CN1688000A - Method for increasing sintering Nd-Fe-B coercive force by adding nano-oxide in crystal boundary phase - Google Patents
Method for increasing sintering Nd-Fe-B coercive force by adding nano-oxide in crystal boundary phase Download PDFInfo
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- 238000005245 sintering Methods 0.000 title claims abstract description 24
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- 239000000843 powder Substances 0.000 claims abstract description 52
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- 238000005496 tempering Methods 0.000 claims description 22
- -1 poly(ethylene oxide) Polymers 0.000 claims description 18
- 239000001257 hydrogen Substances 0.000 claims description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims description 14
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 13
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- 239000003963 antioxidant agent Substances 0.000 claims description 12
- 230000003078 antioxidant effect Effects 0.000 claims description 12
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- 238000003801 milling Methods 0.000 claims description 11
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- 229910052802 copper Inorganic materials 0.000 claims description 10
- 230000000171 quenching effect Effects 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 7
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 5
- 229910052771 Terbium Inorganic materials 0.000 claims description 5
- 150000005215 alkyl ethers Chemical class 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 229910052758 niobium Inorganic materials 0.000 claims description 5
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- ATVJXMYDOSMEPO-UHFFFAOYSA-N 3-prop-2-enoxyprop-1-ene Chemical compound C=CCOCC=C ATVJXMYDOSMEPO-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
This invention discloses a method for increasing sintered Nd FeB coercive force by adding nm oxide in grain-boundary phase including the following steps: 1,applying casting technology to produce NdFeB ingot alloy or applying rapid hardening film technology to produce NdFeB rapid hardening film of with host phase alloy, applying casting technology to produce ingot alloy or rapid hardening film technology to get rapid hardening film or rapid quench technology to manufacture a rapid quench strip with the grain boundary phase alloy, 2, processing powder with the two alloys, 3, adding a nm oxide to the grain boundary phase alloy powder, 4, pressing the mixed powder into formation, 5, producing sintered magnetic body in a vacuum sintering oven.
Description
Technical field
The present invention relates to the middle mutually nano-oxide that adds of a kind of crystal boundary and improve sintered NdFeB coercive force method.
Background technology
Nd-Fe-B rare earth permanent magnetic material is that people such as 1983 SUMITOMO CHEMICAL particulate metal Sagawa of company are at first produced.Rare-earth Nd-Fe-B permanent magnet is the strongest permanent magnet of contemporary magnetic, it not only has excellent specific properties such as high energy product, high performance-price ratio, and be 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 specially adapted to develop the various regeneration products of high-performance, miniaturization, lightness with in the device and equipment of permanent-magnetic field.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.
The basic mechanical design feature index of Nd-Fe-B 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 Tc.The researcher of permanent magnetic material and the producer's main task are exactly the potentiality of excavated material to greatest extent, improve the B of permanent magnetic material
r, H
c, (BH)
MaxAnd T
cB
rLimiting value be J
s, (BH)
MaxLimiting value be 1/4J
s 2, and J
sDepend on the magnetic atom number of forming this material and the size of atomic magnetic moment.H
CjLimiting value be magnetocrystalline anisotropy field H
A, it depends on the magnetocrystalline anisotropy constant K of material
1And K
2
Nd
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.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.Element adds and substitutes is to improve coercitive common method, discovers that elements such as Dy, Al, Nb, Ga, Tb, W, Mo can improve the coercive force and the temperature stability thereof of alloy, but magnet remanent magnetism and magnetic energy product are all had adverse effect.
Adopting two alloyages is 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, crystal-boundary phase alloy is rich rare earth (R=Nd, Pr, Dy, Tb etc.), and contain one or more the element of Co, Al, Cu, Ga, B, Ti etc., two kinds of alloys are broken respectively, proportioning according to a certain percentage, pass through magnetic field orientating compression moulding then, be prepared into Sintered NdFeB magnet through the oversintering tempering process at last.
Utilizing two alloyages also 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, and the content of rare earth of principal phase can be more near Nd simultaneously
2Fe
14B is just dividing ratio, also can obtain higher H
CjThis is because principal phase is Nd
2Fe
14During B, there is not unnecessary neodymium metal to be present in the alloy, so be difficult for oxidation, though crystal boundary has the very high neodymium of content mutually, but the amorphous alloy with the fast quenching technology obtains does not exist crystal grain and grain boundary, so also be difficult for oxidation, therefore two alloyages can guarantee to also have when very low neodymium content enough crystal boundary phase and rich boron borderline phase to exist, and guarantee that alloy has high H
Cj
The present invention adopts two alloyages, by the interpolation of nano-oxide, with nano-oxide be dispersed in crystal boundary mutually in, to modified grain boundary phase to improve the coercive force of sintered NdFeB.In the invention, main-phase alloy and crystal-boundary phase alloy are prepared respectively, adopt the airflow milling flouring technology, by add nano-oxide particles in crystal boundary mutually in, and add lubricant, antioxidant, the non magnetic crystal boundary phase through the nano-oxide 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-oxide 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 to improve.
Summary of the invention
The purpose of this invention is to provide the middle mutually nano-oxide that adds of a kind of crystal boundary and improve sintered NdFeB coercive force 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, and 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;
2) adopt the quick-fried method of hydrogen or by alloy of ingot, rapid hardening thin slice or the rapid tempering belt fragmentation of disintegrating machine with alloy of ingot or the rapid hardening thin slice and the crystal-boundary phase alloy of main-phase alloy, broken back is by the airflow milling abrasive material, making average particulate diameter respectively is 2-10 μ m powder;
3) in the crystal-boundary phase alloy powder, add account for its weight 2-20%, through the nano-oxide of dispersion treatment, and the antioxidant of 1-10%, evenly mixed in batch mixer;
4) will mix with the main-phase alloy powder through the crystal-boundary phase alloy powder that nano-oxide mixes, 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;
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.
Magnet coercive force that the present invention makes does not add nano-oxide than adopting the pairing gold process and makes magnet coercive force height, more makes magnet coercive force height than single alloyage, and principal phase and crystal boundary powder mutually are difficult for oxidation, and technical process is suitable for mass production.By two alloyages and add nano-oxide, can prepare the sintered NdFeB of high-coercive force.
Embodiment
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
100a-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, add account for its weight 2-20%, through the nano-oxide of dispersion treatment, and the antioxidant of 1-10%, evenly mixed 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 that nano-oxide mixes, 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 nano-oxide is SiO
2, ZrO
2, CuO, Fe
2O
3, Al
2O
3, Y
2O
3, TiO
2In one or more, average particulate diameter is 2-40nm.
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.
Casting technique of the present invention is made alloy of ingot, is the alloy liquid after the melting to be cast in the water cooled mo(u)ld of 3-10mm thickness the Nd of alloy of ingot
2Fe
14The B crystal is grown in the sheet mode, the about 30-50 μ of the brilliant thickness of sheet m, and the about 500-1500 μ of width m, length depends on ingot casting cooling direction ingot mould size, its cooling rate is slow.
Rapid hardening thin slice technology is made the rapid hardening thin slice, it is the surface of the alloy liquid after the melting being watered the cooling running roller, about running roller rotational line speed 1-2m/s, the strip of near quick setting is sent in the cooling bath, obtain the about 0.3mm of thickness, the about 5-25 μ of the brilliant thickness of sheet m in the wide tens millimeters thin slice, crystal, its cooling rate about 2.5 * 10
3K/s.
Rapid quenching technique is made rapid tempering belt, is the red copper wheel surface that the alloy liquid after the melting is watered high speed rotating, and about rotational line speed 18m/s, the thickness that makes strip is 30-80 μ m, width 1-30mm, cooling rate about 10
5K/s.
The quick-fried method technology of hydrogen is with the rustless steel container of packing into of the NdFeB alloy with unsalted surface, after vacuumizing, charge into high-purity hydrogen, reach about an atmospheric pressure, will hear behind the process 20-30min that the cracker of alloy and the temperature of container raise, this is to form hydride behind the absorption hydrogen and explosion vacuumizes dehydrogenase 12-10h at 400-600 ℃ then.The airflow milling flouring technology is to utilize air-flow that powder particle is accelerated to supersonic speed to make it head-on collision mutually and fragmentation.
The particular content of above technology is seen Zhou Shouzeng, Dong Qingfei " superpower permanet magnetic body---rare-earth system permanent magnetic material " Beijing, metallurgical industry publishing house, 2004.2 second editions, p159-164, p498-504, p326-332, p508-511, p169-172 respectively.
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
80.31B
5.73(Dy
0.32Al
0.24Nb
0.28) (at%), crystal-boundary phase alloy adopts 20m/s fast quenching speed to be prepared into rapid tempering belt, composition is Nd
17.2Fe
75.04B
6.38Dy
0.64Ga
0.2Cu
0.54(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 μ m then by airflow milling.
3) in the crystal-boundary phase alloy powder, add account for its weight 10%, through the nanometer Al of dispersion treatment
2O
3Powder (average particulate diameter is 30nm), and 3% antioxidant polyethylene oxide alkyl ethers, evenly mixed in batch mixer.
4) will be through nanometer Al
2O
3The crystal-boundary phase alloy powder that mixes mixes with the main-phase alloy powder, makes its weight account for 8% of total weight, adds 1% gasoline simultaneously, is uniformly mixed into mixed-powder in batch mixer.
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 600 ℃ 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 8% composition mixed-powder, but do not add nanometer Al
2O
3, adopt identical magnetic field orientating die mould and sintering, tempering process to be prepared into magnet.
8) in addition, with the single alloy Nd of rapid hardening thin slice prepared
13.42Fe
79.87B
5.82(Dy
0.35Al
0.22Nb
0.26Ga
0.02Cu
0.04) (at%), promptly crystal-boundary phase alloy and main-phase alloy are by weight the composition of being formed at 8: 92, copper roller linear resonance surface velocity is 1.2m/s.Make the powder that average particulate diameter is 3 μ m by jaw crusher, middle disintegrating machine and airflow milling respectively.Add 1% gasoline, evenly mix after 0.24% the antioxidant polyethylene oxide alkyl ethers, in identical magnetic field orientating die mould and sintering, tempering process, be prepared into magnet.
Adopt the magnetic property of characteristic of magnetization automatic measuring instrument AMF measurement magnet, performance such as table one.
Table one, the magnet performance that adopts different process to prepare
| Preparation technology | ??B r(kGs) | ??H cj(kOe) | ??(BH) max(MGOe) |
| Single alloy technique | ???13.52 | ???11.3 | ????42.13 |
| The pairing gold process does not add nanometer Al 2O 3 | ???13.50 | ???12.08 | ????42.56 |
| The pairing gold process adds nanometer Al 2O 3 | ???13.49 | ???14.21 | ????43.22 |
Therefrom as can be seen, adopt the pairing gold process to add nanometer Al
2O
3Make the sintered NdFeB coercive force and do not add nano-oxide and make magnet coercive force height, more make magnet coercive force height, therefore add nanometer Al by the pairing gold process than single alloyage than adopting the pairing gold process
2O
3Can prepare the sintered NdFeB of high-coercive force.
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
78.13B
5.81(Tb
0.21Al
0.24Co
1.12Nb
0.28) (at%), crystal-boundary phase alloy adopts 18m/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 10%, through the nanometer SiO of dispersion treatment
2Powder (average particulate diameter is 10nm), and 4% antioxidant poly(ethylene oxide) mono fatty acid ester, evenly mixed in batch mixer.
4) will be through nanometer SiO
2The crystal-boundary phase alloy powder that mixes mixes with the main-phase alloy powder, makes its weight account for 5% of total weight, adds 1.2% gasoline simultaneously, is uniformly mixed into mixed-powder in batch mixer.
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, 1070 ℃ of sintering 3h, and 510 ℃ 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 nanometer SiO
2, adopt identical magnetic field orientating die mould and sintering, tempering process to be prepared into magnet.
8) in addition, with the single alloy Nd of rapid hardening thin slice prepared
14.48Fe
77.77B
5.89(Tb
0.2Dy
0.04Al
0.25Co
1.07Nb
0.27Ga
0.01Cu
0.02) (at%), promptly crystal-boundary phase alloy and main-phase alloy are by weight the composition of being formed at 5: 95, copper roller linear resonance surface velocity is 2.0m/s.Make the powder that average particulate diameter is 3.3 μ m by jaw crusher, middle disintegrating machine and airflow milling respectively.Add 1.2% gasoline, evenly mix behind 0.2% the antioxidant poly(ethylene oxide) mono fatty acid ester, in identical magnetic field orientating die mould and sintering, tempering process, be prepared into magnet.
Adopt the magnetic property of characteristic of magnetization automatic measuring instrument AMF measurement magnet, performance such as table two.
Table two, the magnet performance that adopts different process to prepare
| Preparation technology | ??B r(kGs) | ???H cj(kOe) | ???(BH) max(MGOe) |
| Single alloy technique | ????12.15 | ????15.81 | ??????35.51 |
| The pairing gold process does not add nanometer SiO 2 | ????12.05 | ????16.58 | ??????37.36 |
| The pairing gold process adds nanometer SiO 2 | ????12.02 | ????17.02 | ??????38.43 |
Therefrom as can be seen, adopt the pairing gold process to add nanometer SiO
2Make the sintered NdFeB coercive force and do not add nano-oxide and make magnet coercive force height, also make magnet coercive force height, therefore add nanometer SiO by the pairing gold process than single alloyage than adopting the pairing gold process
2Can prepare the sintered NdFeB of high-coercive force.
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 2.2m/s, and composition is Nd
11.06Fe
82.25B
5.9Dy
0.79(at%), adopt the fast quenching technology, with crystal-boundary phase alloy Nd
27.83Fe
56.2B
6.68Dy
2.47Co
6.82(at%) be prepared into rapid tempering belt, fast quenching speed 18m/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 nanometer SiO that accounts for its weight 5% through dispersion treatment
2Powder (average particulate diameter is 10nm), 5% nanometer ZrO
2Powder (average particulate diameter is 20nm), and 1% antioxidant polyethylene oxide alkyl ethers, evenly mixed in batch mixer.
4) will be through nanometer SiO
2, ZrO
2The crystal-boundary phase alloy powder that powder mixes mixes with the main-phase alloy powder, makes its weight account for 18% of alloy total weight, adds 2% gasoline simultaneously, is uniformly mixed into mixed-powder in batch mixer.
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, 1065 ℃ of sintering 4.5h, and 560 ℃ of tempering heat treatment 3h make sintered magnet again.
Adopt the magnetic property of characteristic of magnetization automatic measuring instrument AMF measurement magnet, performance such as table three.
Table three. adopt the pairing gold process to add nanometer SiO
2, ZrO
2The magnet performance of preparation
| Preparation technology | ????B r(kGs) | ???H cj(kOe) | (BH) max(MGOe) |
| The pairing gold process adds nanometer SiO 2、ZrO 2 | ????12.20 | ????16.53 | ????37.18 |
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
12.59Fe
81.32B
5.7Dy
0.4(at%), crystal-boundary phase alloy adopts 18m/s fast quenching speed to be prepared into rapid tempering belt, and composition is Nd
23.74Fe
64.78B
6.89(Dy
0.92Co
1.27Cu
0.35Nb
0.4Al
1.66) (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 3.5 μ m by airflow milling then under nitrogen protection.
3) in the crystal-boundary phase alloy powder, add the nanometer SiO that accounts for its weight 5% through dispersion treatment
2Powder (average particulate diameter is 10nm), 3% nanometer Al
2O
3Powder (average particulate diameter is 30nm), and 1% antioxidant poly(ethylene oxide) allyl ether, evenly mixed in batch mixer.
4) will be through nanometer SiO
2, Al
2O
3The crystal-boundary phase alloy powder that mixes mixes with the main-phase alloy powder, makes its weight account for 20% of total weight, adds 2% gasoline simultaneously, is uniformly mixed into mixed-powder in batch mixer.
4) 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.
5) 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.
Adopt the magnetic property of characteristic of magnetization automatic measuring instrument AMF measurement magnet, performance such as table five.
Table five adopts the pairing gold process to add nanometer SiO
2, Al
2O
3The magnet performance of preparation
| Preparation technology | ??B r(kGs) | ???H cj(kOe) | ????BH) max(MGOe) |
| The pairing gold process adds nanometer SiO 2、Al 2O 3 | ????13.2 | ????14.69 | ?????42.38 |
Claims (5)
1. the middle mutually nano-oxide that adds of crystal boundary improves sintered NdFeB coercive force method, it 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, and 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;
2) adopt the quick-fried method of hydrogen or by alloy of ingot, rapid hardening thin slice or the rapid tempering belt fragmentation of disintegrating machine with alloy of ingot or the rapid hardening thin slice and the crystal-boundary phase alloy of main-phase alloy, broken back is by the airflow milling abrasive material, making average particulate diameter respectively is 2-10 μ m powder;
3) in the crystal-boundary phase alloy powder, add account for its weight 2-20%, through the nano-oxide of dispersion treatment, and the antioxidant of 1-10%, evenly mixed in batch mixer;
4) will mix with the main-phase alloy powder through the crystal-boundary phase alloy powder that nano-oxide mixes, 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;
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.
2. the middle mutually nano-oxide that adds of crystal boundary according to claim 1 improves sintered NdFeB coercive force method, it is characterized in that its composition of said main-phase alloy 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.
3. the middle mutually nano-oxide that adds of crystal boundary according to claim 1 improves sintered NdFeB coercive force method, it is characterized in that its composition of said crystal-boundary phase alloy is Nd
dFe
100-d-e-fB
eR
f(at%), 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 middle mutually nano-oxide that adds of crystal boundary according to claim 1 improves sintered NdFeB coercive force method, it is characterized in that said nano-oxide is SiO
2, ZrO
2, CuO, Fe
2O
3, Al
2O
3, Y
2O
3, TiO
2In one or more, average particulate diameter is 2-40nm.
5. crystal boundary according to claim 1 adds nano-oxide in mutually and improves sintered NdFeB coercive force method, it is characterized in that said 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.
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