CN100517520C - Method for preparing high coercitive force and high corrosion resistance magnetic body by nanometer powdered aluminium crystal boundary modified - Google Patents
Method for preparing high coercitive force and high corrosion resistance magnetic body by nanometer powdered aluminium crystal boundary modified Download PDFInfo
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- CN100517520C CN100517520C CNB2007101161265A CN200710116126A CN100517520C CN 100517520 C CN100517520 C CN 100517520C CN B2007101161265 A CNB2007101161265 A CN B2007101161265A CN 200710116126 A CN200710116126 A CN 200710116126A CN 100517520 C CN100517520 C CN 100517520C
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Abstract
The invention discloses a method for preparing a magnet with high intrinsic coercivity and high corrosion resistance by applying the modification in grain boundary of nano aluminum powders. The steps are the following: 1) main phase alloy is made into ingot alloy of Nd-Fe-B by adopting a casting technology or into rapidly solidified flakes of Nd-Fe-B by adopting a rapidly solidified flake technology, and phase alloy of the grain boundary is made into ingot alloy by adopting the casting technology or into rapidly solidified flakes by adopting the rapidly solidified flake technology or into rapid quenched ribbons by adopting a rapid quenching technology; 2) the main phase alloy and the phase alloy of the grain boundary are made into powders respectively; 3) nano aluminum is added in phase alloy powders of the gain boundary; 4) the mixed powders of main phase alloy and the phase alloy of the grain boundary is suppressed and molded in a magnetic field; 5) a sintered magnet is made inside a high vacuum sintering furnace. The sintered Nd-Fe-B obtained by the invention has high coercivity and good corrosion resistance. The technology is applicable for batch production in a large scope. By adopting the invention, sintered Nd-Fe-B with high coercivity and good corrosion resistance can be prepared.
Description
Technical field
The present invention relates to the crystal boundary modified preparation high-coercive force of a kind of nanometer aluminium powder, high corrosion-resistant magnet method.
Background technology
The rare-earth Nd-Fe-B series permanent magnetic material is current and most important permanent magnetic material in significant period of time from now on, and the new beginning in rare earth permanent magnet field has been opened up in its appearance.Rare-earth Nd-Fe-B permanent magnet is the strongest permanent magnet of contemporary magnetic, and it not only has excellent specific properties such as high energy product, high performance-price ratio, and is processed into various sizes easily.Aeronautics and Astronautics, short-wave communication tedhnology, electronics, electroacoustic, electromechanics, computing technique, automatic technology, auto industry, petrochemical industry, magnetic separation technique, instrument and meter, magnetic medical skill now have been widely used in and other need be with in the device and equipment of permanent-magnetic field.
The basic mechanical design feature index of Nd-Fe-B series permanent magnetic material is remanent magnetism B
r, coercive force H
c(HCJ H
CjWith magnetic strength coercive force H
Cb), magnetic energy product (BH)
MaxWith Curie temperature T
cH
CjLimiting value be magnetocrystalline anisotropy field H
A, it depends on the magnetocrystalline anisotropy constant K of material
1And K
2Nd
2Fe
14The anisotropy field of B compound, promptly coercitive theoretical boundary is 80kOe, however the actual coercive force of sintered Nd-Fe-B alloy only is the 1/3-1/30 of its theoretical value, thereby the coercive force of raising Sintered NdFeB magnet is also had great potentialities and can be dug.Coercitive minimizing mainly is that (relative orientation that comprises intergranule) causes because grainiess defective and crystal grain interact.Generally believe that at present the coercive force mechanism of nd-fe-b permanent magnetic alloy is relevant with temperature, nucleation mechanism control coercive force when room temperature and above temperature thereof, pinning mechanism control coercive force during higher temperature.A large amount of experimental results show: the Sintered NdFeB magnet microstructural undesirable be the main cause that causes coercive force lower than its theoretical value, coercive force is a structure sensitive parameter.
Everybody generally admits, and the microstructure model with high-coercive force sintered neodymium iron boron material should be: the uniform crystal boundary of thickness is wrapped in Nd mutually
2Fe
14B crystal grain, Nd
2Fe
14B crystal grain is tiny, be evenly distributed, and the grain shape rule is spherical in shape, Nd
2Fe
14B grain orientation height unanimity, Nd
2Fe
14The chemical composition of B crystal grain is consistent with even structure.Two alloyages are that principal phase and crystal-boundary phase alloy are smelted respectively, and the main-phase alloy composition is near Nd
2Fe
14B is just dividing ratio, and crystal-boundary phase alloy is rich rare earth, and two kinds of alloys are broken respectively, and proportioning is passed through magnetic field orientating compression moulding then according to a certain percentage, is prepared into Sintered NdFeB magnet through the oversintering tempering process at last.Utilizing two alloyages is to improve the coercitive effective way of magnet, and it had both reduced crystal boundary separating out in principal phase, can reduce it again in the reunion that crystal boundary hands over the corner to locate, and makes principal phase more reasonable with crystal boundary composition mutually, can obtain higher H
CjTherefore we can utilize this principle to improve the Nd-Fe-B permanent magnet performance.
The invention provides a kind of new method and utilize the pairing gold process, add coercive force and corrosion resistance that nano powder improves sintered NdFeB.By add nanometer aluminium powder in crystal boundary mutually in, and, make the non magnetic crystal boundary that is mixed with nanometer aluminium powder be dispersed in principal phase Nd mutually by adding lubricant, antioxidant
2Fe
14B grain surface layer, because the aluminium fusing point is lower, good corrosion resistance, played the effect of the lubricated crystal boundary of resistance, suppressed the exchange-coupling interaction between the hard magnetic phase simultaneously, improved microstructure, thereby improved the coercive force of magnet, and the aluminium modification of high rotproofness corrosion-prone rich neodymium phase, and then improved the corrosion resistance of magnet.
Summary of the invention
The purpose of this invention is to provide the crystal boundary modified preparation high-coercive force of a kind of nanometer aluminium powder, high corrosion-resistant magnet method.
Its step is:
1) main-phase alloy adopts casting technique to make the neodymium iron boron alloy of ingot or make neodymium iron boron rapid hardening thin slice with rapid hardening thin slice technology, by the quick-fried method of hydrogen or disintegrating machine with the main-phase alloy fragmentation, fragmentation is after the airflow milling abrasive material, and making average particulate diameter is the main-phase alloy powder of 2-10 μ m;
2) crystal-boundary phase alloy adopts casting technique to make alloy of ingot or rapid hardening thin slice technology makes the rapid hardening thin slice or rapid quenching technique is made rapid tempering belt, by the quick-fried method of hydrogen or disintegrating machine with the crystal-boundary phase alloy fragmentation, fragmentation is after the airflow milling abrasive material, and making average particulate diameter is the crystal-boundary phase alloy powder of 2-10 μ m;
3) in the crystal-boundary phase alloy powder of 100 weight portions, add the nano aluminum of 2-20 weight portion, the antioxidant of 1-10 weight portion, the evenly mixed crystal-boundary phase alloy powder that obtains the nano aluminum modification in batch mixer;
4) crystal-boundary phase alloy powder and main-phase alloy powder, the gasoline with the nano aluminum modification is uniformly mixed into mixed-powder in batch mixer, and wherein the crystal-boundary phase alloy powder weight of nano aluminum modification accounts for the 1-20% of total weight, and gasoline accounts for the 0.5-5% of total weight;
5) mixed-powder compression moulding blank in the magnetic field of 1.2-2.0T;
6) parison spare is put into high vacuum sintering furnace,, pass through 500-650 ℃ of tempering heat treatment 2-4h again, make sintered magnet at 1050-1125 ℃ of sintering 2-4h.
Described main-phase alloy is in atomic percent, and its composition is Nd
aFe
100-a-b-cB
bM
c, 11≤a≤16,5.4≤b≤6.6,0≤c≤6 wherein, M be in Dy, Tb, Nb, Co, Ga, Zr, Al, the Cu element one or more.Crystal-boundary phase alloy is in atomic percent, and its composition is Nd
dFe
100-d-e-fB
eR
f, 13.5≤d≤30,4≤e≤7,0≤f≤15 wherein, R be in Dy, Tb, Nb, Co, Ga, Zr, C, Al, Cu, the Si element one or more.The nano aluminum average particulate diameter is 5-50nm.Antioxidant is polyethylene oxide alkyl ethers, poly(ethylene oxide) mono fatty acid ester or poly(ethylene oxide) allyl ether.
Magnet coercive force that the present invention makes does not add nano aluminum than adopting the pairing gold process and makes magnet coercive force height, good corrosion resistance, and principal phase and crystal boundary powder mutually are difficult for oxidation, and technical process is suitable for mass production.
Embodiment
The present invention adopts two alloyages, by the interpolation of nano aluminum, with nano aluminum be dispersed in crystal boundary mutually in, to modified grain boundary phase to improve the coercive force of sintered NdFeB.In the invention, the non magnetic crystal boundary phase through the nano aluminum modification is dispersed in principal phase Nd
2Fe
14The B crystal grain boundary improves microstructure, effectively cuts off the exchange-coupling interaction between the hard magnetic phase, thereby improves the magnet coercive force.Adopt two alloyage technologies to add nano aluminum and can effectively improve the crystal boundary phase morphology, make the crystal boundary after the modification be uniformly distributed in around the main phase grain mutually, play an important role at aspects such as magnet densification and degaussing exchange-coupling interactions simultaneously, thereby promote coercive force, corrosion resistance to improve.
Concrete steps of the present invention are as follows:
1) adopt the pairing gold process that main-phase alloy and crystal-boundary phase alloy are made respectively.Main-phase alloy adopts casting technique to make the neodymium iron boron alloy of ingot, or makes neodymium iron boron rapid hardening thin slice with rapid hardening thin slice technology, and its composition is Nd
aFe
100-a-b-cB
bM
c(at%), 11≤a≤16,5.4≤b≤6.6,0≤c≤6 wherein, M be in Dy, Tb, Nb, Co, Ga, Zr, Al, the Cu element one or more.Crystal-boundary phase alloy adopts casting technique to make alloy of ingot or rapid hardening thin slice technology makes the rapid hardening thin slice or rapid quenching technique is made rapid tempering belt, and its composition is by molecular formula Nd
dFe
100-d-e-fB
eR
f(at%) preparation, wherein R be in Dy, Tb, Nb, Co, Ga, Zr, C, Al, Cu, the Si element one or more, 13.5≤d≤30,4≤e≤7,0≤f≤15 wherein.
2) with main-phase alloy and crystal-boundary phase alloy powder process respectively.Undertaken slightly breaking by jaw crusher earlier, broken in being undertaken by middle disintegrating machine then.Perhaps adopt the quick-fried method of hydrogen directly broken, at room temperature saturated suction hydrogen is made the quick-fried powder of hydrogen at 400-600 ℃ of dehydrogenase 12-10h then.Broken back main-phase alloy and crystal-boundary phase alloy are by the airflow milling abrasive material, and making average particulate diameter is 2-10 μ m powder.
3) in the crystal-boundary phase alloy powder of 100 weight portions, add the nano aluminum of 2-20 weight portion, the antioxidant of 1-10 weight portion, the evenly mixed crystal-boundary phase alloy powder that obtains the nano aluminum modification in batch mixer, wherein antioxidant is a kind of in polyethylene oxide alkyl ethers or poly(ethylene oxide) mono fatty acid ester or the poly(ethylene oxide) allyl ether.
4) will mix with the main-phase alloy powder through the crystal-boundary phase alloy powder of nano aluminum modification, the crystal-boundary phase alloy powder weight accounts for the 1-20% of total weight, adds the gasoline of 0.5-5% simultaneously, is uniformly mixed into mixed-powder in batch mixer.Wherein the nano aluminum average particulate diameter is 5-50nm.
4) mixed-powder is compressed to parison spare in the magnetic field orientating moulding press, and moulding alignment magnetic field 1.2-2.0T increases the degree of orientation that magnetic can be improved in magnetic field.And the compression moulding of parison spare is finished in the glove box of sealing fully, makes the magnetic air-isolation, has avoided on the one hand the danger of catching fire because of magnet oxidation heating, has reduced the oxygen content of final magnet on the other hand again.
5) parison spare is put into high vacuum sintering furnace, 1050-1125 ℃ of sintering 2-4h passes through 500-650 ℃ of tempering heat treatment 2-4h again, makes sintered magnet.
The particular content of casting technique of the present invention, rapid hardening thin slice technology, rapid quenching technique, the quick-fried method technology of hydrogen is seen Zhou Shouzeng, Dong Qingfei " superpower permanet magnetic body---rare-earth system permanent magnetic material " Beijing respectively, metallurgical industry publishing house, 2004.2 second edition, p159-164, p498-504, p326-332, p508-511, p169-172.
Embodiment 1:
1) main-phase alloy and crystal-boundary phase alloy are prepared respectively.Main-phase alloy adopts rapid hardening thin slice technology, and copper roller linear resonance surface velocity is 1.2m/s, and composition is Nd
13.12Fe
80.51B
5.73(Dy
0.22Al
0.24Zr
0.18) (at%), crystal-boundary phase alloy adopts 15m/s fast quenching speed to be prepared into rapid tempering belt, composition is Nd
17.2Fe
75.58B
6.38Dy
0.64Ga
0.2(at%).
2) with main-phase alloy and crystal-boundary phase alloy powder process respectively.Undertaken slightly breaking by jaw crusher, broken in being undertaken by middle disintegrating machine, under nitrogen protection, make the powder that average particulate diameter is 3.2 μ m then by airflow milling.
3) in the crystal-boundary phase alloy powder, add account for its weight 2.4%, through the nano aluminum powder (average particulate diameter is 40nm) of dispersion treatment, and 3% antioxidant polyethylene oxide alkyl ethers, evenly mixed in batch mixer.
4) will mix with the main-phase alloy powder through the crystal-boundary phase alloy powder of nano aluminum modification, make its weight account for 10% of total weight, add 1% gasoline simultaneously, in batch mixer, be uniformly mixed into mixed-powder.
5) mixed powder is compressed to parison spare by the magnetic field orientating moulding press, moulding alignment magnetic field 1.6T finishes in the glove box of sealing fully, makes the magnetic air-isolation.
6) parison spare is put into the high vacuum sintering furnace sintering, 1085 ℃ of sintering 3h, and 560 ℃ of tempering heat treatment 3h make sintered magnet again.
7) adopt the pairing gold process, add crystal-boundary phase alloy as stated above and account for total weight 10% composition mixed-powder, but do not add nano aluminum, adopt identical magnetic field orientating die mould and sintering, tempering process to be prepared into magnet.
(5-10psig, 110-115 ℃, (corrosion resistance of Φ 1 * 0.5cm), employing characteristic of magnetization automatic measuring instrument AMF measures the magnetic property of magnet, performance such as table one 100h) to have tested sample to adopt autoclave test.
Table one, the magnet performance that adopts different process to prepare
| Preparation technology | B r (kGs) | H cj (kOe) | (BH) max (MGOe) | Quality (mg) before the test | Test back quality (mg) | Mass loss (mg/cm 2) |
| The pairing gold process does not add nanometer Al | 13.74 | 12.28 | 46.46 | 3120 | 2800 | 320 |
| The pairing gold process adds nanometer Al | 13.82 | 14.41 | 49.12 | 3112 | 3080 | 22 |
From table one as can be seen, adopt the pairing gold process to add nano aluminum and make the sintered NdFeB coercive force and do not add nano aluminum than adopting the pairing gold process and make magnet coercive force height, good corrosion resistance, therefore add the sintered NdFeB that nano aluminum can be prepared high-coercive force, highly corrosion resistant by the pairing gold process.
Embodiment 2:
1) main-phase alloy and crystal-boundary phase alloy are prepared respectively.Main-phase alloy adopts rapid hardening thin slice technology, and copper roller linear resonance surface velocity is 2.0m/s, and composition is Nd
14.2Fe
78.15B
5.81(Tb
0.31Al
0.24Co
1Nb
0.18Zr
0.1) (at%), crystal-boundary phase alloy adopts 15m/s fast quenching speed to be prepared into rapid tempering belt, composition is Nd
16.7Fe
76.27B
6.31(Dy
0.84Ga
0.2Cu
0.32) (at%).
2) with main-phase alloy and crystal-boundary phase alloy powder process respectively.Directly broken by the quick-fried method of hydrogen, at room temperature saturated suction hydrogen is made the quick-fried powder of hydrogen at 500 ℃ of dehydrogenation 8h then, makes the powder that average particulate diameter is 3.3 μ m by airflow milling then under nitrogen protection.
3) in the crystal-boundary phase alloy powder, add account for its weight 20%, through the nano aluminum powder (average particulate diameter is 6nm) of dispersion treatment, and 4% antioxidant poly(ethylene oxide) mono fatty acid ester, evenly mixed in batch mixer.
4) will mix with the main-phase alloy powder through the crystal-boundary phase alloy powder of nano aluminum modification, make its weight account for 5% of total weight, add 1.2% gasoline simultaneously, in batch mixer, be uniformly mixed into mixed-powder.
5) mixed powder is compressed to parison spare by the magnetic field orientating moulding press, moulding alignment magnetic field 1.6T finishes in the glove box of sealing fully, makes the magnetic air-isolation.
6) parison spare is put into the high vacuum sintering furnace sintering, 1080 ℃ of sintering 3h, and 560 ℃ of tempering heat treatment 2.5h make sintered magnet again.
7) adopt the pairing gold process, add crystal-boundary phase alloy as stated above and account for total weight 5% composition mixed-powder, but do not add nano aluminum, adopt identical magnetic field orientating die mould and sintering, tempering process to be prepared into magnet.
(5-10psig, 110-115 ℃, (corrosion resistance of Φ 1 * 0.5cm), employing characteristic of magnetization automatic measuring instrument AMF measures the magnetic property of magnet, performance such as table two 100h) to have tested sample to adopt autoclave test.
Table two, the magnet performance that adopts different process to prepare
| Preparation technology | H cj (kOe) | Quality (mg) before the test | Test back quality (mg) | Mass loss (mg/cm 2) |
| The pairing gold process does not add nanometer Al | 17.88 | 3150 | 2926 | 124 |
| The pairing gold process adds nanometer Al | 21.32 | 3088 | 3042 | 46 |
From table two as can be seen, adopt the pairing gold process to add nano aluminum and make the sintered NdFeB coercive force and do not add nano aluminum than adopting the pairing gold process and make magnet coercive force height, good corrosion resistance, therefore add the sintered NdFeB that nano aluminum can be prepared high-coercive force, highly corrosion resistant by the pairing gold process.
Embodiment 3:
1) main-phase alloy and crystal-boundary phase alloy are prepared respectively.Main-phase alloy adopts rapid hardening thin slice technology, and copper roller linear resonance surface velocity is 2.0m/s, and composition is Nd
11.06Fe
82.3B
5.95Dy
0.89(at%), adopt the fast quenching technology, with crystal-boundary phase alloy Nd
27.83Fe
56.5B
6.68Dy
2.47Co
6.52(at%) be prepared into rapid tempering belt, fast quenching speed 15m/s.
2) with main-phase alloy and crystal-boundary phase alloy powder process respectively.Undertaken slightly breaking by jaw crusher, broken in being undertaken by middle disintegrating machine, under nitrogen protection, make the powder that average particulate diameter is 4.0 μ m then by airflow milling.
3) in the crystal-boundary phase alloy powder, add the nano aluminum powder (average particulate diameter is 15nm) that accounts for its weight 10% through dispersion treatment, and 2% antioxidant polyethylene oxide alkyl ethers, evenly mixed in batch mixer.
4) will mix with the main-phase alloy powder through the crystal-boundary phase alloy powder of nano aluminum powder modification, make its weight account for 10% of alloy total weight, add 2% gasoline simultaneously, in batch mixer, be uniformly mixed into mixed-powder.
5) mixed powder is compressed to parison spare by the magnetic field orientating moulding press, moulding alignment magnetic field 1.6T finishes in the glove box of sealing fully, makes the magnetic air-isolation.
6) parison spare is put into the high vacuum sintering furnace sintering, 1075 ℃ of sintering 4.5h, and 560 ℃ of tempering heat treatment 3h make sintered magnet again.
7) adopt the pairing gold process, add crystal-boundary phase alloy as stated above and account for total weight 10% composition mixed-powder, but do not add nano aluminum, adopt identical magnetic field orientating die mould and sintering, tempering process to be prepared into magnet.
(5-10psig, 110-115 ℃, (corrosion resistance of Φ 1 * 0.5cm), employing characteristic of magnetization automatic measuring instrument AMF measures the magnetic property of magnet, performance such as table three 100h) to have tested sample to adopt autoclave test.
Table three, the magnet performance that adopts different process to prepare
| Preparation technology | H cj(kOe) | Mass loss (mg/cm 2) |
| The pairing gold process does not add nanometer Al | 13.68 | 159 |
| The pairing gold process adds nanometer Al | 16.53 | 21 |
From table three as can be seen, adopt the pairing gold process to add nano aluminum and make the sintered NdFeB coercive force and do not add nano aluminum than adopting the pairing gold process and make magnet coercive force height, good corrosion resistance, therefore add the sintered NdFeB that nano aluminum can be prepared high-coercive force, highly corrosion resistant by the pairing gold process.
Embodiment 4:
1) main-phase alloy and crystal-boundary phase alloy are prepared respectively.Main-phase alloy adopts rapid hardening thin slice technology, and copper roller linear resonance surface velocity is 1.5m/s, and composition is Nd
12.69Fe
81.42B
5.7Dy
0.4(at%), crystal-boundary phase alloy adopts 15m/s fast quenching speed to be prepared into rapid tempering belt, and composition is Nd
23.74Fe
64.98B
6.89(Dy
0.92Co
1.27Cu
0.35Nb
0.4Al
1.46) (at%).
2) with main-phase alloy and crystal-boundary phase alloy powder process respectively.Directly broken by the quick-fried method of hydrogen, at room temperature saturated suction hydrogen is made the quick-fried powder of hydrogen at 500 ℃ of dehydrogenation 8h then, makes the powder that average particulate diameter is 6.5 μ m by airflow milling then under nitrogen protection.
3) in the crystal-boundary phase alloy powder, add the nano aluminum powder (average particulate diameter is 30nm) that accounts for its weight 16% through dispersion treatment, and 8% antioxidant poly(ethylene oxide) allyl ether, evenly mixed in batch mixer.
4) will mix with the main-phase alloy powder through the crystal-boundary phase alloy powder of nano aluminum modification, make its weight account for 10% of total weight, add 3.4% gasoline simultaneously, in batch mixer, be uniformly mixed into mixed-powder.
5) mixed powder is compressed to parison spare by the magnetic field orientating moulding press, moulding alignment magnetic field 1.8T finishes in the glove box of sealing fully, makes the magnetic air-isolation.
6) parison spare is put into the high vacuum sintering furnace sintering, 1100 ℃ of sintering 3h, and 560 ℃ of tempering heat treatment 3h make sintered magnet again.
7) adopt the pairing gold process, add crystal-boundary phase alloy as stated above and account for total weight 10% composition mixed-powder, but do not add nano aluminum, adopt identical magnetic field orientating die mould and sintering, tempering process to be prepared into magnet.
(5-10psig, 110-115 ℃, (corrosion resistance of Φ 1 * 0.5cm), employing characteristic of magnetization automatic measuring instrument AMF measures the magnetic property of magnet, performance such as table four 100h) to have tested sample to adopt autoclave test.
Table four, the magnet performance that adopts different process to prepare
| Preparation technology | H cj(kOe) | Mass loss (mg/cm 2) |
| The pairing gold process does not add nanometer Al | 12.23 | 224 |
| The pairing gold process adds nanometer Al | 13.69 | 16 |
From table four as can be seen, adopt the pairing gold process to add nano aluminum and make the sintered NdFeB coercive force and do not add nano aluminum than adopting the pairing gold process and make magnet coercive force height, good corrosion resistance, therefore add the sintered NdFeB that nano aluminum can be prepared high-coercive force, highly corrosion resistant by the pairing gold process.
Claims (4)
1. the crystal boundary modified preparation high-coercive force of nanometer aluminium powder, high corrosion-resistant magnet method is characterized in that its step is:
1) main-phase alloy adopts casting technique to make the neodymium iron boron alloy of ingot or make neodymium iron boron rapid hardening thin slice with rapid hardening thin slice technology, by the quick-fried method of hydrogen or disintegrating machine with the main-phase alloy fragmentation, fragmentation is after the airflow milling abrasive material, and making average particulate diameter is the main-phase alloy powder of 2-10 μ m;
2) crystal-boundary phase alloy adopts casting technique to make alloy of ingot or rapid hardening thin slice technology makes the rapid hardening thin slice or rapid quenching technique is made rapid tempering belt, by the quick-fried method of hydrogen or disintegrating machine with the crystal-boundary phase alloy fragmentation, fragmentation is after the airflow milling abrasive material, and making average particulate diameter is the crystal-boundary phase alloy powder of 2-10 μ m;
3) in the crystal-boundary phase alloy powder of 100 weight portions, add the nano aluminum of 2-20 weight portion, the antioxidant of 1-10 weight portion, the evenly mixed crystal-boundary phase alloy powder that obtains the nano aluminum modification in batch mixer;
4) crystal-boundary phase alloy powder and main-phase alloy powder, the gasoline with the nano aluminum modification is uniformly mixed into mixed-powder in batch mixer, and wherein the crystal-boundary phase alloy powder weight of nano aluminum modification accounts for the 1-20% of total weight, and gasoline accounts for the 0.5-5% of total weight;
5) mixed-powder compression moulding blank in the magnetic field of 1.2-2.0T;
6) parison spare is put into high vacuum sintering furnace,, passes through 500-650 ℃ of tempering heat treatment 2-4h again, make sintered magnet at 1050-1125 ℃ of sintering 2-4h,
Described nano aluminum average particulate diameter is 5-50nm.
2. the crystal boundary modified preparation high-coercive force of nanometer aluminium powder according to claim 1, high corrosion-resistant magnet method is characterized in that described main-phase alloy in atomic percent, and its composition is Nd
aFe
100-a-b-cB
bM
c, 11≤a≤16,5.4≤b≤6.6,0≤c≤6 wherein, M be in Dy, Tb, Nb, Co, Ga, Zr, Al, the Cu element one or more.
3. the crystal boundary modified preparation high-coercive force of nanometer aluminium powder according to claim 1, high corrosion-resistant magnet method is characterized in that described crystal-boundary phase alloy in atomic percent, and its composition is Nd
dFe
100-d-e-fB
eR
f, 13.5≤d≤30,4≤e≤7,0≤f≤15 wherein, R be in Dy, Tb, Nb, Co, Ga, Zr, C, Al, Cu, the Si element one or more.
4. the crystal boundary modified preparation high-coercive force of nanometer aluminium powder according to claim 1, high corrosion-resistant magnet method is characterized in that described antioxidant is polyethylene oxide alkyl ethers, poly(ethylene oxide) mono fatty acid ester or poly(ethylene oxide) allyl ether.
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| CN104752013A (en) * | 2013-12-27 | 2015-07-01 | 比亚迪股份有限公司 | Rare earth permanent magnetic material and preparation method thereof |
| DE102018107491A1 (en) * | 2017-03-31 | 2018-10-04 | Tdk Corporation | R-T-B BASED PERMANENT MAGNET |
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| CN107424702A (en) * | 2017-09-06 | 2017-12-01 | 京磁材料科技股份有限公司 | The preparation method of high-coercive force NdFeB magnets |
| CN110911149A (en) * | 2019-11-28 | 2020-03-24 | 烟台首钢磁性材料股份有限公司 | Preparation method for improving coercive force of neodymium iron boron sintered permanent magnet |
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2007
- 2007-12-03 CN CNB2007101161265A patent/CN100517520C/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| Effects of Al and Al/Mo addition on microstructures andmagnetic properties of sintered Nd22Fe71B magnets. Yang S, etc.Transactions of Nonferrous Metals Society of China,Vol.10 No.5. 2000 |
| Effects of Al and Al/Mo addition on microstructures andmagnetic properties of sintered Nd22Fe71B magnets. Yang S, etc.Transactions of Nonferrous Metals Society of China,Vol.10 No.5. 2000 * |
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| CN101178963A (en) | 2008-05-14 |
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