CN102360655A - Yttrium-containing neodymium-iron-boron permanent magnetic material - Google Patents
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Abstract
The invention discloses an yttrium-containing neodymium-iron-boron permanent magnetic material. The composition of the material is RealphaYdeltaGdbetaBxiCuepsilonNupsilonFe100-alpha-beta-delta-xi-epsilon-upsilon, wherein Re is Nd or at least one element or more than one element of Nd, Pr, Ho, Tb, La, Ce and Dy; N is an adding element which comprises one or more than one element of Al, Mn, Ti, Ni, Zn, Ga, Cr and Mo; alpha, beta, delta, xi, epsilon and upsilon are weight percentage contents of each element; Fe is Fe and inevitable impurities; alpha+beta+delta is greater than or equal to 28 and is less than or equal to 33; delta is greater than or equal to 1 and is less than or equal to 10; beta is greater than 0.5 and is less than or equal to 5; xi is greater than or equal to 1 and is less than or equal to 1.2; epsilon is greater than or equal to 0.03 and is less than or equal to 0.25; and upsilon is greater than 0 and is less than or equal to 0.25. By compositely adding Y and Gd, expensive neodymium element can be substituted as much as possible while coercive force of a magnet is guaranteed, and the manufacturing cost is reduced. Particularly, the density of the magnet is reduced by composite addition of Y and Gd, so that processing performance of the neodymium-iron-boron material is improved.
Description
Technical field
The present invention relates to the technology of preparing of nd-fe-b permanent magnetic alloy, relate in particular to a kind of Nd-Fe-Bo permanent magnet material that contains yttrium.
Background technology
Nd-Fe-Bo permanent magnet material is the present the strongest permanent magnet of magnetic in the world, is described as " king of permanent magnetism ".Replace other permanent magnetic materials with it, device volume and weight are descended at double, thereby obtained to use very widely.Become the indispensable functional material of automobile making, universal machine, electronics and information industry and sophisticated technology at present.At present along with country significantly rises to its price of control of rare earth element, NdFeB material exists that processing characteristics is relatively poor, cutting speed is slow, processing cost is high simultaneously, the not high defective of passing rate of processing.
The technological improvement of pair the problems referred to above is also arranged in the prior art; As the comparatively advanced Chinese invention patent patent No. 2,007 1 0090597.3 disclosed Nd-Fe-B rare earth permanent magnetic material and the manufacturing approaches thereof that contain gadolinium wherein adopt Nd-Fe-Bo permanent magnet material to add gadolinium to improve performance and to reduce manufacturing price; Wherein use a kind of element cobalt of necessity; Present part cobalt has radioactivity and need detect use; Do not describe the technical scheme of the Nd-Fe-B rare earth permanent magnetic material of not using cobalt in this technology, do not specifically describe the Nd-Fe-B rare earth permanent magnetic material of using yttrium yet.The Chinese invention patent patent No. 200910119435.7 discloses the Nd-Fe-Bo permanent magnet material that contains yttrium and this kind of manufacturing approach technical scheme thereof and discloses the technical scheme that Nd-Fe-Bo permanent magnet material adds yttrium and produced beneficial effect in addition, does not wherein describe the technical scheme that Nd-Fe-Bo permanent magnet material adds gadolinium.The combination of above-mentioned two kinds of schemes can not be inferred the concrete technical scheme that gadolinium and yttrium can add together.
Summary of the invention
The present invention provides a kind of and reduces manufacturing cost, improves processing characteristics, improves the coercitive Nd-Fe-Bo permanent magnet material that contains yttrium.
A kind of Nd-Fe-Bo permanent magnet material that contains yttrium, it consists of: Re
αY
δGd
βB
ξCu
εN
νFe
100-alpha-beta-δ-ξ-ε-ν,
Re is at least a element or more than one element among Nd or Nd and Pr, Ho, Tb, La, Ce, the Dy;
N comprises one or more elements of Al, Mn, Ti, Ni, Zn, Ga, Cr and Mo for adding element;
α, β, δ, ε, ν, ξ are the weight percent content of each element;
Fe is Fe and unavoidable impurities;
Wherein, 28≤alpha+beta+δ≤33,1≤δ≤10,0.5＜β≤5,1≤ξ≤1.2,0.03≤ε≤0.25,0＜ν≤0.25.Can find out that according to prescription provided by the invention Y and Gd are necessary element; Through being used in combination under the prerequisite that keeps NdFeB permanent magnetic material performance of Y and Gd; More substitute present expensive Nd to reduce manufacturing cost, reduced the Nd-Fe-Bo permanent magnet material difficulty of processing simultaneously.Gd can improve the thermal endurance of magnet specifically, and improves coercive force, and the weight ratio that excessive interpolation does not have significantly to act on zone of reasonableness is 0.5-5%.The density that Y can reduce Nd-Fe-Bo permanent magnet material makes process velocity be improved, and the weight ratio that excessive interpolation will influence the magnetism of material zone of reasonableness is 1-10%.Can significantly improve the thermal endurance and the coercive force Nd that substituted as much as possible of magnet through compound interpolation Y and Gd, the weight ratio of compound interpolation Y and its zone of reasonableness of Gd is 1.5-15%
Can be 28≤alpha+beta+δ＜31 as preferred described alpha+beta+δ value; Described δ value is 4≤δ≤8; Described β value is that 1≤β≤3 are to realize best magnet structure.
Contain at least a element or the magnet of more than one elements among Nd in the rare earth element Re or Nd and Pr, Ho, Tb, La, Ce, the Dy, can in magnet, produce higher coercive force and remanent magnetism.Preferred Nd of above element and Ce; Or Nd and La.The compound use of Nd and Ce is crystal grain thinning further, improves coercive force, and the weight ratio of Ce its zone of reasonableness in Re is 0.5-3%.Same Nd and the compound use of La be further crystal grain thinning also, the raising coercive force, and the weight ratio of La its zone of reasonableness in Re is 0.5-5%.
Contain the magnet that adds one or more elements of Al, Mn, Ti, Ni, Zn, Ga, Cr and Mo among the element N, can improve coercive force and remanent magnetism in the magnet.Be preferably and add Al; Or Al and Ga.Can significantly improve the coercive force in the magnet after adding Al, adding the rational weight ratio of excessive not remarkable effect is 0.1-0.25%.Can significantly improve the coercive force in the magnet behind same interpolation Al and the Ga, adding the rational weight ratio of excessive not remarkable effect is 0.1 5-0.25%.
The present invention also provides a kind of manufacturing as the arbitrary described method that contains the Nd-Fe-Bo permanent magnet material of yttrium of aforementioned claim, and said method comprises the steps:
(1) with joining raw material, in vaccum sensitive stove, being smelted into thickness under the argon shield is the square square ingot casting of 1～50mm, prevents that magnet material is oxidized, and forms rational institutional framework.
(2) handle in hydrogen broken furnace, inhaling hydrogen after the coarse crushing of square ingot casting; And then 55-600 ℃ carried out dehydrogenation and handle; Carry out mixing the first time powder after the cooling, add the grinding aid (Ma'an Mountain nine and Chemical Industry Science Co., Ltd make) that accounts for raw material weight percentage 0.3-0.5% before mixing powder, mix powder half an hour; Inhaling the hydrogen process carries out on the crystal boundary of rich neodymium phase; The process of inhaling hydrogen is accompanied by the release of heat. and the absorption hydrogen after the heating not only carries out along rich neodymium phase crystal boundary; And can in its lattice, carry out. the product principal phase is NdH2.9 and α-Fe behind the absorption hydrogen; The Fe2B and the Fe2Nd that also have trace, the release that the process of suction hydrogen is accompanied by big calorimetric can obtain high-quality hydride, and carries out dehydrogenation at 55-600 ℃ and handle to prevent to destroy its structure.
(3) powder with completing steps 2 adds air-flow abrasive dust in the air-flow grinding machine; The control powder mean particle sizes adds in the mixed powder jar then and adds the lubricant (Ma'an Mountain nine and Chemical Industry Science Co., Ltd make) that accounts for raw material weight percentage 0.3-1% and carry out mixed powder 1.5-3 hour of the second time between 3-5 μ m;
(4) adopt Magnetic field press to be pressed into square in the powder of completing steps 3 and wait static pressure; Hydrostatic pressure is 150-200MP; In vacuum sintering furnace, carry out sintering and Ageing Treatment then, technological parameter be 1000-1200 ℃ of following 4-5 hour then 800-1000 ℃ following 3-4 hour then 400-650 ℃ following 4-5 hour; This step through in the vacuum sintering furnace by the height sintering tempering of three times on earth, improve contact between powder, optimize structure and obtain high-quality permanent magnet.
(5) final magnetic property measuring instrument carries out Performance Detection.
The present invention improves expensive neodymium element, the reduction manufacturing cost of having substituted as much as possible of coercitive while of magnet through compound being added on of Y and Gd.Particularly the compound interpolation of Y and the Gd density that reduced magnet has been improved the processing characteristics of NdFeB material.The manufacturing approach of NdFeB material provided by the invention can sintering goes out the Nd-Fe-B permanent magnet of high-quality.
Embodiment
Embodiment 1
A kind of Nd-Fe-Bo permanent magnet material that contains yttrium, by being described in table 1 below proportioning raw materials according to the following steps manufacturing:
1 with joining raw material, in vaccum sensitive stove, is smelted into the square ingot casting that thickness is 30mm under the argon shield;
2 with in hydrogen broken furnace, inhaling the hydrogen processing after the coarse crushing of square ingot casting; And then 400 ℃ carried out dehydrogenation and handle; Carry out mixing the first time powder after the cooling, add the grinding aid (Ma'an Mountain nine and Chemical Industry Science Co., Ltd make) that accounts for raw material weight percentage 0.5% before mixing powder, mix powder half an hour;
3 powder with completing steps 2 add air-flow abrasive dust in the air-flow grinding machine; The control powder mean particle sizes is at 5 μ m, add to mix in the powder jar then and adds the lubricant (Ma'an Mountain nine and Chemical Industry Science Co., Ltd make) that accounts for raw material weight percentage 1% and carry out mixed powder 3 hours second time;
4 powder with completing steps 3 adopt Magnetic field press to be pressed into square and wait static pressure; Hydrostatic pressure is 200MP; In vacuum sintering furnace, carry out sintering and Ageing Treatment then, technological parameter be 1200 ℃ following 4 hours then 1000 ℃ following 3 hours then 400 ℃ following 5 hours;
5 final magnetic property measuring instruments carry out Performance Detection.
Table 1
Remanent magnetism and the coercive force of embodiment 1 magnet that can find to have added Y and Gd element through contrast be greater than existing magnet, and density is lower than and has magnet now and be convenient to process, and reduced the use reduction manufacturing cost of neodymium element.
Embodiment 2
A kind of Nd-Fe-Bo permanent magnet material that contains yttrium, by being described in table 2 below proportioning raw materials according to the following steps manufacturing:
1 with joining raw material, in vaccum sensitive stove, is smelted into the square ingot casting that thickness is 25mm under the argon shield;
2 with in hydrogen broken furnace, inhaling the hydrogen processing after the coarse crushing of square ingot casting; And then 55 ℃ carried out dehydrogenation and handle; Carry out mixing the first time powder after the cooling, add the grinding aid (Ma'an Mountain nine and Chemical Industry Science Co., Ltd make) that accounts for raw material weight percentage 0.3% before mixing powder, mix powder half an hour;
3 powder with completing steps 2 add air-flow abrasive dust in the air-flow grinding machine; The control powder mean particle sizes is at 3 μ m, add to mix in the powder jar then and adds the lubricant (Ma'an Mountain nine and Chemical Industry Science Co., Ltd make) that accounts for raw material weight percentage 0.3% and carry out mixed powder 1.5 hours second time;
4 powder with completing steps 3 adopt Magnetic field press to be pressed into square and wait static pressure; Hydrostatic pressure is 150MP; In vacuum sintering furnace, carry out sintering and Ageing Treatment then, technological parameter be 1000 ℃ following 5 hours then 800 ℃ following 4 hours then 650 ℃ following 4 hours;
5 final magnetic property measuring instruments carry out Performance Detection
Table 2
Remanent magnetism and the coercive force of embodiment 2 magnets that can find to have added Y and Gd element through contrast be greater than the existing magnet that adds Y element separately, and density is lower than existing magnet and is convenient to process, and reduced the use reduction manufacturing cost of neodymium element.
Embodiment 3
A kind of Nd-Fe-Bo permanent magnet material that contains yttrium, by being described in table 3 below proportioning raw materials according to the following steps manufacturing:
1 with joining raw material, in vaccum sensitive stove, is smelted into the square ingot casting that thickness is 1mm under the argon shield;
2 with in hydrogen broken furnace, inhaling the hydrogen processing after the coarse crushing of square ingot casting; And then 600 ℃ carried out dehydrogenation and handle; Carry out mixing the first time powder after the cooling, add the grinding aid (Ma'an Mountain nine and Chemical Industry Science Co., Ltd make) that accounts for raw material weight percentage 0.5% before mixing powder, mix powder half an hour;
3 powder with completing steps 2 add air-flow abrasive dust in the air-flow grinding machine; The control powder mean particle sizes is at 5 μ m, add to mix in the powder jar then and adds the lubricant (Ma'an Mountain nine and Chemical Industry Science Co., Ltd make) that accounts for raw material weight percentage 1% and carry out mixed powder 3 hours second time;
4 powder with completing steps 3 adopt Magnetic field press to be pressed into square and wait static pressure; Hydrostatic pressure is 200MP; In vacuum sintering furnace, carry out sintering and Ageing Treatment then, technological parameter be 1100 ℃ following 4.5 hours then 1000 ℃ following 3.5 hours then 500 ℃ following 4.5 hours;
5 final magnetic property measuring instruments carry out Performance Detection.
Table 3
Remanent magnetism and the coercive force of embodiment 3 magnets that can find to have added Y and Gd and Ce element through contrast be greater than the existing magnet that adds Gd separately, and density is lower than existing magnet and is convenient to process, and reduced the use reduction manufacturing cost of neodymium element.
Embodiment 4
A kind of Nd-Fe-Bo permanent magnet material that contains yttrium, by being described in table 4 below proportioning raw materials according to the following steps manufacturing:
1 with joining raw material, in vaccum sensitive stove, is smelted into the square ingot casting that thickness is 50mm under the argon shield;
2 with in hydrogen broken furnace, inhaling the hydrogen processing after the coarse crushing of square ingot casting; And then 5 00 ℃ carried out dehydrogenation and handle; Carry out mixing the first time powder after the cooling, add the grinding aid (Ma'an Mountain nine and Chemical Industry Science Co., Ltd make) that accounts for raw material weight percentage 0.4% before mixing powder, mix powder half an hour;
3 powder with completing steps 2 add air-flow abrasive dust in the air-flow grinding machine; The control powder mean particle sizes is at 4 μ m, add to mix in the powder jar then and adds the lubricant (Ma'an Mountain nine and Chemical Industry Science Co., Ltd make) that accounts for raw material weight percentage 0.5% and carry out mixed powder 3 hours second time;
4 powder with completing steps 3 adopt Magnetic field press to be pressed into square and wait static pressure; Hydrostatic pressure is 200MP; In vacuum sintering furnace, carry out sintering and Ageing Treatment then, technological parameter be 1100 ℃ following 4.5 hours then 900 ℃ following 3.5 hours then 500 ℃ following 4.5 hours;
5 final magnetic property measuring instruments carry out Performance Detection.
Table 4
Remanent magnetism and the coercive force of embodiment 4 magnets that can find to have added Y and Gd and La element through contrast be greater than the existing magnet that adds Y element separately, and density is lower than existing magnet and is convenient to process, and reduced the use reduction manufacturing cost of neodymium element.
Embodiment 5
A kind of Nd-Fe-Bo permanent magnet material that contains yttrium, by being described in table 5 below proportioning raw materials according to the following steps manufacturing:
1 with joining raw material, in vaccum sensitive stove, is smelted into the square ingot casting that thickness is 45mm under the argon shield;
2 with in hydrogen broken furnace, inhaling the hydrogen processing after the coarse crushing of square ingot casting; And then 500 ℃ carried out dehydrogenation and handle; Carry out mixing the first time powder after the cooling, add the grinding aid (Ma'an Mountain nine and Chemical Industry Science Co., Ltd make) that accounts for raw material weight percentage 0.3% before mixing powder, mix powder half an hour;
3 powder with completing steps 2 add air-flow abrasive dust in the air-flow grinding machine; The control powder mean particle sizes is at 4 μ m, add to mix in the powder jar then and adds the lubricant (Ma'an Mountain nine and Chemical Industry Science Co., Ltd make) that accounts for raw material weight percentage 0.5% and carry out mixed powder 3 hours second time;
4 powder with completing steps 3 adopt Magnetic field press to be pressed into square and wait static pressure; Hydrostatic pressure is 200MP; In vacuum sintering furnace, carry out sintering and Ageing Treatment then, technological parameter be 1100 ℃ following 4.5 hours then 1000 ℃ following 3.5 hours then 600 ℃ following 4.5 hours;
5 final magnetic property measuring instruments carry out Performance Detection.
Table 5
Remanent magnetism and the coercive force of embodiment 5 magnets that can find to have added Y and Gd element through contrast be greater than existing magnet, and density is lower than and has magnet now and be convenient to process, and reduced the use reduction manufacturing cost of neodymium element.
Embodiment 6
A kind of Nd-Fe-Bo permanent magnet material that contains yttrium, by being described in table 6 below proportioning raw materials according to the following steps manufacturing:
1 with joining raw material, in vaccum sensitive stove, is smelted into the square ingot casting that thickness is 25mm under the argon shield;
2 with in hydrogen broken furnace, inhaling the hydrogen processing after the coarse crushing of square ingot casting; And then 500 ℃ carried out dehydrogenation and handle; Carry out mixing the first time powder after the cooling, add the grinding aid (Ma'an Mountain nine and Chemical Industry Science Co., Ltd make) that accounts for raw material weight percentage 0.3% before mixing powder, mix powder half an hour;
3 powder with completing steps 2 add air-flow abrasive dust in the air-flow grinding machine; The control powder mean particle sizes is at 4 μ m, add to mix in the powder jar then and adds the lubricant (Ma'an Mountain nine and Chemical Industry Science Co., Ltd make) that accounts for raw material weight percentage 0.5% and carry out mixed powder 3 hours second time;
4 powder with completing steps 3 adopt Magnetic field press to be pressed into square and wait static pressure; Hydrostatic pressure is 150MP; In vacuum sintering furnace, carry out sintering and Ageing Treatment then, technological parameter be 1100 ℃ following 4.5 hours then 1000 ℃ following 3.5 hours then 600 ℃ following 4.5 hours;
5 final magnetic property measuring instruments carry out Performance Detection.
Table 6
Remanent magnetism and the coercive force of embodiment 6 magnets that can find to have added Y and Gd element through contrast be greater than existing magnet, and density is lower than and has magnet now and be convenient to process, and reduced the use reduction manufacturing cost of neodymium element.
The foregoing description 1-6 only the explanation the present invention point out pass through Y and Gd be used in combination the maintenance NdFeB permanent magnetic material performance prerequisite under; More substituted present expensive Nd to reduce manufacturing cost; Reducing the Nd-Fe-Bo permanent magnet material difficulty of processing simultaneously, is not the qualification to the scope of the invention.The employed interpolation element of embodiment of the invention 1-6 has mainly played and has improved coercitive effect.
Claims (6)
1. Nd-Fe-Bo permanent magnet material that contains yttrium, it is characterized in that: it consists of: Re
αY
δGd
βB
ξCu
εN
νFe
100-alpha-beta-δ-ξ-ε-ν,
Re is at least a element or more than one element among Nd or Nd and Pr, Ho, Tb, La, Ce, the Dy;
N comprises one or more elements of Al, Mn, Ti, Ni, Zn, Ga, Cr and Mo for adding element;
α, β, δ, ε, ν, ξ are the weight percent content of each element;
Fe is Fe and unavoidable impurities;
Wherein, 28≤alpha+beta+δ≤33,1≤δ≤10,0.5＜β≤5,1≤ξ≤1.2,0.03≤ε≤0.25,0＜ν≤0.25.
2. the Nd-Fe-Bo permanent magnet material that contains yttrium as claimed in claim 1 is characterized in that: described δ value is 4≤δ≤8.
3. the Nd-Fe-Bo permanent magnet material that contains yttrium as claimed in claim 1 is characterized in that: described β value is 1≤β≤3.
4. the Nd-Fe-Bo permanent magnet material that contains yttrium as claimed in claim 1 is characterized in that: described Re comprises Nd and Ce; Or Nd and La.
5. the Nd-Fe-Bo permanent magnet material that contains yttrium as claimed in claim 1 is characterized in that: described N comprises Al; Or Al and Ga.
6. the arbitrary described method that contains the Nd-Fe-Bo permanent magnet material of yttrium of a manufacturing such as aforementioned claim, said method comprises the steps:
(1), in vaccum sensitive stove, is smelted into the square ingot casting that thickness is 1～50mm under the argon shield with joining raw material;
(2) handle in hydrogen broken furnace, inhaling hydrogen after the coarse crushing of square ingot casting, and then 55-600 ℃ carried out dehydrogenation and handle, carry out after the cooling mixing powder first time, add the grinding aid that accounts for raw material weight percentage 0.3-0.5% before mixing powder, mixed powder half an hour;
(3) powder with completing steps 2 adds air-flow abrasive dust in the air-flow grinding machine, controls powder mean particle sizes between 3-5 μ m, adds then to mix in the powder jar and add the lubricant that accounts for raw material weight percentage 0.3-1% to carry out mixed powder 1.5-3 hour of the second time;
(4) adopt Magnetic field press to be pressed into square in the powder of completing steps 3 and wait static pressure; Hydrostatic pressure is 150-200MP; In vacuum sintering furnace, carry out sintering and Ageing Treatment then, technological parameter be 1000-1200 ℃ of following 4-5 hour then 800-1000 ℃ following 3-4 hour then 400-650 ℃ following 4-5 hour;
(5) final magnetic property measuring instrument carries out Performance Detection.
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| CN104272403A (en) * | 2013-03-22 | 2015-01-07 | Tdk株式会社 | R-t-b-type permanent magnet |
| CN105895289A (en) * | 2016-06-28 | 2016-08-24 | 无锡新大力电机有限公司 | Permanent magnet material for manufacturing permanent magnet motor |
| CN105931783A (en) * | 2016-06-27 | 2016-09-07 | 无锡新大力电机有限公司 | Preparation method for gadolinium-doped permanent magnet material |
| CN109346259A (en) * | 2018-09-08 | 2019-02-15 | 江西理工大学 | A kind of Cutting free sintered permanent magnet and preparation method thereof containing Y |
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| CN109346259A (en) * | 2018-09-08 | 2019-02-15 | 江西理工大学 | A kind of Cutting free sintered permanent magnet and preparation method thereof containing Y |
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| CN113223800A (en) * | 2021-04-28 | 2021-08-06 | 慈溪市兴发磁业科技有限公司 | Low-cost neodymium iron boron permanent magnet and preparation method thereof |
| CN113921263A (en) * | 2021-11-10 | 2022-01-11 | 赣州市钜磁科技有限公司 | Preparation method of sintered neodymium-iron-boron permanent magnet material containing lanthanum and yttrium |
| CN117542641A (en) * | 2023-11-08 | 2024-02-09 | 江苏普隆磁电有限公司 | Preparation method of heat-resistant NdFeB magnet |
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Application publication date: 20120222 |