CN103794323B - A kind of rare-earth permanent magnet applying high abundance Rare Earth Production and preparation method thereof - Google Patents
A kind of rare-earth permanent magnet applying high abundance Rare Earth Production and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of commercial rare-earth permanent magnet applying high abundance Rare Earth Production and preparation method thereof.Including principal phase and crystal boundary modified phase, described principal phase includes low<i>h</i>A(RE100-aMMa)-Fe-B alloy and height<i>h</i>ANd-Fe-B alloy.The present invention adopts double; two master alloying, controls magnet composition, makes high abundance rare earth form stable 2:14:1 phase, will not decompose all the time in sintering process；Crystal boundary modified phase adds the Cu element that electrode potential is higher, improves the decay resistance of magnet, and crystal boundary modified phase can optimize the microstructure of magnet simultaneously.Double; two master alloying methods are combined by this method with crystal boundary modified technology, the advantage simultaneously having both concurrently, the problem improving magnet corrosion resistance decline and remanent magnetism and the magnetic energy product decline caused by the interpolation of high abundance rare earth, the rare-earth permanent magnet of preparation reaches the application requirement of commercial magnet.
Description
Technical field
The present invention relates to rare-earth permanent-magnet material technical field, particularly relate to a kind of rare-earth permanent magnet applying high abundance Rare Earth Production and preparation method thereof.
Background technology
The explored rare earth resources commercial reserves in the whole world totally 9900 ~ 10000 tons, within 2008, global rare earth volume of metal consumption is 130,000 tons, predicting global rare earth consumption figure in 2015 and be about 21 tons, if rare earth consumption figure 300,000 tons calculating per year, whole world light rare earth metal only can with about 300 years.Moreover along with social development and scientific and technological progress, rare-earth usage increases year by year, whole world rare earth resources consumes too fast and produces " rare earth crisis theory ".China is global rare earth big country, more should focus on the present situation of rare earth resources.Current rare earth resources application occur in that energy imbalance, in light rare earth, praseodymium, neodymium are widely used, and lanthanum, cerium etc. create resource excess, cause lanthanum, the price of cerium is only praseodymium, neodymium about 1/10, how to change the status quo is urgent problem.
For this, Chinese scholars is attempted with the lanthanum of low cost, cerium part replaces Nd and prepares low cost magnet.La2Fe14B、Ce2Fe14The intrinsic magnetic properties of B can far below Nd2Fe14B, the performance adding reduction magnet of lanthanum cerium, therefore major part is only capable of preparing the Sintered NdFeB magnet of the low trade mark.But what the perishable problem occurred in application process thereupon was more serious limits LaCe application in rare earth permanent-magnetic material.Therefore, the LaCe rare-earth permanent magnet prepared is utilized only in magnetic property reaches requirement, more can not to take into account the index of decay resistance.
Based on above several aspects, we provide one can meet magnetic property to meet again resistance to
The method of corrosive nature.
Summary of the invention
The present invention seeks to overcome the deficiencies in the prior art, it is provided that a kind of rare-earth permanent magnet applying high abundance Rare Earth Production and preparation method thereof.
The rare-earth permanent magnet of application high abundance Rare Earth Production includes principal phase and crystal boundary modified phase, and principal phase accounts for the 90% ~ 99.99% of gross mass；Crystal boundary modified phase accounts for the 0.01% ~ 10% of gross mass, and described principal phase includes low HA(RE100-aMMa)-Fe-B alloy and high HANd-Fe-B alloy, low HA(RE100-aMMa)-Fe-B alloy accounts for the 50% ~ 99.99% of principal phase quality, high HANd-Fe-B alloy account for the 0.01% ~ 50% of principal phase quality.
Described low HA(RE100-aMMa)-Fe-B alloying component is (RE100-aMMa)xFe100-x-y-zByTMz, described high HANd-Fe-B alloying component be REx’Fe100-x’-y-zByTMz；Wherein, RE is one or more in other rare earth elements except La, Ce, and MM is one or more in La, Ce, LaCe alloy, LaCePrNd mischmetal；TM is one or more in Cu, Al, Co, Nb, Zr, Ga, Ta, Si, Ti, V, Mo, Mn, Ag, Mg, Zn；Wherein 1≤a≤50,26.7≤x≤31.0,29≤x '≤45,0.9≤y≤1.2,0.1≤z≤3.0.
Described crystal boundary modified coordinating is divided into R100-uTM’uWherein R is one or more in rare earth La, Ce, Pr, Pm, Sm, Eu, Nd, Dy, Gd, Tb, Ho, Er, Tm, Yb, Lu, and TM ' is one or more in Cu, H, O, F, Fe, Ga, Ti, Al, Co, Nb, Zr, Ta, Si, V, Mo, Mn, Ag, Mg, Zn；0 < u < 100.
Specifically comprising the following steps that of the preparation method of the rare-earth permanent magnet of application high abundance Rare Earth Production
1) according to low HA(RE100-aMMa)-Fe-B alloy and high HAThe composition of Nd-Fe-B alloy carry out dispensing respectively, and be respectively adopted strip cast alloys technology and obtain the rejection tablet of two kinds of alloys that thickness is 0.2 ~ 0.5mm；The rejection tablet of two kinds of alloys being mixed, airflow milling broken through hydrogen makes the magnetic powder that particle mean size is 3 ~ 5 μm；
2) crystal boundary modified phase passes sequentially through melting, thick broken, ball milling prepares crystal boundary modified phase powder or passes sequentially through that strip cast alloys, hydrogen is broken, airflow milling prepares crystal boundary modified phase powder, and crystal boundary modified phase powder mean particle sizes is 0.01 ~ 3.0 μm；
3) crystal boundary modified phase powder is mixed under nitrogen protection with step 1) gained magnetic powder, after mix homogeneously under the magnetic field of 1.5 ~ 2T oriented moulding, and make green compact through 17MPa isostatic cool pressing；
4) being placed in vacuum sintering furnace by green compact and be sintered, sintering temperature is 1020 ~ 1120 DEG C, is incubated 1 ~ 6h；Then carry out one-level heat treatment 1 ~ 3h at 850 ~ 950 DEG C respectively, carry out two grades of heat treatment 2 ~ 5h at 450 ~ 650 DEG C, obtain rare-earth permanent magnet.
Compared with prior art, the useful achievement of the present invention is: 1) control low HAAlloy (RE100-aMMa)xFe100-x-y- zByTMzComposition, make high abundance rare earth form stable Re2Fe14B phase, and will not decompose all the time in sintering process；2) low H is adoptedAWith high HATwo kinds of master alloyinies, it is possible to increase the remanent magnetism of magnet and magnetic energy product；3) crystal boundary modified phase adds the elements such as electrode potential higher Cu, Ni, improves the decay resistance of magnet, and crystal boundary modified phase can optimize the microstructure of magnet simultaneously, improves magnet performance；4) this method improves the problem of magnet corrosion resistance decline and remanent magnetism and the magnetic energy product decline caused by the interpolation of high abundance rare earth, and the Sintered NdFeB magnet of preparation reaches magnetic property and the decay resistance that application requires；5) the method technique is simple, can effectively reduce cost, it is adaptable to the production in enormous quantities of bulk magnet.
Detailed description of the invention
The rare-earth permanent magnet of application high abundance Rare Earth Production includes principal phase and crystal boundary modified phase, and principal phase accounts for the 90% ~ 99.99% of gross mass；Crystal boundary modified phase accounts for the 0.01% ~ 10% of gross mass, and described principal phase includes low HA(RE100-aMMa)-Fe-B alloy and high HANd-Fe-B alloy, low HA(RE100-aMMa)-Fe-B alloy accounts for the 50% ~ 99.99% of principal phase quality, high HANd-Fe-B alloy account for the 0.01% ~ 50% of principal phase quality.
Described low HA(RE100-aMMa)-Fe-B alloying component is (RE100-aMMa)xFe100-x-y-zByTMz, described high HANd-Fe-B alloying component be REx’Fe100-x’-y-zByTMz；Wherein, RE is one or more in other rare earth elements except La, Ce, and MM is one or more in La, Ce, LaCe alloy, LaCePrNd mischmetal；TM is one or more in Cu, Al, Co, Nb, Zr, Ga, Ta, Si, Ti, V, Mo, Mn, Ag, Mg, Zn；Wherein 1≤a≤50,26.7≤x≤31.0,29≤x '≤45,0.9≤y≤1.2,0.1≤z≤3.0.
Described crystal boundary modified coordinating is divided into R100-uTM’uWherein R is one or more in rare earth La, Ce, Pr, Pm, Sm, Eu, Nd, Dy, Gd, Tb, Ho, Er, Tm, Yb, Lu, and TM ' is one or more in Cu, H, O, F, Fe, Ga, Ti, Al, Co, Nb, Zr, Ta, Si, V, Mo, Mn, Ag, Mg, Zn；0 < u < 100.
Specifically comprising the following steps that of the preparation method of the rare-earth permanent magnet of application high abundance Rare Earth Production
1) according to low HA(RE100-aMMa)-Fe-B alloy and high HAThe composition of Nd-Fe-B alloy carry out dispensing respectively, and be respectively adopted strip cast alloys technology and obtain the rejection tablet of two kinds of alloys that thickness is 0.2 ~ 0.5mm；The rejection tablet of two kinds of alloys being mixed, airflow milling broken through hydrogen makes the magnetic powder that particle mean size is 3 ~ 5 μm；
2) crystal boundary modified phase passes sequentially through melting, thick broken, ball milling prepares crystal boundary modified phase powder or passes sequentially through that strip cast alloys, hydrogen is broken, airflow milling prepares crystal boundary modified phase powder, and crystal boundary modified phase powder mean particle sizes is 0.01 ~ 3.0 μm；
3) crystal boundary modified phase powder is mixed under nitrogen protection with step 1) gained magnetic powder, after mix homogeneously under the magnetic field of 1.5 ~ 2T oriented moulding, and make green compact through 17MPa isostatic cool pressing；
4) being placed in vacuum sintering furnace by green compact and be sintered, sintering temperature is 1020 ~ 1120 DEG C, is incubated 1 ~ 6h；Then carry out one-level heat treatment 1 ~ 3h at 850 ~ 950 DEG C respectively, carry out two grades of heat treatment 2 ~ 5h at 450 ~ 650 DEG C, obtain rare-earth permanent magnet.
Below in conjunction with specific embodiment, the present invention is further described, but protection scope of the present invention is not limited to following example:
Embodiment 1:
1) being calculated in mass percent, composition is (Nd70(LaCe)30)29.3B1.03Fe70.68(PrNd)31.5Fe61.93Al0.3Nb0.2Zr0.1B0.97Master alloying respectively dispensing, the raw material of preparation is contained in the crucible of intermediate frequency furnace, treats that vacuum reaches 10-2Begin to warm up during more than Pa, when aluminium alloy temperature rises to about 1500 DEG C, by tundish, aluminium alloy is poured on cooling copper roller, roller speed 2m/s, rejection tablet thickness 0.2 ~ 0.5mm；
2), after the rejection tablet of two kinds of master alloyinies being mixed in the ratio of 5:5, airflow milling broken through hydrogen makes the magnetic powder that particle mean size is 3.5 μm；
3) powder that Grain-Boundary Phase adopts melting, thick broken, ball grinding method makes particle mean size 1.5 μm, its composition is Nd32.5Fe62Cu5.5。
4) be calculated in mass percent, master alloying powder by 90.0%, 10.0% crystal boundary powder and 0.2% aviation gasoline and 0.2% antioxidant mix homogeneously after, under nitrogen protection by magnetic powder oriented moulding under the magnetic field of 2T, and make green compact through 17MPa isostatic cool pressing；
5) being placed in vacuum sintering furnace by green compact and be sintered, sintering temperature is 1025 DEG C, is incubated 6h；Then 850 DEG C of one-level heat treatment 3h, carry out two grades of heat treatment 2h at 650 DEG C.
6) gained magnet performance is Br=13.6kGs, Hcj=12.6kOe, (BH)max=45.8MGOe, Hk/Hcj=97.1%；
7) under 135 DEG C, 0.2MPa and 100% damp condition, carry out 96h accelerate weightless test, it is shown that the average quality of magnet prepared by this method is lost less than 1mg/cm2, meet magnet applications requirement.
Embodiment 2:
1) being calculated in mass percent, composition is (Nd60(LaCe)40)29.3B1.03Fe70.68(PrNd)30.5Gd1.0Fe61.93Al0.3Nb0.2Zr0.1B0.97Master alloying respectively dispensing, the raw material of preparation is contained in the crucible of intermediate frequency furnace, treats that vacuum reaches 10-2Begin to warm up during more than Pa, when aluminium alloy temperature rises to about 1500 DEG C, by tundish, aluminium alloy is poured on cooling copper roller, roller speed 2m/s, rejection tablet thickness 0.2 ~ 0.5mm；
2), after the rejection tablet of two kinds of master alloyinies being mixed in the ratio of 6:4, airflow milling broken through hydrogen makes the magnetic powder that particle mean size is 5 μm；
3) be calculated in mass percent, master alloying powder by 99.9%, 0.1% nano Cu powder with 0.2% aviation gasoline and after 0.2% antioxidant mixs homogeneously, under nitrogen protection by magnetic powder oriented moulding under the magnetic field of 2T, and make green compact through 17MPa isostatic cool pressing；
4) being placed in vacuum sintering furnace by green compact and be sintered, sintering temperature is 1120 DEG C, is incubated 1h；Then 950 DEG C of one-level heat treatment 1h, carry out two grades of heat treatment 5h at 450 DEG C.
5) gained magnet performance is Br=12.7kGs, Hcj=13.9kOe, (BH)max=39.5MGOe, Hk/Hcj=93%；
6) under 135 DEG C, 0.2MPa and 100% damp condition, carry out 96h accelerate weightless test, it is shown that the average quality of magnet prepared by this method is lost less than 1mg/cm2, meet magnet applications requirement.
Embodiment 3:
1) being calculated in mass percent, composition is (Nd60(LaCe)40)29.3B1.03Fe70.68(PrNd)31.5Fe61.93Al0.3Nb0.2Zr0.1B0.97Master alloying respectively dispensing, raw material is contained in the crucible of intermediate frequency furnace by preparation, treats that vacuum reaches 10-2Begin to warm up during more than Pa, when aluminium alloy temperature rises to about 1500 DEG C, by tundish, aluminium alloy is poured on cooling copper roller, roller speed 2m/s, rejection tablet thickness 0.2 ~ 0.5mm；
2), after the rejection tablet of two kinds of master alloyinies being mixed in the ratio of 6:4, airflow milling broken through hydrogen makes the magnetic powder that particle mean size is 3 μm；
3) powder that Grain-Boundary Phase adopts melting, thick broken, ball grinding method makes particle mean size 1.5 μm, its composition is Al85Cu15。
4) be calculated in mass percent, master alloying powder by 99.4%, 0.6% crystal boundary powder and 0.2% aviation gasoline and 0.2% antioxidant mix homogeneously after, under nitrogen protection by magnetic powder oriented moulding under the magnetic field of 2T, and make green compact through 17MPa isostatic cool pressing；
5) being placed in vacuum sintering furnace by green compact and be sintered, sintering temperature is 1055 DEG C, is incubated 3h；Then 900 DEG C of one-level heat treatment 2h, carry out two grades of heat treatment 3h at 580 DEG C.
6) gained magnet performance is Br=13.0kGs, Hcj=12.7kOe, (BH)max=43.1MGOe, Hk/Hcj=94.2%；
7) under 135 DEG C, 0.2MPa and 100% damp condition, carry out 96h accelerate weightless test, it is shown that the average quality of magnet prepared by this method is lost less than 1mg/cm2, meet magnet applications requirement.
Claims (3)
1. the rare-earth permanent magnet applying high abundance Rare Earth Production, it is characterised in that: including principal phase and crystal boundary modified phase, principal phase accounts for the 90% ~ 99.99% of gross mass；Crystal boundary modified phase accounts for the 0.01% ~ 10% of gross mass, and described principal phase includes low HA(RE100- aMMa)-Fe-B alloy and high HANd-Fe-B alloy, low HA(RE100-aMMa)-Fe-B alloy accounts for the 50% ~ 99.99% of principal phase quality, high HANd-Fe-B alloy account for the 0.01% ~ 50% of principal phase quality；Described low HA(RE100-aMMa)-Fe-B alloying component is (RE100-aMMa)xFe100-x-y-zByTMz, described high HANd-Fe-B alloying component be REx’Fe100-x’-y-zByTMz；Wherein, RE is one or more in other rare earth elements except La, Ce, and MM is one or more in La, Ce, LaCe alloy, LaCePrNd mischmetal；TM is one or more in Cu, Al, Co, Nb, Zr, Ga, Ta, Si, Ti, V, Mo, Mn, Ag, Mg, Zn；Wherein 1≤a≤50,26.7≤x≤31.0,29≤x '≤45,0.9≤y≤1.2,0.1≤z≤3.0.
2. a kind of rare-earth permanent magnet applying high abundance Rare Earth Production according to claim 1, it is characterised in that: described crystal boundary modified coordinating is divided into R100-uTM’u, wherein R is one or more in rare earth La, Ce, Pr, Pm, Sm, Eu, Nd, Dy, Gd, Tb, Ho, Er, Tm, Yb, Lu；TM ' is one or more in Cu, H, O, F, Fe, Ga, Ti, Al, Co, Nb, Zr, Ta, Si, V, Mo, Mn, Ag, Mg, Zn；0 < u < 100.
3. the preparation method of a rare-earth permanent magnet as claimed in claim 1, it is characterised in that specifically comprising the following steps that of it
1) according to low HA(RE100-aMMa)-Fe-B alloy and high HAThe composition of Nd-Fe-B alloy carry out dispensing respectively, and be respectively adopted strip cast alloys technology and obtain the rejection tablet of two kinds of alloys that thickness is 0.2 ~ 0.5mm；The rejection tablet of two kinds of alloys being mixed, airflow milling broken through hydrogen makes the magnetic powder that particle mean size is 3 ~ 5 μm；
2) crystal boundary modified phase passes sequentially through melting, thick broken, ball milling prepares crystal boundary modified phase powder or passes sequentially through that strip cast alloys, hydrogen is broken, airflow milling prepares crystal boundary modified phase powder, and crystal boundary modified phase powder mean particle sizes is 0.01 ~ 3.0 μm；
3) crystal boundary modified phase powder is mixed under nitrogen protection with step 1) gained magnetic powder, after mix homogeneously under the magnetic field of 1.5 ~ 2T oriented moulding, and make green compact through 17MPa isostatic cool pressing；
4) being placed in vacuum sintering furnace by green compact and be sintered, sintering temperature is 1020 ~ 1120 DEG C, is incubated 1 ~ 6h；Then carry out one-level heat treatment 1 ~ 3h at 850 ~ 950 DEG C respectively, carry out two grades of heat treatment 2 ~ 5h at 450 ~ 650 DEG C, obtain rare-earth permanent magnet.
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| CN104275487B (en) * | 2014-08-26 | 2017-01-11 | 宁波鑫丰磁业有限公司 | Preparation method of sintered NdFeB added with MM alloy |
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| CN107275027B (en) * | 2017-05-11 | 2019-02-05 | 浙江大学 | Using the cerium-rich rare earth permanent magnet and preparation method thereof of yttrium |
| CN107146674B (en) * | 2017-05-27 | 2018-11-09 | 浙江大学 | From the cerium-rich rare earth permanent magnet and its production method of heat treatment |
| CN107578870B (en) * | 2017-09-13 | 2019-03-12 | 内蒙古科技大学 | A method of permanent-magnet material is prepared using high abundance rare earth element |
| CN108231312A (en) * | 2017-12-26 | 2018-06-29 | 钢铁研究总院 | A kind of permanent-magnet alloy prepared based on mischmetal and preparation method thereof |
| CN108987017A (en) * | 2018-07-23 | 2018-12-11 | 浙江东阳东磁稀土有限公司 | A kind of no heavy rare earth sintered NdFeB |
| CN111029074B (en) * | 2019-12-30 | 2022-05-17 | 江西师范大学 | Preparation method of sintered rare earth iron boron permanent magnet material for regulating grain boundary |
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