature is 1380 DEG C.
The ratio of nano zinc powder and Nd Fe B alloys powder 1:50 in mass ratio mixes in described step (5), utilizes three-dimensional mixer to stir 4 hours.
In described step (7), sintering temperature is 1070 DEG C, and sintering time is 4 hours; One-level temperature is 850 DEG C, is incubated 1.5 hours; Second annealing temperature is 490 DEG C, is incubated 4 hours.
Beneficial effect of the present invention:
The present invention by adding nano zinc powder in Nd Fe B alloys powder, and improve neodymium iron boron Grain-Boundary Phase, Sintered NdFeB magnet remanent magnetism and coercive force rise all to some extent, and particularly the coercive force of magnet has a distinct increment, and comprehensive magnetic can be improved.
Embodiment
Embodiments of the invention are only for illustration of technical scheme of the present invention, and non-limiting the present invention.
Utilize the crystal boundary modified method preparing N38SH sintered Nd-Fe-B permanent magnet of nano zinc powder of the present invention, concrete steps are as follows:
(1) prepare following alloy raw material by mass fraction: 20%Nd, 5.5%Pr, 1.5%Gd, 3.5%Ho, 64.65%Fe, 1%B, 1%Nb, 2%Co, 0.7%Al, 0.15%Cu, utilize vacuum induction rapid hardening slab stove that raw material metal good for proportioning is carried out melting at the temperature of 1380 DEG C.Before melting, furnace chamber first vacuumizes, then is filled with protective gas high-purity argon gas.Aluminium alloy after raw material fusing is even through electromagnetic agitation, and be poured on the water-cooled copper rod of rotation, alloy solution is 10
2-10
4dEG C/cooling rate of s under cooling forms thickness is fast the alloy sheet of 0.2-0.5mm;
(2) utilize hydrogen crushing furnace, under 0.1MPa hydrogen-pressure, inhale hydrogen, dehydrogenation at 550 DEG C of temperature, Nd Fe B alloys thin slice is broken into the Nd Fe B alloys particle of 120-200 μm;
(3) by step 2) particle that obtains is broken into the Nd Fe B alloys powder of 2.5-3.0 μm further across airflow milling;
(4) by spelter order through melting, dust, wet ball mill, annealing, smart ball milling, the operation such as polishing process the imperceptible nano level metal powder of more than 1500 orders;
(5) by the 1:50 mixing in mass ratio of the nano zinc powder of preparation; And utilize three-dimensional mixer fully to stir 4 hours, powder is fully mixed;
(6) Magnetic field press is utilized, by step 3) middle powder oriented moulding under the magnetic field of 1.8T, then through isostatic cool pressing, pressure is 200MPa, the first base density obtained is 4.5-5.0g/cm
3;
(7) pressed compact is placed in vacuum sintering furnace, 1070 DEG C of sintered heat insulatings 4 hours; One-level temperature is 850 DEG C, is incubated 1.5 hours; Second annealing temperature is 490 DEG C, is incubated 4 hours; Final acquisition sintered permanent magnet;
8) magnetic property is tested: the magnetic property at 20 DEG C, result is as following table.To not add the crystal boundary modified sintered NdFeB of nano zinc powder sample as a comparison, other composition of Nd Fe B alloys powder is just the same.
Claims (4)
1. the crystal boundary modified method preparing high-coercivity magnet of nano zinc powder, it is characterized in that, concrete steps are as follows:
(1) prepare following alloy raw material by mass fraction: 20%Nd, 5.5%Pr, 1.5%Gd, 3.5%Ho, 64.65%Fe, 1%B, 1%Nb, 2%Co, 0.7%Al, 0.15%Cu, utilize vacuum induction rapid hardening slab stove that raw material metal good for proportioning is carried out melting at 1200-1400 DEG C of temperature; Before melting, furnace chamber first vacuumizes, then is filled with protective gas high-purity argon gas; Aluminium alloy after raw material fusing is even through electromagnetic agitation, is poured on the water-cooled copper rod of rotation, and alloy solution cools fast and forms thickness under the cooling rate of 102-104 DEG C/s is the alloy sheet of 0.2-0.5mm;
(2) utilize hydrogen crushing furnace, under 0.1MPa hydrogen-pressure, inhale hydrogen, dehydrogenation at 550 DEG C of temperature, Nd Fe B alloys thin slice is broken into the Nd Fe B alloys particle of 120-200 μm;
(3) particle step (2) obtained is broken into the Nd Fe B alloys powder of 2.5-3.0 μm further across airflow milling;
(4) by spelter order through melting, dust, wet ball mill, annealing, smart ball milling, the operation such as polishing process the imperceptible nano level metal powder of more than 1500 orders;
(5) nano zinc powder of preparation is joined by a certain percentage in the obtained Nd Fe B alloys powder of step (3), and utilize three-dimensional mixer, powder is fully mixed;
(6) utilize Magnetic field press, by powder oriented moulding under the magnetic field of 1.8T in step (5), then through isostatic cool pressing, pressure is 200MPa, and the first base density obtained is 4.5-5.0g/cm
3;
(7) pressed compact is placed in vacuum sintering furnace, at 1060-1100 DEG C of sintered heat insulating 3-4 hour; One-level temperature is 850-950 DEG C, insulation 1-2 hour; Second annealing temperature is 450-600 DEG C, insulation 3-4 hour; Final acquisition sintered permanent magnet.
2. the crystal boundary modified method preparing high-coercivity magnet of a kind of nano zinc powder according to claim 1, is characterized in that, in described step (1), smelting temperature is 1380 DEG C.
3. the crystal boundary modified method preparing high-coercivity magnet of a kind of nano zinc powder according to claim 1, it is characterized in that, the ratio of nano zinc powder and Nd Fe B alloys powder 1:50 in mass ratio mixes in described step (5), utilizes three-dimensional mixer to stir 4 hours.
4. the crystal boundary modified method preparing high-coercivity magnet of a kind of nano zinc powder according to claim 1, is characterized in that, in described step (7), sintering temperature is 1070 DEG C, and sintering time is 4 hours; One-level temperature is 850 DEG C, is incubated 1.5 hours; Second annealing temperature is 490 DEG C, is incubated 4 hours.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105355412A (en) * | 2015-12-07 | 2016-02-24 | 北京科技大学 | Method for obtaining high-magnetism sintered NdFeB through sulfidizing |
| CN105355413A (en) * | 2015-12-07 | 2016-02-24 | 北京科技大学 | Method for preparing high-magnetism sintered neodymium iron boron by reducing sintering temperature |
| CN106229102A (en) * | 2016-08-23 | 2016-12-14 | 南京工程学院 | A kind of Ultra-fine Grained NdFeB permanent magnet material and preparation method thereof |
| CN107134338A (en) * | 2017-05-17 | 2017-09-05 | 张卫华 | A kind of neodymium iron boron binding magnetic of compound addition zinc and gadolinium and preparation method thereof |
| TWI672725B (en) * | 2017-09-27 | 2019-09-21 | 大陸商北京北方華創微電子裝備有限公司 | Process chamber and capacitively coupled plasma device |
| CN110379580A (en) * | 2019-06-25 | 2019-10-25 | 宁波合力磁材技术有限公司 | A kind of neodymium-iron-boron preparation and the not neodymium iron boron magnetic body of cracky |
| CN113838622A (en) * | 2021-09-26 | 2021-12-24 | 太原理工大学 | High-coercivity sintered neodymium-iron-boron magnet and preparation method thereof |
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| JPH09223617A (en) * | 1996-12-17 | 1997-08-26 | Mitsubishi Materials Corp | Rare earth-b-fe sintered magnet superior in corrosion resistance and magnetic characteristic and manufacturing method thereof |
| CN102568731A (en) * | 2011-12-31 | 2012-07-11 | 北京工业大学 | High-corrosion-resistance sintered neodymium-iron-boron-based permanent magnet material prepared by doping zinc nano-particles and preparation method thereof |
| CN104821218A (en) * | 2015-05-07 | 2015-08-05 | 安徽万磁电子有限公司 | Sintered Nd-Fe-B magnet with zinc-aluminum-titanium-cobalt composite additive and preparation method thereof |
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| JPH09223617A (en) * | 1996-12-17 | 1997-08-26 | Mitsubishi Materials Corp | Rare earth-b-fe sintered magnet superior in corrosion resistance and magnetic characteristic and manufacturing method thereof |
| CN102568731A (en) * | 2011-12-31 | 2012-07-11 | 北京工业大学 | High-corrosion-resistance sintered neodymium-iron-boron-based permanent magnet material prepared by doping zinc nano-particles and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105355412A (en) * | 2015-12-07 | 2016-02-24 | 北京科技大学 | Method for obtaining high-magnetism sintered NdFeB through sulfidizing |
| CN105355413A (en) * | 2015-12-07 | 2016-02-24 | 北京科技大学 | Method for preparing high-magnetism sintered neodymium iron boron by reducing sintering temperature |
| CN106229102A (en) * | 2016-08-23 | 2016-12-14 | 南京工程学院 | A kind of Ultra-fine Grained NdFeB permanent magnet material and preparation method thereof |
| CN106229102B (en) * | 2016-08-23 | 2019-05-31 | 南京工程学院 | A kind of Ultra-fine Grained NdFeB permanent-magnet material and preparation method thereof |
| CN107134338A (en) * | 2017-05-17 | 2017-09-05 | 张卫华 | A kind of neodymium iron boron binding magnetic of compound addition zinc and gadolinium and preparation method thereof |
| CN107134338B (en) * | 2017-05-17 | 2020-06-23 | 成都银磁材料有限公司 | Neodymium-iron-boron bonded magnetic powder compositely added with zinc and gadolinium and preparation method thereof |
| TWI672725B (en) * | 2017-09-27 | 2019-09-21 | 大陸商北京北方華創微電子裝備有限公司 | Process chamber and capacitively coupled plasma device |
| CN110379580A (en) * | 2019-06-25 | 2019-10-25 | 宁波合力磁材技术有限公司 | A kind of neodymium-iron-boron preparation and the not neodymium iron boron magnetic body of cracky |
| CN110379580B (en) * | 2019-06-25 | 2021-07-23 | 宁波合力磁材技术有限公司 | Preparation method of neodymium iron boron magnet and neodymium iron boron magnet not easy to damage |
| CN113838622A (en) * | 2021-09-26 | 2021-12-24 | 太原理工大学 | High-coercivity sintered neodymium-iron-boron magnet and preparation method thereof |
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