CN100559518C - Nd-Fe-Bo permanent magnet material with zirconium to substitute niobium - Google Patents
Nd-Fe-Bo permanent magnet material with zirconium to substitute niobium Download PDFInfo
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Abstract
With the Nd-Fe-Bo permanent magnet material of zirconium to substitute niobium, it is formed proportioning and is (28～35) % praseodymium neodymium alloy, (1～10) % gadolinium, (0.1～0.5) % zirconium, (0.95～1.3) % boron, (0.1～1.5) % aluminium, (0.01～0.3) % copper, all the other are iron and unavoidable impurities, above-mentioned being weight percentage.By adjusting alloying component, add the metallic element zirconium, replace the niobium element in the Nd Fe B alloys.The present invention replaces rare refractory metal niobium with the abundant zirconium of china natural resources, is guaranteeing to reduce the cost of raw material under the situation that magnetic property does not reduce, and the addition of zirconium obviously is less than the addition of niobium, still can obtain the Nd Fe B alloys material of same magnetic property.Reach the technology stability and the magnetic property of comprehensive raising NdFeB alloy, reduce the cost of manufacture of Nd-Fe-B permanent magnet and improve the ratio of performance to price, improve the competitiveness of product in market.
Description
Technical field
The present invention relates to a kind of Nd-Fe-Bo permanent magnet material, particularly use the sintered Nd-Fe-B permanent magnetic material of zirconium to substitute niobium.
Background technology
The rare earth permanent magnet neodymium iron boron is the novel magnetic material that the eighties develops, and it has excellent specific properties such as high remanent magnetism, high energy product, high-coercive force and high performance-price ratio, is the strongest permanent magnet of current magnetic, is described as the magnetic king in the permanent magnetic material.But the magnetic property of ternary Nd Fe B alloys is unsatisfactory, and HCJ is lower, has only about 1/10 of theoretical anisotropy field; Because to the sintering temperature sensitivity, in the sintering process, the crystal grain phenomenon of growing up unusually often appears.Adding alloying element can effectively address the above problem.In Nd Fe B alloys, the interpolation niobium can suppress α-Fe effectively and form mutually, and can obviously improve the HCJ of magnet.
Because nonferrous metal price sharp rises in recent years, the niobium metal price also significantly rises, and causes the neodymium iron boron production cost constantly to rise.Niobium is the high-melting-point rare metal, and nature content is little, and zirconium is wide in distributed in nature, content is big, China's zirconium aboundresources, and the price of zirconium is more much lower than rare metal niobium.For this reason, replace expensive rare metal by the low metal of price, the product that preparation has same magnetic properties reaches and reduces production costs, and improves the purpose of the market competitiveness.If CN1986856A mentions and adds metals such as Nb, Zr, Ti will change its microstructure in neodymium iron boron fast quenching permanent-magnet alloy, make the crystal refining grain size even, the magnet coercive force is improved, temperature stability also improves, but does not see the relevant report that adopts zirconium to substitute niobium to make the sintered NdFeB permanent magnet alloy.
Summary of the invention
The technical problem to be solved in the present invention is by adjusting alloying component, add the metallic element zirconium, replace the niobium element in the Nd Fe B alloys, reach the technology stability and the magnetic property of comprehensive raising NdFeB alloy, improve coercive force, reduce the cost of manufacture of Nd-Fe-B permanent magnet and improve the ratio of performance to price, improve the competitiveness of product in market.
Technical scheme of the present invention is: with the Nd-Fe-Bo permanent magnet material of zirconium to substitute niobium, it forms proportioning, (28～35) % praseodymium neodymium alloy, (1～10) % gadolinium, (0.1～0.5) % zirconium, (0.95～1.3) % boron, (0.1～1.5) % aluminium, (0.01～0.3) % copper, all the other are iron and unavoidable impurities, above-mentioned being weight percentage.
The present invention replaces rare refractory metal niobium with the abundant zirconium of china natural resources, its beneficial effect is to guarantee to reduce the cost of raw material under the situation that magnetic property does not reduce, the price of zirconium is less than 1/2 of ferro-niobium, and the addition of zirconium obviously is less than the addition of niobium, still can obtain the Nd Fe B alloys material of same magnetic property.
Embodiment
Embodiment one:
Batching: according to following proportioning components weight batching, praseodymium neodymium alloy 30.2% weight, gadolinium 2.0% weight, boron element 1.03% weight, aluminium 0.64% weight, zirconium 0.3% weight, copper 0.02% weight, surplus are iron and other impurity, wherein in the praseodymium neodymium alloy, praseodymium accounts for 25% weight, neodymium accounts for 75% weight, boron element adds with the BFe alloy state, and boron content is 19%, and iron content is 81%; The gadolinium element adds with the GdFe alloy state, and gadolinium concentrations is 75%, and iron content is 25%;
With 100 kilograms of Nd Fe B alloyses of melting is example:
Pack in the vaccum sensitive stove by the described raw material metal of last table.
Founding: after in the vaccum sensitive stove of packing into, the air in the vaccum sensitive stove is evacuated to less than 1Pa, begins the melting of heating, when batching is rubescent to stove, close vacuum valve, charge into argon gas, treat that material is molten clear after, refining pours into spindle, and powered-down treats that the spindle temperature is lower than 60 ℃ and comes out of the stove then;
Powder process: the material piece that spindle is crushed to 90～110mm, discharging particle disposal through expecting piece behind jaw crusher and the intermediate crusher becomes below 20 orders, then airflow milling is put in discharging and carried out powder process, powder particles is controlled between 2.7～5.5 μ m, powder is put into batch mixer, add gasoline and carried out batch mixing 30～60 minutes by proportioning;
Moulding: after mixed powder is weighed, put into the mould of moulding press, add magnetic field orientating, compression moulding, green compact are taken out in demagnetization then, vacuumize encapsulation rapidly, packaged blank is put into the isostatic pressing machine 150-200Mpa that pressurizes, the green compact of making are taken out in pressurize after 1～3 minute again;
Sintering: green compact are packed into behind the magazine, put into the vacuum sintering furnace sintering, after sintering 3.5-4.5 under 1080-1115 ℃ the sintering temperature hour, from sintering furnace, take out, promptly make neodymium iron boron magnetic body.
According to above-described processing step, the Zr composition with 0.3% all replaces 1% Nb, other components unchanged, the sintered Nd-Fe-B alloy of making, detection method is with reference to GB/T 3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, and after testing, magnetic property reaches:
Remanent magnetism can Br:12.6KGs
HCJ Hcj:13.5KOe
Magnetic induction coercivity H b:12.1KOe
Magnetic energy product BH (max): 39MGOe
The magnetic property that does not replace the sintered Nd-Fe-B alloy that Nb makes with Zr:
Remanent magnetism can Br:12.4KGs
HCJ Hcj:13.5KOe
Magnetic induction coercivity H b:11.9KOe
Magnetic energy product BH (max): 38.4MGOe
The data of contrast properties test are as can be seen: after using 0.3% zr element to substitute 1% niobium element, the value of above four parameters of magnetic property obtains improving and improves, and as seen, uses the substitute element zirconium, adopt above-mentioned technology to make sintered Nd-Fe-B alloy, reach the purpose of saving cost.
Embodiment two:
Batching: according to following composition weight proportion batching, praseodymium neodymium alloy 31% weight, gadolinium 2.5% weight, boron element 1.02% weight, aluminium 0.64% weight, zirconium 0.1% weight, copper 0.02% weight, surplus are iron and other impurity, wherein in the praseodymium neodymium alloy, praseodymium is 25% weight, and neodymium is 75% weight; Boron element adds with the BFe alloy state, and boron content is 19%, and iron content is 81%; The gadolinium element adds with the GdFe alloy state, and gadolinium concentrations is 75%, and iron content is 25%;
With 100 kilograms of Nd Fe B alloyses of melting is example:
Pack in the vaccum sensitive stove by the described raw material metal of last table;
Founding: after in the vaccum sensitive stove of packing into, the air in the vaccum sensitive stove is evacuated to less than 1Pa, begins the melting of heating, when batching is rubescent to stove, close vacuum valve, charge into argon gas, treat that material is molten clear after, refining pours into spindle, and powered-down treats that the spindle temperature is lower than 60 ℃ and comes out of the stove then;
Powder process: the material piece that spindle is crushed to 90～110mm, discharging particle disposal through expecting piece behind jaw crusher and the intermediate crusher becomes below 20 orders, then airflow milling is put in discharging and carried out powder process, powder particles is controlled between 2.7～5.5 μ m, powder is put into batch mixer, add gasoline and carried out batch mixing 30～60 minutes by proportioning;
Moulding: after mixed powder is weighed, put into the mould of moulding press, add magnetic field orientating, compression moulding, green compact are taken out in demagnetization then, vacuumize encapsulation rapidly, packaged blank is put into the isostatic pressing machine 150～200Mpa that pressurizes, the green compact of making are taken out in pressurize after 1～3 minute again;
Sintering: green compact are packed into behind the magazine, put into the vacuum sintering furnace sintering, from sintering furnace, take out after 3.5～4.5 hours, promptly make neodymium iron boron magnetic body at sintering under 1080～1115 ℃ the sintering temperature.
According to above-described process, the Zr composition with 0.1% all replaces 1% Nb, other components unchanged, make sintered Nd-Fe-B alloy after testing, detection method is with reference to GB/T 3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, and after testing, magnetic property reaches:
Remanent magnetism can Br:12.5KGs
HCJ Hcj:13.3KOe
Magnetic induction coercivity H b:12.1KOe
Magnetic energy product BH (max): 38.5MGOe
The magnetic property that does not replace the sintered Nd-Fe-B alloy that Nb makes with Zr:
Remanent magnetism can Br:12.4KGs
HCJ Hcj:13.6KOe
Magnetic induction coercivity H b:12.0Koe
Magnetic energy product BH (max): 38.4MGOe
The data of contrast properties test are as can be seen: after using 0.1% zr element to substitute the niobium element, the value of above four parameters of magnetic property obtains improving, and as seen, uses the substitute element zirconium, adopt above-mentioned technology to make sintered Nd-Fe-B alloy, reach the purpose of saving cost.
Embodiment three:
Batching: according to following proportioning components weight batching, praseodymium neodymium alloy 30.5% weight, gadolinium 2% weight, boron element 1.02% weight, aluminium 0.64% weight, zirconium 0.5% weight, copper 0.02% weight, surplus are iron and other impurity, wherein in the praseodymium neodymium alloy, praseodymium is 25% weight, neodymium is 75% weight, boron element adds with the BFe alloy state, and boron content is 19%, and iron content is 81%; The gadolinium element adds with the GdFe alloy state, and gadolinium concentrations is 75%, and iron content is 25%;
With 100 kilograms of Nd Fe B alloyses of melting is example:
Pack in the vaccum sensitive stove by the described raw material metal of last table;
Founding: after in the vaccum sensitive stove of packing into, the air in the vaccum sensitive stove is evacuated to less than 1Pa, begins the melting of heating, when batching is rubescent to stove, close vacuum valve, charge into argon gas, treat that material is molten clear after, refining pours into spindle, and powered-down treats that the spindle temperature is lower than 60 ℃ and comes out of the stove then;
Powder process: the material piece that spindle is crushed to 90～110mm, discharging particle disposal through expecting piece behind jaw crusher and the intermediate crusher becomes below 20 orders, then airflow milling is put in discharging and carried out powder process, powder particles is controlled between 2.7～5.5 μ m, powder is put into batch mixer, add gasoline and carried out batch mixing 30～60 minutes by proportioning;
Moulding: after mixed powder is weighed, put into the mould of moulding press, add magnetic field orientating, compression moulding, green compact are taken out in demagnetization then, vacuumize encapsulation rapidly, packaged blank is put into the isostatic pressing machine 150～200Mpa that pressurizes, the green compact of making are taken out in pressurize after 1～3 minute again;
Sintering: green compact are packed into behind the magazine, put into the vacuum sintering furnace sintering, from sintering furnace, take out after 3.5～4.5 hours, promptly make neodymium iron boron magnetic body at sintering under 1080～1115 ℃ the sintering temperature.
According to above-mentioned process, the Zr composition with 0.5% all replaces 1% Nb, and other components unchanged is made sintered Nd-Fe-B alloy after testing, and detection method is with reference to GB/T 3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, and after testing, magnetic property reaches:
Remanent magnetism can Br:12.7KGs
HCJ Hcj:13.5KOe
Magnetic induction coercivity H b:12.5KOe
Magnetic energy product BH (max): 39.5MGOe
The magnetic property that does not replace the sintered Nd-Fe-B alloy that Nb makes with Zr:
Remanent magnetism can Br:12.4KGs
HCJ Hcj:13.4KOe
Magnetic induction coercivity H b:11.9KOe
Magnetic energy product BH (max): 38.5MGOe
The data of contrast properties test are as can be seen: after using 0.5% zr element to substitute the niobium element, and the raising that is significantly improved of the value of above four parameters of magnetic property.As seen, use the substitute element zirconium, making sintered Nd-Fe-B alloy, reach the purpose of saving cost with sampling technology.
Take a broad view of in the foregoing description, effect is the most tangible just to be to use 0.1% zirconium to substitute niobium just can reach to use the magnetic property of 1% niobium.
In a word, by adjusting alloying component, an amount of interpolation zr element replaces the niobium element in the Nd Fe B alloys, can play crystal grain thinning, comprehensively improve the effect of magnet magnetic property, reach the magnetic property that adds Nb, and meet the trade mark requirement that neodymium iron boron magnetic body reached that adds Nb, finally reduced production cost.
Claims (5)
1, uses the Nd-Fe-Bo permanent magnet material of zirconium to substitute niobium, it forms proportioning, (28～35) % praseodymium neodymium alloy, (1～10) % gadolinium, (0.1～0.5) % zirconium, (0.95～1.3) % boron, (0.1～1.5) % aluminium, (0.01～0.3) % copper, all the other are iron and unavoidable impurities, above-mentioned being weight percentage.
2, the Nd-Fe-Bo permanent magnet material with zirconium to substitute niobium according to claim 1, it is characterized in that forming proportioning is, praseodymium neodymium alloy 30.2% weight, gadolinium 2.0% weight, boron element 1.03% weight, aluminium 0.64% weight, zirconium 0.3% weight, copper 0.02% weight, surplus are iron and other impurity.
3, the Nd-Fe-Bo permanent magnet material with zirconium to substitute niobium according to claim 1, it is characterized in that forming proportioning and be praseodymium neodymium alloy 31% weight, gadolinium 2.5% weight, boron element 1.02% weight, aluminium 0.64% weight, zirconium 0.1% weight, copper 0.02% weight, surplus is iron and other impurity.
4, the Nd-Fe-Bo permanent magnet material with zirconium to substitute niobium according to claim 1, it is characterized in that forming proportioning and be praseodymium neodymium alloy 30.5% weight, gadolinium 2% weight, boron element 1.02% weight, aluminium 0.64% weight, zirconium 0.5% weight, copper 0.02% weight, surplus is iron and other impurity.
5, according to each described Nd-Fe-Bo permanent magnet material with zirconium to substitute niobium in the claim 1～4, it is characterized in that gadolinium adds with the GdFe alloy state, wherein gadolinium concentrations is 75% weight, and iron content is 25% weight.
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| CNB2007101645757A CN100559518C (en) | 2007-12-08 | 2007-12-08 | Nd-Fe-Bo permanent magnet material with zirconium to substitute niobium |
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| CNB2007101645757A CN100559518C (en) | 2007-12-08 | 2007-12-08 | Nd-Fe-Bo permanent magnet material with zirconium to substitute niobium |
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| CN102103917B (en) * | 2009-12-22 | 2013-04-17 | 北京有色金属研究总院 | Neodymium iron boron magnet, preparation method and device applying same |
| CN105006327A (en) * | 2015-08-23 | 2015-10-28 | 宁德市星宇科技有限公司 | High-performance Gd containing cast sheet magnet and preparation method thereof |
| CN105070446A (en) * | 2015-08-23 | 2015-11-18 | 宁德市星宇科技有限公司 | High-performance cerium-neodymium-praseodymium cast sheet magnet and preparation method thereof |
| CN111613407B (en) * | 2020-06-03 | 2022-05-03 | 福建省长汀金龙稀土有限公司 | R-T-B series permanent magnet material, raw material composition, preparation method and application thereof |
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Non-Patent Citations (2)
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| 特开JP2000-234151A 2000.08.29 |
| 特开JP3-278406A 1991.12.10 |
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Address after: 315034, No. 1 West Chengxi Road, Ningbo, Zhejiang Patentee after: Ningbo Ketian Magnetic Industry Co.,Ltd. Address before: 315034, No. 1 West Chengxi Road, Ningbo, Zhejiang Patentee before: NINGBO KETIAN MAGNET Co.,Ltd. |
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