CN101240392A - Rare earth alloy - Google Patents
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- CN101240392A CN101240392A CN 200710063646 CN200710063646A CN101240392A CN 101240392 A CN101240392 A CN 101240392A CN 200710063646 CN200710063646 CN 200710063646 CN 200710063646 A CN200710063646 A CN 200710063646A CN 101240392 A CN101240392 A CN 101240392A
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Abstract
The invention relates to a rare-earth additive alloy for producing magnetic material. The composition formula can be represent as R1R2M, the alloy includes 0.5wt%<=R1<=30wt%, 0wt%<=R2<=99.0wt% and residue M, the R1 represents at least one element selected from Tb and Dy, R2 represents at least one element selected from La, Ce, Pr, Nd, Y, Sc, Sm, Eu, Gd, Ho, Er, Tm, Yb and Lu, M represents one or more transition metal selected from Fe, Co, Cu, Zr, Ga, Al, Mn, Ni, Cr, Zn, Ge, Sem, Mo, V, Ti, In, Sn, Sb, Pb and Hf. Compared with rare-earth permanent-magnet material added with single metal, the rare-earth permanent-magnet material prepared with the additive alloy has advantages of low melting point, precise composition control, uniform elements dispersion and high magnet performance.
Description
Technical field
The present invention relates to a kind of rare earth interpolation alloy that is used to make new function material, particularly relate to Nd-Fe-B series permanent magnetic material with fine magnetic property.
Background technology
Rare earth is made various new function materials because high-performances such as its unique magnetic, light, electricity are widely used in, and is the basic raw material of preparation rare earth functional materials.For example:, in preparation process, need to add rare earth metals such as Nd, Pr, to obtain higher magnet coercive force and good temperature profile at the NdFeB permanent magnet material of rare earth permanent-magnetic material in occupation of extremely important position.Traditional NdFeB magnet directly adds above-mentioned single heavy rare earth metal in preparation process.And preparation technology's long flow path of single rare earth metal, the metal yield is low, the market value height, therefore, along with the aggravation of market competition, the mixed gradually rare earth alloy of single rare earth metal replaces in recent years, and each big rare earth permanent magnet producer generally adopts the Pr-Nd alloy, binary alloys such as Dy-Fe alloy replace the single rare earth metal, to reduce material cost.In order to prepare high performance NdFeB permanent magnet material, also often need to add Cu, Zr, magnesium-yttrium-transition metals such as Co, Al.But the above rare earth alloy of the ternary of the transiting group metal elements that contains at present is actually rare, and magnesium-yttrium-transition metal such as Cu, Zr, Co, Al etc. must realize by the mode of adding single metal.Facts have proved, directly the single magnesium-yttrium-transition metal of interpolation causes very big influence to the composition uniformity coefficient of NdFeB mother alloy, this is because when melting NdFeB mother alloy, generally be that refining is 5～10 minutes again after refractory metal such as Fe fusing finishes, in the so short time, multiple element, it is very difficult that general 7～10 kinds of elements mix, and certainly will cause the NdFeB mother alloy to have component segregation, is unfavorable for preparing high-quality rare earth permanent-magnetic material.If raw material is a multicomponent alloy before the melting, as the PrNdDyFeCu alloy, this alloy not only fusing point is low, and each unit have certain mixedness, and therefore the mother alloy component segregation of preparing is few.
The homogeneity of mother alloy composition to the performance of Nd-Fe-B series permanent magnetic material particularly coercive force play an important role, according to research, the desirable microstructure of high performance Nd-Fe-B series permanent magnetic material is: (1) Nd
2Fe
14B crystal grain is surrounded by the rich Nd phase thin layer of the about 2nm of a layer thickness, and crystal grain and intergranule are isolated each other, makes not have the magnetic exchange coupling between them; (2) Nd
2Fe
14The chemical ingredients of B crystal grain is consistent with even structure.Nd
2Fe
14The about 5.2nm of B crystalline domain wall thickness.If in the scope of 3～5 atomic shells, have composition and structural inhomogeneity, will make the magnetocrystalline anisotropy constant K in inhomogeneous district
1Reduce, just may become the nucleating center on reversal magnetization farmland, under lower reversal magnetization field action, form the reversal magnetization farmland, thereby cause the reversal magnetization of whole crystal grain, the coercive force of magnet is reduced; (3) ideal border structure the rich Nd phase thin layer of the 2nm that has an appointment, also requires the contacted Nd of thin layer mutually with rich Nd on the border
2Fe
14The inner uniformity of the composition of B grain surface layer, structure and crystal grain.As long as with the rich Nd contacted Nd of thin layer mutually
2Fe
14B grain surface floor has the uneven components district of 5～6nm thickness, will make the magnetocrystalline anisotropy constant K in inhomogeneous district
1Reduce, will become the nucleating center that forms the reversal magnetization farmland, reduce the coercive force of magnet.
According to the above, the small fluctuating of composition may cause changes of microstructure, thereby influences the performance of magnet, facts have proved, can prepare high performance Nd-Fe-B series magnet with alloy of the present invention, especially can improve the coercive force of magnet, can improve 5% at least.Therefore this alloy that contains light rare earths, heavy rare earths and magnesium-yttrium-transition metal has stronger practicality and bright development prospect.
Chinese patent 200510054067.4 discloses a kind of producing Dy-Fe alloy by molten salt electrolysis method technology and equipment thereof, mainly is rare earth alloy process for producing and equipment thereof but it relates to, and the rare earth alloy that relates to is Dy-Fe alloy just also, does not contain light rare earths.Chinese patent 96108301.8 discloses a kind of method of producing the mixed light rare earth alloy, but its alloy does not contain heavy rare earth elements such as Tb, Dy, Ho.
Summary of the invention:
The present invention is directed to the problems referred to above, proposed a kind of alloy that contains light rare earths, heavy rare earths and magnesium-yttrium-transition metal, this alloy especially is adapted to produce the high-performance rare-earth permanent-magnetic material.
1. rare earth alloy, it is characterized in that: composition formula can be represented that wherein the R1 percentage composition is 0.5wt%≤R1≤30wt% by R1R2M, and the R2 percentage composition is 0wt%≤R2≤99.0wt%, surplus is M and inevitable impurity.Described R1 representative is selected from least a element among Tb and the Dy, R2 representative is selected from least a element among La, Ce, Pr, Nd, Y, Sc, Sm, Eu, Gd, Ho, Er, Tm, Yb and the Lu, and M represents one or more among magnesium-yttrium-transition metal Fe, Co, Cu, Zr, Ga, Al, Mn, Ni, Cr, Zn, Ge, Se, Mo, V, Ti, In, Sn, Sb, Pb, the Hf.
2. rare earth alloy according to claim 1 is characterized in that wherein R1, R2 percentage composition are respectively 1wt%≤R1≤20wt%, 30wt%≤R2≤99wt%, and surplus is M and inevitable impurity.
3. rare earth alloy according to claim 2 is characterized in that R1 comprises at least a element among Tb and the Dy, and its percentage composition is 1wt%＜R1≤15wt%, and the R2 percentage composition is 60wt%≤R2≤99wt%, and surplus is M and inevitable impurity.
4. rare earth alloy according to claim 1, this alloy have following main composition: TbR2M, and wherein the percentage composition of Tb is 1wt%＜Tb≤9wt%, and the R2 percentage composition is 70wt%≤R2≤99wt%, and surplus is M and inevitable impurity.
5. rare earth alloy according to claim 1, wherein R2 is at least a element among La, Ce, Pr, Nd, Ho and the Er, M is at least a element among Fe, Co, Cu, Zr, Mn, Ga, Nb, Mo and the Al.
6. rare earth alloy according to claim 6, wherein R2 is an at least a element among Pr and the Nd, at least a element among M Fe, Co, Cu, Zr, Ga and the Al.
7. rare earth alloy according to claim 1 is characterized in that: R1+R2＜30wt% or R1+R2＞60wt%.
8. rare earth alloy according to claim 1 is characterized in that: when M is Al, and R1+R2＜4wt% or R1+R2＞58wt%.
9. according to the described rare earth alloy of claim 1～8, it is characterized in that: the oxygen level of alloy is less than 0.3wt%.
10. according to the described rare earth alloy of claim 1～8, it is characterized in that: the carbon content of alloy is less than 0.05wt%.
11. according to the described rare earth alloy of claim 1～8, it is characterized in that: the nitrogen content of alloy is less than 0.05wt%.
In addition, because rare earth adds the crucial starting material that alloy is the preparation rare earth permanent-magnetic material, the content height of its elemental oxygen, carbon, nitrogen is to the performance important influence of permanent magnet product.The present invention has done clear and definite qualification by a large amount of experimental studies to oxygen, carbon, the nitrogen content scope of the used interpolation alloy of preparation high-performance rare-earth permanent magnet material.
This rare earth alloy not only can obtain mixing the melting casting with smelting furnace, and can obtain by direct electrolysis mixed rare-earth oxide.For example, make negative electrode, directly obtain to contain the PrNdDyFe interpolation alloy of heavy rare earth element Dy by direct electrolytic oxidation praseodymium neodymium and dysprosium oxide with iron staff.Make negative electrode with tungsten bar, directly obtain to contain the PrNdTbZr alloy of heavy rare earth element Tb and magnesium-yttrium-transition metal Zr by direct electrolytic oxidation praseodymium neodymium, terbium sesquioxide and zirconium white.Adopt above-mentioned alloy to prepare rare earth permanent-magnetic material, compare interpolation dysprosium iron or terbium iron alloy and single metal zirconium that present technology generally adopts, not only cost reduces greatly, and in the subsequent process of preparation NdFeB magnet, can obviously reduce smelting temperature, avoid the volatilization of Dy element, make the magnet Composition Control more accurate, even, be convenient to prepare high performance NdFeB magnet.Because this alloy has added transiting group metal elements, form intermetallic compound, so more broken, instant packed than easy with the pure rare-earth metals alloy phase.
Embodiment
Below the invention will be further described with example.Protection domain of the present invention is not subjected to the restriction of these embodiment, and protection domain of the present invention is determined by claims.
The test of embodiment is carried out in the following manner among the present invention:
Metal detection adopts the ICP-MS test according to national standards such as GB/T18115.1-2006;
The detection of C is adopted high-frequency combustion-infrared method test according to GB/T12690.13-1990;
The detection of O is adopted noble gas pulse-infrared method test according to GB/T12690.4-2003;
The detection of N is adopted the test of rare gas element melting heat inducing defecation by enema and suppository according to GB/T20124-2006.
Magnet performance detects according to GB/T 13560-2000 and GB/T 3217-1992, adopts the test of magnet performance tester.
The standard deviation S of chemical ingredients is calculated by following formula: S
2=1/ (n-1) ∑ (Xi-X mean value)
2, wherein Xi is the chemical ingredients of sample, X mean value is the average of the chemical composition of sample n point, n=10 among the present invention.
Embodiment 1
The R1R2M alloy of present embodiment is the NdDyFe alloy, and its alloy preparation method is: with plumbago crucible as reactor, iron staff as the catholyte gained.Ionogen is neodymium fluoride 50wt%, dysprosium fluoride 30wt%, lithium fluoride 20wt%, logical direct current electrolysis, average current intensity 2200A, cathode current density 12A/cm
2, electrolysis temperature maintains 1000～1020 ℃.Adding purity is 99.5% dysprosium oxide Dy in the electrolytic process
2O
31.8 kilogram and purity are 99.5% Neodymium trioxide Nd
2O
33 kilograms, make 5.3 kilograms of NdDyFe alloys.Its main component, oxygen level and other foreign matter content see Table 1-1.
Add the alloy for preparing in the present embodiment to the neodymium iron boron principal constituent, adopt melt-spun → hydrogen fragmentation to prepare Sintered NdFeB magnet with airflow milling powder process → pressing under magnetic field → vacuum sintering technology, and the magnet sample carried out Chemical Composition and magnet performance check and analysis, represent the homogeneity of chemical ingredients with standard deviation.The sampling method of Chemical Composition is: get 10 point analysiss arbitrarily in same magnet.For relatively, use conventional method (promptly adding each element separately) preparation Sintered NdFeB magnet simultaneously, all the other items are all identical with the embodiment scheme.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 1-2 and 1-3 respectively.(remarks: embodiment 2～24 all does similarly to analyze relatively.)
Table 1-1 (wt%)
| Nd | Dy | Fe | O | C | N |
| 45.0 | 30.0 | BAL | 0.050 | 0.020 | 0.005 |
The standard deviation of table 1-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | / | 0.12 | / | 0.13 | 0.20 | 0.01 |
| The tradition method | / | 0.42 | / | 0.30 | 0.35 | 0.03 |
Table 1-3 magnet performance
Embodiment 2
It is the PrDyFe alloy that the R1R2M of present embodiment adds alloy, and its alloy preparation method is: with plumbago crucible as reactor, iron staff as the catholyte gained.Ionogen is praseodymium fluoride 78wt%, dysprosium fluoride 12wt%, lithium fluoride 10wt%, logical direct current electrolysis, average current intensity 2400A, cathode current density 8A/cm
2, electrolysis temperature maintains 1000～1020 ℃.Adding purity is 99.5% dysprosium oxide Dy in the electrolytic process
2O
30.8 kilogram and purity are 99.5% Praseodymium trioxide Pr
6O
113 kilograms, make 4 kilograms of PrDyFe alloys.Its main component, oxygen level and other foreign matter content see Table 2-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 2-2 and 2-3 respectively.
Table 2-1 (wt%)
| Pr | Dy | Fe | O | C | N |
| 60 | 8 | BAL | 0.050 | 0.020 | 0.005 |
The standard deviation of table 2-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | 0.2 | 0.14 | / | 0.14 | 0.21 | 0.01 |
| The tradition method | 0.36 | 0.45 | / | 0.36 | 0.32 | 0.02 |
Table 2-3 magnet performance
Embodiment 3
It is the PrNdDy alloy that the R1R2M of present embodiment adds alloy, and its alloy preparation method is: with plumbago crucible as reactor, tungsten bar as the catholyte gained.Ionogen is praseodymium fluoride neodymium 37wt%, dysprosium fluoride 53wt%, lithium fluoride 10wt%, logical direct current electrolysis, average current intensity 2400A, cathode current density 13A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding purity is 99.5% dysprosium oxide Dy in the electrolytic process
2O
32 kilograms, purity is 1.2 kilograms of 99.5% Praseodymium trioxide neodymiums, makes 3 kilograms of PrNdDy alloys.Its main component, oxygen level and other foreign matter content see Table 3-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 3-2 and 3-3 respectively.
Table 3-1 (wt%)
| Nd | Pr | Dy | O | C | N | Other impurity |
| 59 | 20 | 20 | 0.050 | 0.020 | 0.005 | BAL |
The standard deviation of table 3-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | 0.15 | 0.11 | / | 0.12 | 0.22 | 0.01 |
| The tradition method | 0.24 | 0.43 | / | 0.29 | 0.3 | 0.03 |
Table 3-3 magnet performance
Embodiment 4
It is the PrNdDy alloy that the R1R2M of present embodiment adds alloy, and its alloy preparation method is: with plumbago crucible as reactor, tungsten bar as the catholyte gained.Ionogen is praseodymium fluoride neodymium 77wt%, dysprosium fluoride 13wt%, lithium fluoride 10wt%, logical direct current electrolysis, average current intensity 2400A, cathode current density 13A/cm
2, electrolysis temperature maintains 1000～1020 ℃.Adding purity is 99.5% dysprosium oxide Dy in the electrolytic process
2O
30.5 kilogram, purity are 2.5 kilograms of 99.5% Praseodymium trioxide neodymiums, make 2.8 kilograms of PrNdDy alloys.Its main component, oxygen level and other foreign matter content see Table 4-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 4-2 and 4-3 respectively.
Table 4-1 (wt%)
| Nd | Pr | Dy | O | C | N | Other impurity |
| 65 | 19 | 15 | 0.050 | 0.019 | 0.005 | BAL |
The standard deviation of table 4-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | 0.13 | 0.12 | / | 0.10 | 0.21 | 0.01 |
| The tradition method | 0.32 | 0.35 | / | 0.25 | 0.31 | 0.02 |
Table 4-3 magnet performance
Embodiment 5
It is the PrNdDy alloy that the R1R2M of present embodiment adds alloy, and its alloy preparation method is: with plumbago crucible as reactor, tungsten bar as the catholyte gained.Ionogen is praseodymium fluoride neodymium 82wt%, dysprosium fluoride 8wt%, lithium fluoride 10wt%, logical direct current electrolysis, average current intensity 2200A, cathode current density 15A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding purity is 99.5% dysprosium oxide Dy in the electrolytic process
2O
30.3 kilogram, purity are 2.5 kilograms of 99.5% Praseodymium trioxide neodymiums, make 2.2 kilograms of PrNdDy alloys.Its main component, oxygen level and other foreign matter content see Table 5-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 5-2 and 5-3 respectively.
Table 5-1 (wt%)
| Nd | Pr | Dy | O | C | N | Other impurity |
| 70 | 21 | 8 | 0.050 | 0.020 | 0.0048 | BAL |
The standard deviation of table 5-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | 0.15 | 0.15 | / | 0.13 | 0.24 | 0.01 |
| The tradition method | 0.37 | 0.44 | / | 0.28 | 0.37 | 0.03 |
Table 5-3 magnet performance
Embodiment 6
It is the PrNdTb alloy that the R1R2M of present embodiment adds alloy, and its alloy preparation method is: get rid of plumbago crucible as reactor, tungsten bar as the catholyte gained.Ionogen is praseodymium fluoride neodymium 85wt%, fluoridizes terbium 5wt%, lithium fluoride 10wt%, leads to direct current electrolysis, average current intensity 2200A, cathode current density 15A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding purity is 99.5% terbium sesquioxide Tb in the electrolytic process
4O
70.2 kilogram, purity are 2.8 kilograms of 99.5% Praseodymium trioxide neodymiums, make 2.2 kilograms of PrNdTb alloys.Its main component, oxygen level and other foreign matter content see Table 6-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 6-2 and 6-3 respectively.
Table 6-1 (wt%)
| Nd | Pr | Tb | O | C | N | Other impurity |
| 74 | 20 | 5 | 0.050 | 0.019 | 0.004 | BAL |
The standard deviation of table 6-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | 0.15 | 0.12 | 0.11 | / | 0.18 | 0.01 |
| The tradition method | 0.44 | 0.34 | 0.26 | / | 0.25 | 0.02 |
Table 6-3 magnet performance
Embodiment 7
It is the PrNdTb alloy that the R1R2M of present embodiment adds alloy, and its alloy preparation method is: with plumbago crucible as reactor, tungsten bar as the catholyte gained.Ionogen is praseodymium fluoride neodymium 87wt%, fluoridizes terbium 3wt%, lithium fluoride 10wt%, leads to direct current electrolysis, average current intensity 2200A, cathode current density 15A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding purity is 99.5% terbium sesquioxide Tb in the electrolytic process
4O
70.02 kilogram, purity are 3.4 kilograms of 99.5% Praseodymium trioxide neodymiums, make 3 kilograms of PrNdTb alloys.Its main component, oxygen level and other foreign matter content see Table 7-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 7-2 and 7-3 respectively.
Table 7-1 (wt%)
| Nd | Pr | Tb | O | C | N | Other impurity |
| 65 | 33.5 | 0.5 | 0.050 | 0.020 | 0.005 | BAL |
The standard deviation of table 7-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | 0.16 | 0.11 | 0.12 | / | 0.24 | 0.01 |
| The tradition method | 0.27 | 0.43 | 0.33 | / | 0.36 | 0.03 |
Table 7-3 magnet performance
Embodiment 8
It is the NdTbDy alloy that the R1R2M of present embodiment adds alloy, and its alloy preparation method is: with plumbago crucible as reactor, tungsten bar as the catholyte gained.Ionogen is neodymium fluoride 70wt%, fluoridizes terbium 10wt%, dysprosium fluoride 10wt%, lithium fluoride 10wt%, leads to direct current electrolysis, average current intensity 2200A, cathode current density 15A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding purity is 99.5% Neodymium trioxide Nd in the electrolytic process
2O
33.8 kilogram, purity is 99.5% terbium sesquioxide Tb
4O
70.75 kilogram, purity is 99.5% dysprosium oxide Dy
2O
3025 kilogram, make 4 kilograms of NdTbDy alloys.Its main component, oxygen level and other foreign matter content see Table 8-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 8-2 and 8-3 respectively.
Table 8-1 (wt%)
| Nd | Tb | Dy | O | C | N | Other impurity |
| 79 | 15 | 5 | 0.048 | 0.020 | 0.004 | BAL |
The standard deviation of table 8-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | / | 0.13 | 0.21 | 0.12 | 0.25 | 0.01 |
| The tradition method | / | 0.35 | 0.44 | 0.28 | 0.35 | 0.02 |
Table 8-3 magnet performance
Embodiment 9
It is the PrNdTbDy alloy that the R1R2M of present embodiment adds alloy, and its alloy preparation method is: with plumbago crucible as reactor, tungsten bar as the catholyte gained.Ionogen is praseodymium fluoride neodymium 84wt%, fluoridizes terbium 3wt%, dysprosium fluoride 3wt%, lithium fluoride 10wt%, leads to direct current electrolysis, average current intensity 2200A, cathode current density 15A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding purity is 99.5% terbium sesquioxide Tb in the electrolytic process
4O
70.02 kilogram, purity is 99.5% dysprosium oxide Dy
2O
30.02 kilogram, purity are 3.45 kilograms of 99.5% Praseodymium trioxide neodymiums, make 3 kilograms of PrNdTbDy alloys.Its main component, oxygen level and other foreign matter content see Table 9-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 9-2 and 9-3 respectively.
Table 9-1 (wt%)
| Nd | Pr | Tb | Dy | O | C | N | Other impurity |
| 65 | 33 | 0.5 | 0.5 | 0.050 | 0.019 | 0.004 | BAL |
The standard deviation of table 9-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | 0.21 | 0.11 | 0.01 | 0.01 | 0.22 | 0.01 |
| The tradition method | 0.46 | 0.43 | 0.03 | 0.03 | 0.38 | 0.03 |
Table 9-3 magnet performance
Embodiment 10
It is the NdTbFe alloy that the R1R2M of present embodiment adds alloy, and its preparation method is: with plumbago crucible as reactor, iron staff as the catholyte gained.Ionogen is neodymium fluoride 89wt%, fluoridizes terbium 1wt%, lithium fluoride 10wt%, leads to direct current electrolysis, average current intensity 2400A, cathode current density 10A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding in the electrolytic process purity is that 99.5% terbium sesquioxide Tb4O70.03 kilogram and purity are 99.5% Neodymium trioxide Nd2O33.1 kilogram, makes 3.3 kilograms of NdTbFe alloys.Its main component, oxygen level and other foreign matter content see Table 10-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 10-2 and 10-3 respectively.
Table 10-1 (wt%)
| Nd | Tb | Fe | O | C | N |
| 97.0 | 1.0 | BAL | 0.045 | 0.018 | 0.003 |
The standard deviation of table 10-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | / | 0.15 | 0.02 | / | 0.26 | 0.01 |
| The tradition method | / | 0.45 | 0.04 | / | 0.39 | 0.02 |
Table 10-3 magnet performance
Embodiment 11
It is the PrNdDyFe alloy that the R1R2M of present embodiment adds alloy, and its preparation method is: with plumbago crucible as reactor, iron staff as the catholyte gained.Ionogen is praseodymium fluoride neodymium 80wt%, lithium fluoride 20wt%, logical direct current electrolysis, average current intensity 2400A, cathode current density 10A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding is 99.5% dysprosium oxide Dy with purity in the electrolytic process
2O
30.7 kilogram, purity are 3 kilograms of 99.5% praseodymium fluoride neodymiums, make 2.8 kilograms of PrNdDyFe alloys.Its main component, oxygen level and other foreign matter content see Table 11-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 11-2 and 11-3 respectively.
Table 11-1 (wt%)
| Pr | Nd | Dy | Fe | O | C | N |
| 20.0 | 35.0 | 20.0 | BAL | 0.050 | 0.020 | 0.005 |
The standard deviation of table 11-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | / | 0.11 | / | 0.15 | 0.2 | 0.01 |
| The tradition method | / | 0.43 | / | 0.32 | 0.35 | 0.03 |
Table 11-3 magnet performance
Embodiment 12
It is the PrNdDyFe alloy that the R1R2M of present embodiment adds alloy, and its preparation method is: with plumbago crucible as reactor, iron staff as the catholyte gained.Ionogen is praseodymium fluoride neodymium 80wt%, lithium fluoride 20wt%, logical direct current electrolysis, average current intensity 2400A, cathode current density 10A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding is 99.5% dysprosium oxide Dy with purity in the electrolytic process
2O
30.78 kilogram, purity are 4.1 kilograms of 99.5% Praseodymium trioxide neodymiums, make 4.5 kilograms of PrNdDyFe alloys.Its main component, oxygen level and other foreign matter content see Table 12-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 12-2 and 12-3 respectively.
Table 12-1 (wt%)
| Pr | Nd | Dy | Fe | O | C | N |
| 17 | 53 | 15.0 | BAL | 0.07 | 0.019 | 0.004 |
The standard deviation of table 12-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | 0.17 | 0.15 | / | 0.16 | 0.22 | 0.01 |
| The tradition method | 0.33 | 0.46 | / | 0.27 | 0.33 | 0.03 |
Table 12-3 magnet performance
Embodiment 13
It is the PrNdDyFe alloy that the R1R2M of present embodiment adds alloy, and its preparation method is: with plumbago crucible as reactor, iron staff as the catholyte gained.Ionogen is praseodymium fluoride neodymium 80wt%, lithium fluoride 20wt%, logical direct current electrolysis, average current intensity 2400A, cathode current density 10A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding is 99.5% dysprosium oxide Dy with purity in the electrolytic process
2O
30.23 kilogram, purity is 99.5% Praseodymium trioxide neodymium Pr
6O
113.3 kilogram makes 3.8 kilograms of PrNdDyFe alloys.Its main component, oxygen level and other foreign matter content see Table 13-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 13-2 and 13-3 respectively.
Table 13-1 (wt%)
| Pr | Nd | Dy | Fe | O | C | N |
| 17.5 | 52.5 | 5.0 | BAL | 0.055 | 0.019 | 0.004 |
The standard deviation of table 13-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | 0.23 | 0.11 | / | 0.16 | 0.24 | 0.01 |
| The tradition method | 0.45 | 0.43 | / | 0.35 | 0.35 | 0.03 |
Table 13-3 magnet performance
Embodiment 14
It is the PrNdTbFe alloy that the R1R2M of present embodiment adds alloy, and its preparation method is: with plumbago crucible as reactor, iron staff as the catholyte gained.Ionogen is praseodymium fluoride neodymium 80wt%, lithium fluoride 20wt%, logical direct current electrolysis, average current intensity 2400A, cathode current density 10A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding is 99.5% terbium sesquioxide Tb with purity in the electrolytic process
4O
70.27 kilogram, purity are 4.15 kilograms of 99.5% Praseodymium trioxide neodymiums, make 4.5 kilograms of PrNdTbFe alloys.Its main component, oxygen level and other foreign matter content see Table 14-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 14-2 and 14-3 respectively.
Table 14-1 (wt%)
| Pr | Nd | Tb | Fe | O | C | N |
| 18.5 | 56.5 | 5.0 | BAL | 0.048 | 0.019 | 0.004 |
The standard deviation of table 14-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | 0.18 | 0.12 | 0.11 | / | 0.26 | 0.01 |
| The tradition method | 0.32 | 0.43 | 0.32 | / | 0.33 | 0.02 |
Table 14-3 magnet performance
Embodiment 15
It is the DyFe alloy that the R1R2M of present embodiment adds alloy, and its preparation method is: with plumbago crucible as reactor, iron staff as the catholyte gained.Ionogen is dysprosium fluoride 85wt%, lithium fluoride 15wt%, logical direct current electrolysis, average current intensity 2400A, cathode current density 10A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding is 99.5% dysprosium oxide Dy with purity in the electrolytic process
2O
30.8 kilogram makes 4.2 kilograms of DyFe alloys.Its main component, oxygen level and other foreign matter content see Table 15-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 15-2 and 15-3 respectively.
Table 15-1 (wt%)
| Dy | Fe | O | C | N |
| 14.0 | BAL | 0.048 | 0.019 | 0.004 |
The standard deviation of table 15-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | / | 0.16 | / | 0.13 | 0.24 | 0.01 |
| The tradition method | / | 0.47 | / | 0.32 | 0.37 | 0.03 |
Table 15-3 magnet performance
Embodiment 16
It is the DyFe alloy that the R1R2M of present embodiment adds alloy, and its preparation method is: with plumbago crucible as reactor, iron staff as the catholyte gained.Ionogen is dysprosium fluoride 80wt%, lithium fluoride 20wt%, logical direct current electrolysis, average current intensity 2400A, cathode current density 10A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding is 99.5% dysprosium oxide Dy with purity in the electrolytic process
2O
30.4 kilogram makes 4.0 kilograms of DyFe alloys.Its main component, oxygen level and other foreign matter content see Table 16-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 16-2 and 16-3 respectively.
Table 16-1 (wt%)
| Dy | Fe | O | C | N |
| 8.0 | BAL | 0.02 | 0.019 | 0.004 |
The standard deviation of table 16-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | / | 0.15 | / | 0.15 | 0.22 | 0.01 |
| The tradition method | / | 0.36 | / | 0.26 | 0.39 | 0.02 |
Table 16-3 magnet performance
Embodiment 17
It is the TbFe alloy that the R1R2M of present embodiment adds alloy, and its preparation method is: with plumbago crucible as reactor, iron staff as the catholyte gained.Ionogen is for fluoridizing terbium 80wt%, lithium fluoride 20wt%, logical direct current electrolysis, average current intensity 2400A, cathode current density 10A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding is 99.5% terbium sesquioxide Tb with purity in the electrolytic process
4O
70.24 kilogram makes 3.8 kilograms of TbFe alloys.Its main component, oxygen level and other foreign matter content see Table 17-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 17-2 and 17-3 respectively.
Table 17-1 (wt%)
| Tb | Fe | O | C | N |
| 5.0 | BAL | 0.018 | 0.02 | 0.004 |
The standard deviation of table 17-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | / | 0.13 | 0.15 | / | 0.24 | 0.01 |
| The tradition method | / | 0.43 | 0.26 | / | 0.35 | 0.03 |
Table 17-3 magnet performance
Embodiment 18
It is the TbFe alloy that the R1R2M of present embodiment adds alloy, and its preparation method is: with plumbago crucible as reactor, iron staff as the catholyte gained.Ionogen is for fluoridizing terbium 82wt%, lithium fluoride 18wt%, logical direct current electrolysis, average current intensity 2400A, cathode current density 10A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding is 99.5% terbium sesquioxide Tb with purity in the electrolytic process
4O
70.2 kilogram makes 4.2 kilograms of TbFe alloys.Its main component, oxygen level and other foreign matter content see Table 18-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 18-2 and 18-3 respectively.
Table 18-1 (wt%)
| Tb | Fe | O | C | N |
| 3.0 | BAL | 0.012 | 0.019 | 0.004 |
The standard deviation of table 18-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | / | 0.17 | 0.15 | / | 0.21 | 0.01 |
| The tradition method | / | 0.38 | 0.33 | / | 0.35 | 0.03 |
Table 18-3 magnet performance
Embodiment 19
It is the TbDyFe alloy that the R1R2M of present embodiment adds alloy, and its preparation method is: with plumbago crucible as reactor, iron staff as the catholyte gained.Ionogen is for fluoridizing terbium 40wt%, dysprosium fluoride 40wt%, lithium fluoride 20wt%, logical direct current electrolysis, average current intensity 2400A, cathode current density 10A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding is 99.5% terbium sesquioxide Tb with purity in the electrolytic process
4O
70.75 kilogram, purity are 0.7 kilogram of 99.5% dysprosium oxide, make 4 kilograms of TbDyFe alloys.Its main component, oxygen level and other foreign matter content see Table 19-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 19-2 and 19-3 respectively.
Table 19-1 (wt%)
| Tb | Dy | Fe | O | C | N |
| 15 | 14 | BAL | 0.023 | 0.018 | 0.004 |
The standard deviation of table 19-2 magnet composition
| Project | Pr | Nd | Tb | Dy | Fe | B |
| Add this alloy | / | 0.13 | 0.14 | 0.18 | 0.25 | 0.01 |
| The tradition method | / | 0.36 | 0.26 | 0.42 | 0.35 | 0.02 |
Table 19-3 magnet performance
Embodiment 20
It is the NdDyFeCu alloy that the R1R2M of present embodiment adds alloy, and its preparation method is: with plumbago crucible as reactor, iron staff as the catholyte gained.Ionogen is praseodymium fluoride 40wt%, dysprosium fluoride 40wt%, lithium fluoride 20wt%, logical direct current electrolysis, average current intensity 2400A, cathode current density 10A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding purity in the electrolytic process is 1.55 kilograms of 99.5% Neodymium trioxide, and purity is 1.1 kilograms of 99.5% dysprosium oxides, and purity is 0.07 kilogram of 99.5% cupric oxide, makes 3 kilograms of TbDyFeCu alloys.Its main component, oxygen level and other foreign matter content see Table 20-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 20-2 and 20-3 respectively.
Table 20-1 (wt%)
| Nd | Dy | Cu | Fe | O | C | N |
| 44 | 29.5 | 2.0 | BAL | 0.035 | 0.019 | 0.005 |
The standard deviation of table 20-2 magnet composition
| Project | Pr | Nd | Cu | Dy | Fe | B |
| Add this alloy | / | 0.21 | 0.01 | 0.11 | 0.23 | 0.01 |
| The tradition method | / | 0.48 | 0.03 | 0.23 | 0.36 | 0.03 |
Table 20-3 magnet performance
Embodiment 21
It is the PrNdDyZr alloy that the R1R2M of present embodiment adds alloy, and its preparation method is: with plumbago crucible as reactor, tungsten bar as the catholyte gained.Ionogen is praseodymium fluoride neodymium 80wt%, dysprosium fluoride 10wt% lithium fluoride 10wt%, logical direct current electrolysis, average current intensity 2400A, cathode current density 10A/cm
2, electrolysis temperature maintains 1000～1020 ℃.About 1 hour of every stove electrolysis, adding purity in the electrolytic process is 0.62 kilogram of 99.5% dysprosium oxide, and purity is 4.15 kilograms of 99.5% Praseodymium trioxide neodymiums, and purity is 0.42 kilogram of 99.5% zirconium white, makes 4.5 kilograms of PrNdDyZr alloys.Its main component, oxygen level and other foreign matter content see Table 21-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 21-2 and 21-3 respectively
Table 21-1 (wt%)
| Pr | Nd | Dy | Zr | O | C | N |
| 60 | 20 | 12 | BAL | 0.048 | 0.019 | 0.003 |
The standard deviation of table 21-2 magnet composition
| Project | Pr | Nd | Zr | Dy | Fe | B |
| Add this alloy | 0.18 | 0.11 | 0.12 | 0.15 | 0.21 | 0.01 |
| The tradition method | 0.44 | 0.43 | 0.32 | 0.34 | 0.35 | 0.02 |
Table 21-3 magnet performance
Embodiment 22
It is the PrNdDyAl alloy that the R1R2M of present embodiment adds alloy, and its preparation method is similar to embodiment 21.Its main component, oxygen level and other foreign matter content see Table 22-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 22-2 and 22-3 respectively
Table 22-1 (wt%)
| Pr | Nd | Dy | Al | O | C | N |
| 60 | 20 | 5 | BAL | 0.048 | 0.02 | 0.004 |
The standard deviation of table 22-2 magnet composition
| Project | Pr | Nd | Al | Dy | Fe | B |
| Add this alloy | 0.22 | 0.15 | 0.10 | 0.16 | 0.23 | 0.01 |
| The tradition method | 0.49 | 0.45 | 0.30 | 0.35 | 0.35 | 0.03 |
Table 22-3 magnet performance
Embodiment 23
It is the PrNdTbGa alloy that the R1R2M of present embodiment adds alloy, and its preparation method is similar to embodiment 21.Its main component, oxygen level and other foreign matter content see Table 23-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 23-2 and 23-3 respectively.
Table 23-1 (wt%)
| Pr | Nd | Tb | Ga | O | C | N |
| 60 | 20 | 3 | BAL | 0.040 | 0.019 | 0.003 |
The standard deviation of table 23-2 magnet composition
| Project | Pr | Nd | Tb | Ga | Fe | B |
| Add this alloy | 0.21 | 0.13 | 0.02 | 0.11 | 0.25 | 0.01 |
| The tradition method | 0.46 | 0.41 | 0.05 | 0.33 | 0.37 | 0.03 |
Table 23-3 magnet performance
Embodiment 24
It is the PrNdTbCo alloy that the R1R2M of present embodiment adds alloy, and its preparation method is similar to embodiment 21.Its main component, oxygen level and other foreign matter content see Table 24-1.The Sintered NdFeB magnet of present embodiment with corresponding conventional method preparation compared, comprise the standard deviation and the magnet performance of chemical ingredients, the result sees Table 24-2 and 24-3 respectively.
Table 24-1 (wt%)
| Pr | Nd | Tb | Co | O | C | N |
| 60 | 20 | 5 | BAL | 0.045 | 0.019 | 0.004 |
The standard deviation of table 24-2 magnet composition
| Project | Pr | Nd | Tb | Co | Fe | B |
| Add this alloy | 0.15 | 0.14 | 0.10 | 0.14 | 0.15 | 0.01 |
| The tradition method | 0.35 | 0.32 | 0.20 | 0.26 | 0.36 | 0.03 |
Table 24-3 magnet performance
Claims (11)
1. rare earth alloy, it is characterized in that: composition formula can be represented that wherein the R1 percentage composition is 0.5wt%≤R1≤30wt% by R1R2M, and the R2 percentage composition is 0wt%≤R2≤99.0wt%, surplus is M and inevitable impurity.Described R1 representative is selected from least a element among Tb and the Dy, R2 representative is selected from least a element among La, Ce, Pr, Nd, Y, Sc, Sm, Eu, Gd, Ho, Er, Tm, Yb and the Lu, and M represents one or more among magnesium-yttrium-transition metal Fe, Co, Cu, Zr, Ga, Al, Mn, Ni, Cr, Zn, Ge, Se, Mo, V, Ti, In, Sn, Sb, Pb, the Hf.
2. rare earth alloy according to claim 1 is characterized in that wherein R1, R2 percentage composition are respectively 1wt%≤R1≤20wt%, 30wt%≤R2≤99wt%, and surplus is M and inevitable impurity.
3. rare earth alloy according to claim 2 is characterized in that R1 comprises at least a element among Tb and the Dy, and its percentage composition is 1wt%＜R1≤15wt%, and the R2 percentage composition is 60wt%≤R2≤99wt%, and surplus is M and inevitable impurity.
4. rare earth alloy according to claim 1, this alloy have following main composition: TbR2M, and wherein the percentage composition of Tb is 1wt%＜Tb≤9wt%, and the R2 percentage composition is 70wt%≤R2≤99wt%, and surplus is M and inevitable impurity.
5. rare earth alloy according to claim 1, wherein R2 is at least a element among La, Ce, Pr, Nd, Ho and the Er, M is at least a element among Fe, Co, Cu, Zr, Mn, Ga, Nb, Mo and the Al.
6. rare earth alloy according to claim 6, wherein R2 is an at least a element among Pr and the Nd, at least a element among M Fe, Co, Cu, Zr, Ga and the Al.
7. rare earth alloy according to claim 1 is characterized in that: R1+R2＜30wt% or R1+R2＞60wt%.
8. rare earth alloy according to claim 1 is characterized in that: when M is Al, and R1+R2＜4wt% or R1+R2＞58wt%.
9. according to the described rare earth alloy of claim 1～8, it is characterized in that: the oxygen level of alloy is less than 0.3wt%.
10. according to the described rare earth alloy of claim 1～8, it is characterized in that: the carbon content of alloy is less than 0.05wt%.
11. according to the described rare earth alloy of claim 1～8, it is characterized in that: the nitrogen content of alloy is less than 0.05wt%.
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