CN101266857A - Method for improving sintered neodymium-iron-boron coercive force and working temperature based on nano Ti powder modification - Google Patents

Method for improving sintered neodymium-iron-boron coercive force and working temperature based on nano Ti powder modification Download PDF

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CN101266857A
CN101266857A CNA2007101160826A CN200710116082A CN101266857A CN 101266857 A CN101266857 A CN 101266857A CN A2007101160826 A CNA2007101160826 A CN A2007101160826A CN 200710116082 A CN200710116082 A CN 200710116082A CN 101266857 A CN101266857 A CN 101266857A
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phase alloy
powder
crystal
nano titanium
coercive force
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于濂清
薛庆忠
郭文跃
郝兰众
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China University of Petroleum East China
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China University of Petroleum East China
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Abstract

The invention discloses a method for improving coercive force and working temperature of sintering neodymium ferroboron by nanometer titanium powder modification, comprising the steps that: 1) a main phase alloy metal adopts a casting procedure to manufacture neodymium ferroboron ingot casting or adopts a rapid hardening slice procedure to manufacture the neodymium ferroboron rapid hardening slice, a crystal boundary phase alloy adopts the cast procedure to manufacture the ingot casting alloy or the rapid hardening slice procedure to manufacture the rapid hardening slice or rapid quenching procedure to manufacture a rapid quenching strip; 2) respectively manufacturing the main phase alloy and the crystal boundary phase alloy to the powder; 3) adding the nanometer titanium powder into the crystal boundary phase alloy powder to mix up; 4) after being mixed up, forming the main phase alloy and the crystal boundary phase alloy powder by pressing in the magnet; 5) manufacturing the sintering magnet in a high vacuum sintering furnace. The sintering neodymium ferroboron manufactured by the invention has the high coercive force and working temperature, the procedure can be used for mass bulk production, and the sintering neodymium ferroboron with high coercive force and high working temperature can be prepared through the invention.

Description

Modifying nano titanium powder improves sintered NdFeB coercive force and working temperature method
Technical field
The present invention relates to a kind of modifying nano titanium powder and improve sintered NdFeB coercive force and working temperature method.
Background technology
The new beginning in rare earth permanent magnet field has been opened up in the appearance of rare-earth Nd-Fe-B series permanent magnetic material.Nd-Fe-B rare earth permanent magnetic material is that people such as 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, 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 specially adapted to develop the various regeneration products of high-performance, miniaturization, lightness with in the device and equipment of permanent-magnetic field.
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 T cThe 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 JX, (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 2For improving the working temperature of NdFeB permanent magnetic material, people are addition element Co in magnet usually.Discover, in Co content is 0～10at% scope, T cImprove every basically increase 1at%Co, T along straight line with the increase of Co content is approximate cImprove 10.9 ℃.But find simultaneously, after adding Co, the coercive force of magnet reduces, this is because Co has formed the soft magnetism phase on crystal boundary, the easy forming core in magnetic reversal farmland under the opposing magnetic field, reduce the coercive force of magnet, improve coercitive alloying element, improve the coercive force of alloy as elements such as Dy, Tb, Al, Nb, Ga so add simultaneously in the magnet.Therefore, improve the neodymium iron boron magnetic body working temperature and just be summed up as the coercive force that improves neodymium iron boron magnetic body to a great extent.
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.The coercive force H of neodymium iron boron magnetic body is described cThe following empirical equation of general employing,
H c＝αH k-N effM s
H kThe expression magnetic moment is consistent to rotate needed anisotropy field, and α represents that the grainiess defective is to the coercitive minimizing factor, N EffThe coupling of expression crystal grain self-heating demagnetizing effect and intergranule interacts and effective demagnetizing factor of formation, M SExpression magnet saturation magnetization.This shows that 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.Two alloyages 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 made principal phase more reasonable with crystal boundary composition mutually, can obtain higher H Cj
The invention provides a kind of new method and utilize the pairing gold process, add coercive force and working temperature that nano titanium powder improves sintered NdFeB.Main-phase alloy and crystal-boundary phase alloy are prepared respectively, by add nano titanium powder in crystal boundary mutually in, and, make the non magnetic crystal boundary that is mixed with nano titanium powder be dispersed in principal phase Nd mutually by adding lubricant, antioxidant 2Fe 14B grain surface layer because the titanium fusing point is higher, has played the effect that hinders grain growth, crystal grain thinning has suppressed the exchange-coupling interaction between the hard magnetic phase simultaneously, has improved microstructure, thereby improved the coercive force of magnet, also improved the working temperature of magnet simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of modifying nano titanium powder and improve sintered NdFeB coercive force and working temperature 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 titanium powder of 2-20 weight portion, the antioxidant of 1-10 weight portion, the evenly mixed crystal-boundary phase alloy powder that obtains modifying nano titanium powder in batch mixer;
4) will be uniformly mixed into mixed-powder in batch mixer through crystal-boundary phase alloy powder and main-phase alloy powder, the gasoline of modifying nano titanium powder, wherein the crystal-boundary phase alloy powder weight of modifying nano titanium powder 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, N, Al, Cu, the Si element one or more.The nano titanium powder average particulate diameter is 2-100nm.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 titanium powder than adopting the pairing gold process and makes magnet coercive force, working temperature height, 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 nano titanium powder is 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 modifying nano titanium powder is dispersed in principal phase Nd 2Fe 14The effect that hinders grain growth has been played in the B grain boundary, refinement crystal grain, simultaneously, effectively cut off the exchange-coupling interaction of hard magnetic between mutually, improve microstructure, thereby improve magnet coercive force and working temperature.
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 titanium powder of 2-20 weight portion, the antioxidant of 1-10 weight portion, the evenly mixed crystal-boundary phase alloy powder that obtains modifying nano titanium powder 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 modifying nano titanium powder, 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 titanium powder average particulate diameter is 2-100nm.
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 80.69B 5.73(Dy 0.22Al 0.24) (at%), crystal-boundary phase alloy adopts 18m/s fast quenching speed to be prepared into rapid tempering belt, composition is Nd 17.2Fe 75.58B 6.388Dy 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 3.0 μ m then by airflow milling.
3) in the crystal-boundary phase alloy powder, add account for its weight 3.4%, through the nano titanium powder end of dispersion treatment (average particulate diameter is 30nm), 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 modifying nano titanium powder, make its weight account for 8% 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 8% composition mixed-powder, but do not add nano titanium powder, adopt identical magnetic field orientating die mould and sintering, tempering process to 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) Maximum operating temperature (℃)
The pairing gold process does not add nanometer Ti 13.84 12.68 46.12 80
The pairing gold process adds nanometer Ti 13.80 14.81 47.62 100
As can be seen from the table, adopt pairing gold process interpolation nano titanium powder to make the sintered NdFeB coercive force and do not make magnet coercive force height, working temperature height, therefore add the sintered NdFeB that nano titanium powder can be prepared high-coercive force, elevated operating temperature by the pairing gold process than not adding nano titanium powder.
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 77.15B 5.81(Tb 0.31Al 0.24Co 2Nb 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 75.27B 6.31(Dy 1.84Ga 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 nano titanium powder end of dispersion treatment (average particulate diameter is 5nm), 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 modifying nano titanium powder, 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, 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 nano titanium powder, adopt identical magnetic field orientating die mould and sintering, tempering process to 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) Maximum operating temperature (℃)
The pairing gold process does not add nanometer Ti 12.32 22.64 34.04 150
The pairing gold process adds nanometer Ti 11.67 29.52 30.62 200
As can be seen from the table, adopt pairing gold process interpolation nano titanium powder to make the sintered NdFeB coercive force and do not make magnet coercive force height, working temperature height, therefore add the sintered NdFeB that nano titanium powder can be prepared high-coercive force, elevated operating temperature by the pairing gold process than not adding nano titanium powder.
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 11.56Fe 81.75B 5.9Dy 0.99(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 3.3 μ m then by airflow milling.
3) in the crystal-boundary phase alloy powder, add the nano titanium powder end (average particulate diameter is 70nm) that accounts for its weight 5% 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 titanium powder end modification, make its weight account for 18% 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, 1065 ℃ 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 18% composition mixed-powder, but do not add nano titanium powder, adopt identical magnetic field orientating die mould and sintering, tempering process to be prepared into magnet.
Adopt the magnetic property of characteristic of magnetization automatic measuring instrument AMF measurement magnet, performance such as table three.
Table three, the magnet performance that adopts different process to prepare
Preparation technology B r (kGs) H cj (kOe) (BH) max (MGOe) Maximum operating temperature (℃)
The pairing gold process does not add nanometer Ti 13.21 14.28 37.12 100
The pairing gold process adds nanometer Ti 13.23 17.53 40.41 120
As can be seen from the table, adopt pairing gold process interpolation nano titanium powder to make the sintered NdFeB coercive force and do not make magnet coercive force height, working temperature height, therefore add the sintered NdFeB that nano titanium powder can be prepared high-coercive force, elevated operating temperature by the pairing gold process than not adding nano titanium powder.
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 80.42B 5.7Dy 1.4(at%), crystal-boundary phase alloy adopts 21m/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 7 μ m by airflow milling then under nitrogen protection.
3) in the crystal-boundary phase alloy powder, add the nano titanium powder end (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 modifying nano titanium powder, make its weight account for 15% 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 610 ℃ 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 15% composition mixed-powder, but do not add nano titanium powder, adopt identical magnetic field orientating die mould and sintering, tempering process to be prepared into magnet.
Adopt the magnetic property of characteristic of magnetization automatic measuring instrument AMF measurement magnet, performance such as table four.
Table four, the magnet performance that adopts different process to prepare
Preparation technology B r (kGs) H cj (kOe) (BH) max (MGOe) Maximum operating temperature (℃)
The pairing gold process does not add nanometer Ti 13.45 12.75 38.22 80
The pairing gold process adds nanometer Ti 13.40 17.44 39.63 120
As can be seen from the table, adopt pairing gold process interpolation nano titanium powder to make the sintered NdFeB coercive force and do not make magnet coercive force height, working temperature height, therefore add the sintered NdFeB that nano titanium powder can be prepared high-coercive force, elevated operating temperature by the pairing gold process than not adding nano titanium powder.
Embodiment 5:
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 2m/s, and composition is Nd 13.12Fe 80.69B 5.73(Dy 0.3Al 0.16) (at%), crystal-boundary phase alloy adopts 18m/s fast quenching speed to be prepared into rapid tempering belt, composition is Nd 18.2Fe 74.48B 6.38Dy 0.64Co 0.3(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 3.5 μ m then by airflow milling.
3) in the crystal-boundary phase alloy powder, add account for its weight 10%, through the nano titanium powder end of dispersion treatment (average particulate diameter is 20nm), 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 modifying nano titanium powder, make its weight account for 6% 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 6% composition mixed-powder, but do not add nano titanium powder, adopt identical magnetic field orientating die mould and sintering, tempering process to be prepared into magnet.
Adopt the magnetic property of characteristic of magnetization automatic measuring instrument AMF measurement magnet, performance such as table five.
Table five, the magnet performance that adopts different process to prepare
Preparation technology B r (kGs) H cj (kOe) (BH) max (MGOe) Maximum operating temperature (℃)
The pairing gold process does not add nanometer Ti 13.68 13.88 45.72 80
The pairing gold process adds nanometer Ti 13.71 15.92 46.68 100
As can be seen from the table, adopt pairing gold process interpolation nano titanium powder to make the sintered NdFeB coercive force and do not make magnet coercive force height, working temperature height, therefore add the sintered NdFeB that nano titanium powder can be prepared high-coercive force, elevated operating temperature by the pairing gold process than not adding nano titanium powder.

Claims (5)

1. a modifying nano titanium powder improves sintered NdFeB coercive force and working temperature 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, 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 titanium powder of 2-20 weight portion, the antioxidant of 1-10 weight portion, the evenly mixed crystal-boundary phase alloy powder that obtains modifying nano titanium powder in batch mixer;
4) will be uniformly mixed into mixed-powder in batch mixer through crystal-boundary phase alloy powder and main-phase alloy powder, the gasoline of modifying nano titanium powder, wherein the crystal-boundary phase alloy powder weight of modifying nano titanium powder 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.
2. modifying nano titanium powder according to claim 1 improves sintered NdFeB coercive force and working temperature method, it 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. modifying nano titanium powder according to claim 1 improves sintered NdFeB coercive force and working temperature method, it 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, N, Al, Cu, the Si element one or more.
4. modifying nano titanium powder according to claim 1 improves sintered NdFeB coercive force and working temperature method, it is characterized in that described nano titanium powder average particulate diameter is 2-100nm.
5. modifying nano titanium powder according to claim 1 improves sintered NdFeB coercive force and working temperature method, it is characterized in that described antioxidant is polyethylene oxide alkyl ethers, poly(ethylene oxide) mono fatty acid ester or poly(ethylene oxide) allyl ether.
CNA2007101160826A 2007-12-24 2007-12-24 Method for improving sintered neodymium-iron-boron coercive force and working temperature based on nano Ti powder modification Pending CN101266857A (en)

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WO2012048654A1 (en) * 2010-10-15 2012-04-19 中国科学院宁波材料技术与工程研究所 High-corrosion resistant sintered ndfeb magnet and preparation method therefor
CN103870644A (en) * 2014-03-11 2014-06-18 中国石油大学(华东) Method for identifying MoP catalyst denitrification active sites
WO2014101247A1 (en) * 2012-12-26 2014-07-03 宁波韵升股份有限公司 Method for preparing sintered neodymium-iron-boron magnet
CN104981883A (en) * 2012-11-23 2015-10-14 罗伯特·博世有限公司 Magnetic material and method for producing same
CN105513735A (en) * 2016-01-08 2016-04-20 宁波宏垒磁业有限公司 High-performance sintered neodymium-iron-boron magnet
CN105513736A (en) * 2016-01-08 2016-04-20 宁波宏垒磁业有限公司 Sintered neodymium-iron-boron magnet
WO2016086397A1 (en) * 2014-12-04 2016-06-09 浙江大学 Method for improving coercive force of sintered neodymium iron boron magnet by adding dysprosium hydrogen compound and product
CN105845303A (en) * 2016-01-08 2016-08-10 宁波宏垒磁业有限公司 Preparation method of sintered Nd-Fe-B magnet with high performance
CN105845302A (en) * 2016-01-08 2016-08-10 宁波宏垒磁业有限公司 Preparation method of sintered Nd-Fe-B magnet
CN105845425A (en) * 2016-01-08 2016-08-10 宁波宏垒磁业有限公司 Preparation method of Nd-Fe-B magnet
CN110428947A (en) * 2019-07-31 2019-11-08 厦门钨业股份有限公司 A kind of rare earth permanent-magnetic material and its feedstock composition, preparation method and application
CN114899004A (en) * 2022-06-01 2022-08-12 宁波铄腾新材料有限公司 Multiphase coupling method and apparatus for preparing high abundance cerium magnet N38SH

Cited By (16)

* Cited by examiner, † Cited by third party
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WO2012048654A1 (en) * 2010-10-15 2012-04-19 中国科学院宁波材料技术与工程研究所 High-corrosion resistant sintered ndfeb magnet and preparation method therefor
CN104981883A (en) * 2012-11-23 2015-10-14 罗伯特·博世有限公司 Magnetic material and method for producing same
CN104981883B (en) * 2012-11-23 2018-08-17 罗伯特·博世有限公司 Magnetic material and the method manufactured for it
WO2014101247A1 (en) * 2012-12-26 2014-07-03 宁波韵升股份有限公司 Method for preparing sintered neodymium-iron-boron magnet
CN103870644B (en) * 2014-03-11 2016-08-03 中国石油大学(华东) A kind of method identifying MoP catalyst Deitrogenatin active sites
CN103870644A (en) * 2014-03-11 2014-06-18 中国石油大学(华东) Method for identifying MoP catalyst denitrification active sites
WO2016086397A1 (en) * 2014-12-04 2016-06-09 浙江大学 Method for improving coercive force of sintered neodymium iron boron magnet by adding dysprosium hydrogen compound and product
CN105845303A (en) * 2016-01-08 2016-08-10 宁波宏垒磁业有限公司 Preparation method of sintered Nd-Fe-B magnet with high performance
CN105513736A (en) * 2016-01-08 2016-04-20 宁波宏垒磁业有限公司 Sintered neodymium-iron-boron magnet
CN105845302A (en) * 2016-01-08 2016-08-10 宁波宏垒磁业有限公司 Preparation method of sintered Nd-Fe-B magnet
CN105845425A (en) * 2016-01-08 2016-08-10 宁波宏垒磁业有限公司 Preparation method of Nd-Fe-B magnet
CN105513735A (en) * 2016-01-08 2016-04-20 宁波宏垒磁业有限公司 High-performance sintered neodymium-iron-boron magnet
CN110428947A (en) * 2019-07-31 2019-11-08 厦门钨业股份有限公司 A kind of rare earth permanent-magnetic material and its feedstock composition, preparation method and application
CN110428947B (en) * 2019-07-31 2020-09-29 厦门钨业股份有限公司 Rare earth permanent magnetic material and raw material composition, preparation method and application thereof
EP3940720A4 (en) * 2019-07-31 2022-06-08 Xiamen Tungsten Co. Ltd. Rare earth permanent magnet material and raw material composition, preparation method therefor and use thereof
CN114899004A (en) * 2022-06-01 2022-08-12 宁波铄腾新材料有限公司 Multiphase coupling method and apparatus for preparing high abundance cerium magnet N38SH

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