CN104143403A - Manufacturing method for improving magnetic performance of sintered neodymium-iron-boron magnet - Google Patents
Manufacturing method for improving magnetic performance of sintered neodymium-iron-boron magnet Download PDFInfo
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- CN104143403A CN104143403A CN201410372680.XA CN201410372680A CN104143403A CN 104143403 A CN104143403 A CN 104143403A CN 201410372680 A CN201410372680 A CN 201410372680A CN 104143403 A CN104143403 A CN 104143403A
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Abstract
A high-magnetism sintered neodymium-iron-boron magnet is characterized by comprising, by weight, 27-31% of rare earth elements, 0.9-1.2% of boron, 0-3.0% of cobalt, 0-2% of adding elements and the balance iron, the rare earth elements comprise two or more of neodymium, praseodymium, dysprosium, terbium and holmium, and the adding elements comprise two or more of aluminum, copper, gallium, niobium, zirconium, titanium and hafnium. A manufacturing method includes the working procedures of batching, smelting, hydrogen breaking, pulverizing, forming and sintering, and argon protection is selected for replacing nitrogen protection in the working procedures from smelting to sintering, so that the content of nitrogen in the sintered neodymium-iron-boron magnet is reduced substantially, the total quantity of the rare earth elements in the magnet is relatively stable, the coercivity of the magnet is improved, and the magnetic performance is kept well. A magnet crystal boundary structure change caused by the nitrogen does not exist in the production process, and the corrosion-resistant capacity of the sintered magnet is improved.
Description
Technical field
The present invention relates to sintered neodymium iron boron material and preparation method thereof, particularly about a kind of preparation method who improves sintered NdFeB magnetic property.
Background technology
In sintered neodymium iron boron material preparation process, inevitably bring the impurity elements such as C, O, N into.If these impurity contents are too high, can cause magnet performance to worsen.Current research all concentrates on how to reduce and control oxygen content in Sintered NdFeB magnet and ensures magnet performance.In hot conditions, after neodymium iron boron powder attenuates, N element can react with Sintered NdFeB magnet rare earth elements, particularly in the time that magnet total amount of rare earth is lower, magnet rare earth elements after oxidized again with nitrogen element reaction, can cause in magnet pure rare earth constituent content too low, can cause like this magnet coercive force to decline, in magnet, bringing into of nitrogen element causes that magnet grain boundary structure changes and causes magnet resistance to corrosion to decline, the magnet making according to existing preparation method, nitrogen content is all in about 500PPm, and what have even exceedes 1500PPm.Therefore, the content of control impurity element nitrogen is also the importance of preparing high-performance permanent magnet.
Summary of the invention
The present invention is directed to and affect sintered NdFeB magnetic property stable problem, put forward a kind of its manufacture method of formula of improving.
A kind of high magnetic sintered NdFeB, it is characterized in that forming percentage by weight: rare earth element is 27～31, boron is 0.9～1.2, cobalt is 0～3.0, add that element is 0～2, surplus is iron, wherein: rare earth element is two or more in neodymium, praseodymium, dysprosium, terbium and holmium, interpolation element is two or more in aluminium, copper, gallium, niobium, zirconium, titanium and hafnium.
A preparation method for high magnetic characteristics sintered NdFeB, comprises the following steps:
1) batching: press product composition composition percentage by weight batching, wherein the Fe in BFe alloy, DyFe alloy, NdFe alloy accounts for a part for Fe total amount;
2) melting: adopt strip casting melting, when casting, copper/molybdenum roller rotating speed of smelting furnace is controlled at 1.0～1.8m/s, between 1430～1460 DEG C of cast temperatures, slab casting and coolingly all adopt the protection of inert gas-0.02～-0.03Mpa negative pressure;
3) hydrogen is broken: above-mentioned slab is put into hydrogen broken furnace and carry out hydrogen fragmentation, make the broken powder of hydrogen that granularity is less than 500 μ m, hydrogen content is controlled at below 800PPm, and when the broken powder discharging of hydrogen, logical inert gas flow pressure is 0.005～0.01Mpa protection discharging;
4) powder process: it is the powder process of 0.5～0.7MPa airflow milling that broken above-mentioned hydrogen powder is put into inert gas flow pressure, obtain the powder of particle size 2～5 μ m, be to stir with protective agent under 0.03～0.06MPa protection at inert gas pressure, logical inert gas gas pressure 0.01～0.05Mpa protection when holding vessel stores;
5) moulding: adopt inert gas shielding magnetic to enter mould molding, in formed gloves case, inert gas flow is controlled at 5～20m
3/ h, Control for Oxygen Content≤0.05% quality;
6) sintering: first adopt inert gas shielding to go out module and enter stove, enter inert gas flow in stove glove box and be controlled at 15～50m
3/ h, Control for Oxygen Content is in≤0.02% quality; Sintering furnace is vacuumized, the vacuum degree control of sintering furnace is 4 × 10 again
-2below Pa, when sintering is cooling, adopt inert gas pressure to be controlled at 0.04～0.02Mpa cooling protection.
Above-mentioned inert gas comprises Ar, He gas, but adopts Ar gas from cost consideration.
With nitrogen content in neodymium iron boron magnetic body after the molding neodymium iron boron sintering of Ar Buchholz protection be 80～200PPm.
The invention has the beneficial effects as follows: by adding rare earth element and other metallic elements, with raising sintered NdFeB magnetic stability time, in melting, hydrogen is broken, powder process, moulding, in operation prepared by the neodymium iron borons such as sintering, utilize existing equipment, adopt inert gas shielding to substitute traditional nitrogen protection, under high-temperature condition, prevent rare earth element and nitrogen generation chemical reaction, particularly powder process adopts inert gas to substitute traditional nitrogen powder process, stop a large amount of nitrogen of fine powder Surface absorption, reduce reacting of rare earth element and nitrogen, make that Sintered NdFeB magnet is nitrogenous to decline to a great extent, thereby make magnet rare earth elements total amount relatively stable, improve magnet coercive force, it is good that magnetic property keeps.Do not exist in process of production nitrogen element to cause that magnet grain boundary structure changes, and has improved the resistance to corrosion of sintered magnet.
Embodiment
Below in conjunction with embodiment, the present invention is elaborated.
Raw material selection: inert gas selects that purity of argon is 99.99%, boron is that ferro-boron, dysprosium are that Dy-Fe alloy, praseodymium are that praseodymium neodymium alloy, niobium are ferrocolumbium; be commercially available intermediate alloy; all the other metallic elements are commercially available buying technical pure metal, and the protective agent adding when powder process is commercially available poly(ethylene oxide) allyl ether or poly(ethylene oxide) allyl glycidyl ether.
Fabrication apparatus thereof is for utilizing existing sintered NdFeB production equipment.
Embodiment mono-
1) batching: adopt pure Nd, Co, Cu, Al, Fe and DyFe(Dy:80wt%, Fe:20wt%), BFe(B:20wt%, Fe:80wt%) press Nd
28.7dy
0.5co
0.5cu
0.2al
0.2b
1.0fe
more thancomposition (percentage by weight) is prepared burden;
2) melting: adopt strip casting to carry out melting, when casting, copper/molybdenum roller speed setting of smelting furnace is 1.6m/s, 1435 DEG C of cast temperatures, casting and cooling employing Ar atmospheric pressure are the protection of-0.02～-0.03Mpa negative pressure;
3) hydrogen is broken: above-mentioned slab is put into hydrogen broken furnace, and to carry out hydrogen broken, granularity control≤500 μ m, and powder hydrogen content≤800PPm, the broken powder discharging of hydrogen adopts the protection of Ar gas, and Ar stream pressure is 0.01MPa;
4) powder process: the airflow milling powder process that broken above-mentioned hydrogen powder is put into argon stream pressure 0.5～0.7Mpa, obtain particle size 2-5 μ m, adopting Ar atmospheric pressure is to stir with protective agent under 0.05Mpa, enters the logical Ar stream pressure 0.05MPa of holding vessel and stores;
5) moulding: adopt Ar gas protection magnetic to enter mould molding, glove box Ar throughput control 15m
3/ h, oxygen content≤0.05%;
6) sintering: first adopt Ar gas to protect into stove, glove box Ar throughput is 40m
3/ h, oxygen content≤0.02%, then vacuumize sintering, vacuum degree≤4 × 10
-2pa, the Ar gas at-0.02MPa when sintering is cooling is protected cooling product.
The NdFeB material magnetic property that employing said method makes is after testing as shown in table 1A; the composition and ratio of comparative example 1 is identical with embodiment 1; compared with the Sintered NdFeB magnet that adopts the technique of traditional nitrogen protection to make, nitrogen content significantly reduces, and magnetic property, density all have a distinct increment.
Table 1A
Corrosion resistance is (test condition: 121 degrees Celsius, 100% humidity, under 2.7 atmospheric pressure) after testing, and weightless data are as shown in table 1B:
Table 1B
As seen from the above table, adopt inert gas shielding less than the Nd-Fe-B magnet steel weightlessness that adopts nitrogen protection to prepare, illustrate that its corrosion resistance is good.
Embodiment bis-
Embodiment 2:
1) batching: adopt PrNd(Nd:75wt%, Pr:25wt%), pure Co, Cu, Al, Ga, Fe and BFe(B:20wt%, Fe:80wt%) press Nd
22.5pr
7.5co
1.0cu
0.2al
0.4ga
0.2b
1.0fe
more thancomposition (percentage by weight) is prepared burden:
2) melting: adopt strip casting to carry out melting, when casting, copper/molybdenum roller speed setting of smelting furnace is 1.4m/s, 1445 DEG C of cast temperatures, casting and cooling employing Ar atmospheric pressure are the protection of-0.02～-0.03Mpa negative pressure;
3) hydrogen is broken: above-mentioned slab is put into hydrogen broken furnace, and to carry out hydrogen broken, granularity control≤500 μ m, and powder hydrogen content≤800PPm, the broken powder discharging of hydrogen adopts the protection of Ar gas, and Ar stream pressure is 0.01MPa;
4) powder process: broken above-mentioned hydrogen powder is put into the airflow milling powder process that argon gas stream pressure is 0.5～0.7Mpa, obtain particle size 2～5 μ m, adopting Ar atmospheric pressure is to stir with protective agent under 0.05Mpa, enters the logical Ar stream pressure 0.03MPa of holding vessel and stores;
5) moulding: adopt Ar gas protection magnetic to enter mould molding, glove box Ar throughput control 15m
3/ h, oxygen content≤0.05%;
6) sintering: first adopt Ar gas to protect into stove, glove box Ar throughput is 40m
3/ h, oxygen content≤0.02%, then vacuumize sintering, vacuum degree≤4 × 10
-2pa, the cooling Ar gas at-0.04MPa of sintering is protected cooling product.
The NdFeB material performance that employing said method makes is after testing as shown in table 2A; comparative example 2 ratio of componentss are identical with embodiment 2; compared with the Sintered NdFeB magnet that adopts the technique of traditional nitrogen protection to make, nitrogen content significantly reduces, and magnetic property, density all have a distinct increment.
Table 2A
Corrosion resistance is (test condition: 121 degrees Celsius, 100% humidity, under 2.7 atmospheric pressure) after testing, and weightless data are as shown in table 2B:
Table 2B
As seen from the above table, adopt inert gas shielding less than the Nd-Fe-B magnet steel weightlessness that adopts nitrogen protection to prepare, illustrate that its corrosion resistance is good.
Embodiment tri-
1) batching: adopt pure Nd, Co, Cu, Al, Fe and DyFe (Dy:80wt%, Fe:20 wt %), NbFe (Nb:20wt%, Fe:80 wt %), BFe(B:20wt%, Fe:80 wt %) press Nd
27.8dy
3.2co
3.0cu
0.2al
0.2nb
0.1b
1.02fe
more thancomposition (percentage by weight) is prepared burden:
2) melting: above-mentioned slab is put into hydrogen broken furnace, and to carry out hydrogen broken, adopt strip casting to carry out melting, when casting, copper/molybdenum roller speed setting of smelting furnace is 1.2m/s, 1450 DEG C of cast temperatures, casting and cooling employing Ar atmospheric pressure are the protection of-0.02～-0.03Mpa negative pressure;
3) hydrogen is broken: above-mentioned slab is put into hydrogen broken furnace, and to carry out hydrogen broken, granularity control≤500 μ m, and powder hydrogen content≤800PPm, the broken powder discharging of hydrogen adopts the protection of Ar gas, and Ar stream pressure is 0.01MPa;
4) powder process: broken above-mentioned hydrogen powder is put into the airflow milling powder process that Ar stream pressure is 0.5～0.7Mpa, obtain particle size 2～5 μ m, adopting Ar atmospheric pressure is to stir with protective agent under 0.05Mpa, enters the logical Ar stream pressure 0.01MPa of holding vessel and stores;
5) moulding: adopt Ar gas protection magnetic to enter mould molding, glove box Ar throughput control 10m
3/ h, oxygen content≤0.05%;
6) sintering: first adopt Ar gas to protect into stove, glove box Ar throughput is 35m
3/ h, oxygen content≤0.02%, then vacuumize sintering, vacuum degree≤4 × 10
-2pa, the cooling Ar gas at-0.04MPa of sintering is protected cooling product.
The NdFeB material performance that employing said method makes is after testing as shown in table 3A; the composition and ratio of comparative example 3 is identical with embodiment 3; compared with the Sintered NdFeB magnet that adopts the technique of traditional nitrogen protection to make, nitrogen content significantly reduces, and magnetic property, density all have a distinct increment.
Table 3A
Corrosion resistance is (test condition: 121 degrees Celsius, 100% humidity, under 2.7 atmospheric pressure) after testing, and weightless data are as shown in table 3B:
Table 3B
As seen from the above table, adopt inert gas shielding less than the Nd-Fe-B magnet steel weightlessness that adopts nitrogen protection to prepare, illustrate that its corrosion resistance is good.
Embodiment tetra-
1) batching: adopt pure Nd, Tb, Co, Cu, Al, Fe and BFe(B:20wt%, Fe:80wt%) press Nd
29.5tb
0.5co
0.5cu
0.2al
0.4b
1.02fe
more thancomposition (percentage by weight) is prepared burden;
2) melting: adopt strip casting to carry out melting, when casting, copper/molybdenum roller speed setting of smelting furnace is 1.5m/s, 1440 DEG C of cast temperatures, casting and cooling employing Ar atmospheric pressure are the protection of-0.02～-0.03Mpa negative pressure;
3) hydrogen is broken: above-mentioned slab is put into hydrogen broken furnace, and to carry out hydrogen broken, granularity control≤500 μ m, and powder hydrogen content≤800PPm, the broken powder discharging of hydrogen adopts the protection of Ar gas, and Ar stream pressure is 0.01MPa;
4) powder process: broken above-mentioned hydrogen powder is put into the airflow milling powder process that Ar stream pressure is 0.5～0.7Mpa, obtain particle size 2～5 μ m, adopting Ar atmospheric pressure is to stir with protective agent under 0.05Mpa, enters the logical Ar stream pressure 0.05MPa of holding vessel and stores;
5) moulding: adopt Ar gas protection magnetic to enter mould molding, glove box Ar throughput control 15m
3/ h, oxygen content≤0.05%;
6) sintering: first adopt Ar gas to protect into stove, glove box Ar throughput is 40m
3/ h, oxygen content≤0.02%, then vacuumize sintering, vacuum degree≤4 × 10
-2pa, the cooling Ar gas at-0.02MPa of sintering is protected cooling product.
The NdFeB material magnetic property that employing said method makes is after testing as table 4A; the composition and ratio of comparative example 4 is identical with embodiment 4; compared with the Sintered NdFeB magnet that adopts the technique of traditional nitrogen protection to make, nitrogen content significantly reduces, and magnetic property, density all have a distinct increment.
Table 4A
Corrosion resistance is (test condition: 121 degrees Celsius, 100% humidity, under 2.7 atmospheric pressure) after testing, and weightless data are as shown in table 4B:
Table 4B
As seen from the above table, adopt inert gas shielding less than the Nd-Fe-B magnet steel weightlessness that adopts nitrogen protection to prepare, illustrate that its corrosion resistance is good.
Embodiment five
1) batching: adopt (Pr:25 wt %, Nd:25 wt%) alloy PrNd, Ho, Co, Cu, Al, Fe and BFe(B:20wt%, Fe:80wt%) press Pr
7.5nd
22.5ho
1.0co
1.0cu
0.2al
0.4b
1.02fe
more thancomposition (percentage by weight) is prepared burden;
2) melting: adopt strip casting to carry out melting, when casting, copper/molybdenum roller speed setting of smelting furnace is 1.4m/s, 1450 DEG C of cast temperatures, casting and cooling employing Ar atmospheric pressure are the protection of-0.02～-0.03Mpa negative pressure;
3) hydrogen is broken: above-mentioned slab is put into hydrogen broken furnace, and to carry out hydrogen broken, granularity control≤500 μ m, and powder hydrogen content≤800PPm, the broken powder discharging of hydrogen adopts the protection of Ar gas, and Ar stream pressure is 0.01MPa;
4) powder process: broken above-mentioned hydrogen powder is put into the airflow milling powder process that Ar stream pressure is 0.5～0.7Mpa, obtain particle size 2～5 μ m, adopting Ar atmospheric pressure is to stir with protective agent under 0.05Mpa, enters the logical Ar stream pressure 0.05MPa of holding vessel and stores;
5) moulding: adopt Ar gas protection magnetic to enter mould molding, glove box Ar throughput control 15m
3/ h, oxygen content≤0.05%;
6) sintering: first adopt Ar gas to protect into stove, glove box Ar throughput is 40m
3/ h, oxygen content≤0.02%, then vacuumize sintering, vacuum degree≤4 × 10
-2pa, the cooling Ar gas at-0.02MPa of sintering is protected cooling product.
The NdFeB material magnetic property that employing said method makes is after testing as table 5A; the composition and ratio of comparative example 5 is identical with enforcement 5; compared with the Sintered NdFeB magnet that adopts the technique of traditional nitrogen protection to make, nitrogen content significantly reduces, and magnetic property, density all have a distinct increment.
Table 5A
Corrosion resistance is (test condition: 121 degrees Celsius, 100% humidity, under 2.7 atmospheric pressure) after testing, and weightless data are as shown in table 5B:
Table 5B
As seen from the above table, adopt inert gas shielding less than the Nd-Fe-B magnet steel weightlessness that adopts nitrogen protection to prepare, illustrate that its corrosion resistance is good.
Claims (9)
1. one kind high magnetic sintered NdFeB, it is characterized in that forming percentage by weight: rare earth element is 27～31, boron is 0.9～1.2, cobalt is 0～3.0, add that element is 0～2, surplus is iron, wherein: rare earth element is two or more in neodymium, praseodymium, dysprosium, terbium and holmium, interpolation element is two or more in aluminium, copper, gallium, niobium, zirconium, titanium and hafnium.
2. the high magnetic sintered NdFeB of one according to claim 1, is characterized in that Nd is that 28.7wt%, Dy are that 0.5wt%, Co are that 0.5wt%, Cu are that 0.2wt%, Al are that 0.2wt%, B are that 1.0wt%, surplus are Fe.
3. the high magnetic sintered NdFeB of one according to claim 1, is characterized in that Nd is that 22.5 wt%, Pr are that 7.5 wt%, Co are that 1.0 wt%, Cu are that 0.2 wt%, Al are that 0.4 wt%, Ga are that 0.2 wt%, B are that 1.0 wt%, surplus are Fe.
4. the high magnetic sintered NdFeB of one according to claim 1, is characterized in that Nd is that 27.8 wt%, Dy are that 3.2 wt%, Co are that 3.0 wt%, Cu are that 0.2 wt%, Al are that 0.2 wt%, Nb are that 0.1 wt%, B are that 1.02 wt%, surplus are Fe.
5. the high magnetic sintered NdFeB of one according to claim 1, is characterized in that Nd is that 29.5 wt%, Tb are that 0.5 wt%, Co are that 0.5 wt%, Cu are that 0.2 wt%, Al are that 0.4 wt%, B are that 1.02 wt%, surplus are Fe.
6. the high magnetic sintered NdFeB of one according to claim 1, is characterized in that Pr is that 7.5 wt%, Nd are that 22.5 wt%, Ho are that 1.0 wt%, Co are that 1.0 wt%, Cu are that 0.2 wt%, Al are that 0.4 wt%, B are that 1.02 wt%, surplus are Fe.
7. the preparation method of a kind of high magnetic characteristics sintered NdFeB according to claim 1, its feature comprises the following steps:
1) batching: press product composition composition percentage by weight batching, wherein the Fe in BFe alloy, DyFe alloy, NdFe alloy accounts for a part for Fe total amount;
2) melting: adopt strip casting melting, when casting, copper/molybdenum roller rotating speed of smelting furnace is controlled at 1.0～1.8m/s, between 1430～1460 DEG C of cast temperatures, slab casting and coolingly all adopt the protection of inert gas-0.02～-0.03Mpa negative pressure;
3) hydrogen is broken: above-mentioned slab is put into hydrogen broken furnace and carry out hydrogen fragmentation, make the broken powder of hydrogen that granularity is less than 500 μ m, hydrogen content is controlled at below 800PPm, and when the broken powder discharging of hydrogen, logical inert gas flow pressure is 0.005～0.01Mpa protection discharging;
4) powder process: it is the powder process of 0.5～0.7MPa airflow milling that broken above-mentioned hydrogen powder is put into inert gas flow pressure, obtain the powder of particle size 2～5 μ m, be to stir with protective agent under 0.03～0.06MPa protection at inert gas pressure, logical inert gas gas pressure 0.01～0.05Mpa protection when holding vessel stores;
5) moulding: adopt inert gas shielding magnetic to enter mould molding, in formed gloves case, inert gas flow is controlled at 5～20m
3/ h, Control for Oxygen Content≤0.05% quality;
6) sintering: first adopt inert gas shielding to go out module and enter stove, enter inert gas flow in stove glove box and be controlled at 15～50m
3/ h, Control for Oxygen Content is in≤0.02% quality; Sintering furnace is vacuumized, the vacuum degree control of sintering furnace is 4 × 10 again
-2below Pa, when sintering is cooling, adopt inert gas pressure to be controlled at 0.04～0.02Mpa cooling protection.
8. the preparation method of a kind of high magnetic characteristics sintered NdFeB according to claim 7, is characterized in that described inert gas is argon gas.
9. the preparation method of a kind of high magnetic characteristics sintered NdFeB according to claim 7, it is characterized in that with nitrogen content in neodymium iron boron magnetic body after the molding neodymium iron boron sintering of Ar Buchholz protection be 80～200PPm.
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| CN104493158A (en) * | 2014-12-23 | 2015-04-08 | 宁波科田磁业有限公司 | Preparation method and device for decreasing sintered NdFeB declination |
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Application publication date: 20141112 |