CN104347218A - Novel sintered ndfeb permanent magnet and preparation method thereof - Google Patents
Novel sintered ndfeb permanent magnet and preparation method thereof Download PDFInfo
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- CN104347218A CN104347218A CN201410595839.4A CN201410595839A CN104347218A CN 104347218 A CN104347218 A CN 104347218A CN 201410595839 A CN201410595839 A CN 201410595839A CN 104347218 A CN104347218 A CN 104347218A
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Abstract
The invention relates to a novel sintered ndfeb permanent magnet and a preparation method thereof. The composition expression of the sintered ndfeb permanent magnet is (Cex, Nd1-x)y-Mz-Fe100-y-zB0.9-1.05, wherein x is greater than or equal to 0.05 and smaller than or equal to 0.1, y is greater than or equal to 0.4 and smaller than or equal to 0.9, z is greater than or equal to 0.5 and smaller than or equal to 5, and M is one or several of Gd, Co, Al, Cu and Zr. After the composition of the sintered ndfeb permanent magnet is designed and the production technology is improved, the material cost of the product is reduced, the integrated performance is improved, the cost performance is increased comprehensively, and the magnetic property and the anti-demagnetization performance are improved; moreover, the manufacturing cost of the product is reduced effectively, and based on the current unit price of raw materials, the cost can be reduced by 16.5 yuan/kilo, and the power consumption can be reduced by 1 kwh/kilo.
Description
Technical field
The present invention relates to a kind of novel sintered Nd-Fe-B permanent magnet and preparation method thereof.
Background technology
Neodymium iron boron (chemical name Nd-Fe-B) rare earth permanent-magnetic material is third generation rare earth permanent magnet, due to its high energy product, high-coercive force and be referred to as " magnetic king ", has been widely used in the fields such as electronics, computer, automobile, machinery, the energy and medicine equipment.In Nd-Fe-B series permanent magnetic material, sintered Nd-Fe-B based magnet occupies an important position.
The quick growth of Nd-Fe-Bo permanent magnet material, the demand that rare earth metal Nd etc. are a large amount of, advantageously facilitate the development of rare earth raw material industry, but also result in the unbalance of rare earth resources utilization, in addition, raw material neodymium is on the high side, cause the production cost of sintered Nd-Fe-B permanent magnet high, and require higher sintering temperature in production process, energy consumption is high, require high to equipment performance, therefore need to develop the low sintered Nd-Fe-B permanent magnet of a kind of production cost.
Summary of the invention
The object of the invention is to solve the deficiencies in the prior art, a kind of novel sintered Nd-Fe-B permanent magnet is provided.The prices of raw and semifnished materials of cerium gadolinium are 1/8 of neodymium price, and the present invention's cerium, gadolinium replace part neodymium, can reduce cost of material, and reduce the sintering temperature of production technology, the performance of obtained sintered Nd-Fe-B permanent magnet and the Nd-Fe-B permanent magnet of prior art is suitable.
Another object of the present invention is to provide a kind of preparation method of novel sintered Nd-Fe-B permanent magnet, and the method technological design is reasonable, and sintering temperature is reduced, and energy consumption is low.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of novel sintered Nd-Fe-B permanent magnet, the composition expression formula of described sintered Nd-Fe-B permanent magnet is: (Ce
x, Nd
1-x)
y-M
z-Fe
100-y-zb
0.95-1.05, wherein 0.05≤x≤0.1,0.4≤y≤0.9,0.5≤z≤5, M is one or more in Gd and Co, Al, Cu, Zr.
A preparation method for novel sintered Nd-Fe-B permanent magnet, the preparation method of novel sintered Nd-Fe-B permanent magnet, is characterized in that: described method is carried out as follows:
(1) vacuum induction rapid hardening furnace is utilized, by ready NdFeB material, cerium and gadolinium iron under argon shield, melting at 1400-1600 DEG C of temperature, the molten steel of fusing is cast on the cooling copper rod of rotation, prepares the Nd Fe B alloys thin slice of 0.2-0.8mm thickness;
(2) utilize hydrogen broken 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 powder of 100-200 μm;
(3) powder step (2) obtained is broken into the Nd Fe B alloys powder of 2.8-3.1 μm further across airflow milling;
(4) utilize Magnetic field press, by the oriented moulding under the magnetic field of 1.5T of the powder mixed in step (3), then through isostatic cool pressing, pressure is 200Mpa, and obtaining density is 4.5-4.8g/cm
3pressed compact;
(5) pressed compact is placed in vacuum sintering furnace, at 1065-1090 DEG C of sintered heat insulating 4-5h, at 850-900 DEG C of one-level tempering insulation 0.5-2h, at 450-510 DEG C of second annealing insulation 3-5h, finally obtains sintered Nd-Fe-B permanent magnet.
As preferably, the preparation method of described novel sintered Nd-Fe-B permanent magnet carries out as follows:
(1) vacuum induction rapid hardening furnace is utilized, by ready NdFeB material, cerium and gadolinium iron under argon shield, melting at 1500-1550 DEG C of temperature, the molten steel of fusing is cast on the cooling copper rod of rotation, prepares the Nd Fe B alloys thin slice of 0.4-0.6mm thickness;
(2) utilize hydrogen broken 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 powder of 120-160 μm;
(3) powder step (2) obtained is broken into the Nd Fe B alloys powder of 3.0 μm further across airflow milling;
(4) utilize Magnetic field press, by the oriented moulding under the magnetic field of 1.5T of the powder mixed in step (3), then through isostatic cool pressing, pressure is 200Mpa, and obtaining density is 4.5-4.8g/cm
3pressed compact;
(5) pressed compact is placed in vacuum sintering furnace, at 1075-1085 DEG C of sintered heat insulating 4-5h, at 860-880 DEG C of one-level tempering insulation 0.5-2h, at 480-500 DEG C of second annealing insulation 3-5h, finally obtains sintered Nd-Fe-B permanent magnet.
As preferably, in described step (1), the purity of cerium used is 99.5%, and in gadolinium iron used, the mass fraction of gadolinium is 71-72%.
The invention has the beneficial effects as follows:
1, by design the composition of sintered Nd-Fe-B permanent magnet and production technology is improved, the material cost of product is reduced, combination property improves, and General Promotion in cost performance, improves magnetic property, anti-demagnetization;
2, adopt fast solidifying slab, hydrogen decrepitation route, take forced airflow abrasive dust simultaneously, control granularity of magnet powder distribution, realize particle mean size between 2.8 ~ 3.1 microns, adopt multi-steps sintering, reduce most high sintering temperature, realize crystal grain thinning, improve the target of micro-structural;
3, improve granularity of magnet powder distribution, improve magnet structure, improve the stability and magnetism energy uniformity of magnet.
4, effectively reduce production cost, by current raw material unit price, 16.5 yuan/kilogram can be reduced costs, reduce power consumption 1 degree/kilogram.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1:
A kind of novel sintered Nd-Fe-B permanent magnet, the composition expression formula of described sintered Nd-Fe-B permanent magnet is: (Ce
0.05, Nd
0.95)
0.4-Co
0.2-Gd
0.3-Fe
99.1b
0.95.
The preparation method of above-mentioned sintered Nd-Fe-B permanent magnet carries out as follows:
(1) vacuum induction rapid hardening furnace is utilized, by ready NdFeB material, cerium, gadolinium iron and cobalt under argon shield, melting at 1400-1450 DEG C of temperature, the molten steel of fusing is cast on the cooling copper rod of rotation, prepare the Nd Fe B alloys thin slice of 0.2-0.4mm thickness, the purity of cerium used is 99.5%, and in gadolinium iron used, the mass fraction of gadolinium is 71%;
(2) utilize hydrogen broken 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 powder of 100-150 μm;
(3) powder step (2) obtained is broken into the Nd Fe B alloys powder of 2.8-3.0 μm further across airflow milling;
(4) utilize Magnetic field press, by the oriented moulding under the magnetic field of 1.5T of the powder mixed in step (3), then through isostatic cool pressing, pressure is 200Mpa, and obtaining density is 4.5g/cm
3pressed compact;
(5) pressed compact is placed in vacuum sintering furnace, at 1065-1075 DEG C of sintered heat insulating 5h, at 850-870 DEG C of one-level tempering insulation 2h, at 450-470 DEG C of second annealing insulation 5h, finally obtains sintered Nd-Fe-B permanent magnet.
Embodiment 2:
A kind of novel sintered Nd-Fe-B permanent magnet, the composition expression formula of described sintered Nd-Fe-B permanent magnet is: (Ce
0.1, Nd
0.9)
0.9-Cu
1.0-Gd
2.0-Zr
2.0-Fe
94.1b
1.05.
The preparation method of above-mentioned sintered Nd-Fe-B permanent magnet carries out as follows:
(1) vacuum induction rapid hardening furnace is utilized, by ready NdFeB material, cerium, gadolinium iron, copper and zirconium under argon shield, melting at 1550-1600 DEG C of temperature, the molten steel of fusing is cast on the cooling copper rod of rotation, prepare the Nd Fe B alloys thin slice of 0.6-0.8mm thickness, the purity of cerium used is 99.5%, and in gadolinium iron used, the mass fraction of gadolinium is 72%;
(2) utilize hydrogen broken 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 powder of 180-200 μm;
(3) powder step (2) obtained is broken into the Nd Fe B alloys powder of 3.0-3.1 μm further across airflow milling;
(4) utilize Magnetic field press, by the oriented moulding under the magnetic field of 1.5T of the powder mixed in step (3), then through isostatic cool pressing, pressure is 200Mpa, and obtaining density is 4.8g/cm
3pressed compact;
(5) pressed compact is placed in vacuum sintering furnace, at 1080-1090 DEG C of sintered heat insulating 4h, at 880-900 DEG C of one-level tempering insulation 0.5h, at 500-510 DEG C of second annealing insulation 3h, finally obtains sintered Nd-Fe-B permanent magnet.
Embodiment 3:
A kind of novel sintered Nd-Fe-B permanent magnet, the composition expression formula of described sintered Nd-Fe-B permanent magnet is: (Ce
0.075, Nd
0.925)
0.5-Gd
0.5-Al
2.0-Fe
97b
1.0.
The preparation method of above-mentioned sintered Nd-Fe-B permanent magnet carries out as follows:
(1) vacuum induction rapid hardening furnace is utilized, by ready NdFeB material, cerium and gadolinium iron under argon shield, melting at 1500-1550 DEG C of temperature, the molten steel of fusing is cast on the cooling copper rod of rotation, prepare the Nd Fe B alloys thin slice of 0.4-0.6mm thickness, the purity of cerium used is 99.5%, and in gadolinium iron used, the mass fraction of gadolinium is 71%;
(2) utilize hydrogen broken 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 powder of 120-160 μm;
(3) powder step (2) obtained is broken into the Nd Fe B alloys powder of 3.0 μm further across airflow milling;
(4) utilize Magnetic field press, by the oriented moulding under the magnetic field of 1.5T of the powder mixed in step (3), then through isostatic cool pressing, pressure is 200Mpa, and obtaining density is 4.6g/cm
3pressed compact;
(5) pressed compact is placed in vacuum sintering furnace, at 1075-1080 DEG C of sintered heat insulating 4.5h, at 860-880 DEG C of one-level tempering insulation 1.5h, at 480-500 DEG C of second annealing insulation 4h, finally obtains sintered Nd-Fe-B permanent magnet.
The novel sintered Nd-Fe-B permanent magnet that embodiment 1-3 is obtained, magnetic property testing result is as follows:
Above-described embodiment is one of the present invention preferably scheme, not does any pro forma restriction to the present invention, also has other variant and remodeling under the prerequisite not exceeding the technical scheme described in claim.
Claims (4)
1. a novel sintered Nd-Fe-B permanent magnet, is characterized in that: the composition expression formula of described sintered Nd-Fe-B permanent magnet is: (Ce
x, Nd
1-x)
y-M
z-Fe
100-y-zb
0.95-1.05, wherein 0.05≤x≤0.1,0.4≤y≤0.9,0.5≤z≤5, M is one or more in Gd and Co, Al, Cu and Zr.
2. a preparation method for novel sintered Nd-Fe-B permanent magnet according to claim 1, is characterized in that: the preparation method of novel sintered Nd-Fe-B permanent magnet, is characterized in that: described method is carried out as follows:
(1) vacuum induction rapid hardening furnace is utilized, by ready raw material under argon shield, melting at 1400-1600 DEG C of temperature, the molten steel of fusing is cast on the cooling copper rod of rotation, prepares the Nd Fe B alloys thin slice of 0.2-0.8mm thickness;
(2) utilize hydrogen broken 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 powder of 100-200 μm;
(3) powder step (2) obtained is broken into the Nd Fe B alloys powder of 2.8-3.1 μm further across airflow milling;
(4) utilize Magnetic field press, by the oriented moulding under the magnetic field of 1.5T of the powder mixed in step (3), then through isostatic cool pressing, pressure is 200Mpa, and obtaining density is 4.5-4.8g/cm
3pressed compact;
(5) pressed compact is placed in vacuum sintering furnace, at 1065-1090 DEG C of sintered heat insulating 4-5h, at 850-900 DEG C of one-level tempering insulation 0.5-2h, at 450-510 DEG C of second annealing insulation 3-5h, finally obtains sintered Nd-Fe-B permanent magnet.
3. the preparation method of novel sintered Nd-Fe-B permanent magnet according to claim 2, is characterized in that: described method is carried out as follows:
(1) vacuum induction rapid hardening furnace is utilized, by ready NdFeB material, cerium and gadolinium iron under argon shield, melting at 1500-1550 DEG C of temperature, the molten steel of fusing is cast on the cooling copper rod of rotation, prepares the Nd Fe B alloys thin slice of 0.4-0.6mm thickness;
(2) utilize hydrogen broken 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 powder of 120-160 μm;
(3) powder step (2) obtained is broken into the Nd Fe B alloys powder of 3.0 μm further across airflow milling;
(4) utilize Magnetic field press, by the oriented moulding under the magnetic field of 1.5T of the powder mixed in step (3), then through isostatic cool pressing, pressure is 200Mpa, and obtaining density is 4.6g/cm
3pressed compact;
(5) pressed compact is placed in vacuum sintering furnace, at 1075-1085 DEG C of sintered heat insulating 4-5h, at 860-880 DEG C of one-level tempering insulation 0.5-2h, at 480-500 DEG C of second annealing insulation 3-5h, finally obtains sintered Nd-Fe-B permanent magnet.
4. the preparation method of the novel sintered Nd-Fe-B permanent magnet according to Claims 2 or 3, is characterized in that: in described step (1), the purity of cerium used is 99.5%, and in gadolinium iron used, the mass fraction of gadolinium is 71-72%.
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Cited By (8)
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CN104821226A (en) * | 2015-05-07 | 2015-08-05 | 安徽万磁电子有限公司 | Method for making high-square-degree sintered NdFeB permanent magnets with cerium, titanium, cobalt and zirconium compound additive |
CN104900360A (en) * | 2015-05-28 | 2015-09-09 | 钢铁研究总院 | Novel permanent magnet alloy with composite low-price rare earth added and preparation method thereof |
CN105185500A (en) * | 2015-08-28 | 2015-12-23 | 包头天和磁材技术有限责任公司 | Preparation method of permanent magnet material |
CN106024242A (en) * | 2016-07-14 | 2016-10-12 | 安徽万磁电子有限公司 | Corrosion-resistant nickel-plated neodymium-iron-boron raw material powder and preparation method thereof |
CN107393711A (en) * | 2017-07-12 | 2017-11-24 | 浙江中科磁业有限公司 | A kind of preparation method of high-coercivity magnet |
CN108022708A (en) * | 2017-12-20 | 2018-05-11 | 包头金山磁材有限公司 | A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous and preparation method thereof |
CN108630369A (en) * | 2018-06-19 | 2018-10-09 | 江苏江淮磁业有限公司 | A kind of neodymium cerium Fe-Mn magnetism material preparation method based on cerium |
CN110257724A (en) * | 2019-07-16 | 2019-09-20 | 宁德市星宇科技有限公司 | A kind of preparation method of the neodymium iron boron magnetic body containing lanthanum and cerium |
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Cited By (10)
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CN104821226A (en) * | 2015-05-07 | 2015-08-05 | 安徽万磁电子有限公司 | Method for making high-square-degree sintered NdFeB permanent magnets with cerium, titanium, cobalt and zirconium compound additive |
CN104900360A (en) * | 2015-05-28 | 2015-09-09 | 钢铁研究总院 | Novel permanent magnet alloy with composite low-price rare earth added and preparation method thereof |
CN104900360B (en) * | 2015-05-28 | 2017-07-25 | 钢铁研究总院 | A kind of permanent-magnet alloy for adding compound low price rare earth and preparation method thereof |
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CN106024242A (en) * | 2016-07-14 | 2016-10-12 | 安徽万磁电子有限公司 | Corrosion-resistant nickel-plated neodymium-iron-boron raw material powder and preparation method thereof |
CN107393711A (en) * | 2017-07-12 | 2017-11-24 | 浙江中科磁业有限公司 | A kind of preparation method of high-coercivity magnet |
CN108022708A (en) * | 2017-12-20 | 2018-05-11 | 包头金山磁材有限公司 | A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous and preparation method thereof |
CN108630369A (en) * | 2018-06-19 | 2018-10-09 | 江苏江淮磁业有限公司 | A kind of neodymium cerium Fe-Mn magnetism material preparation method based on cerium |
CN110257724A (en) * | 2019-07-16 | 2019-09-20 | 宁德市星宇科技有限公司 | A kind of preparation method of the neodymium iron boron magnetic body containing lanthanum and cerium |
CN110257724B (en) * | 2019-07-16 | 2020-05-22 | 宁德市星宇科技有限公司 | Preparation method of neodymium-iron-boron magnet containing lanthanum and cerium |
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