CN102031445A - Method for preparing high-magnetic energy product high-coercive force low-cost sintered neodymium iron boron - Google Patents
Method for preparing high-magnetic energy product high-coercive force low-cost sintered neodymium iron boron Download PDFInfo
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 25
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 title abstract description 10
- 230000005291 magnetic effect Effects 0.000 claims abstract description 34
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 239000010949 copper Substances 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000032683 aging Effects 0.000 claims abstract description 11
- 229910052802 copper Inorganic materials 0.000 claims abstract description 11
- 238000000465 moulding Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 3
- 238000003801 milling Methods 0.000 claims description 15
- 238000005516 engineering process Methods 0.000 claims description 12
- 238000002844 melting Methods 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 11
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 238000013022 venting Methods 0.000 claims description 9
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 239000004615 ingredient Substances 0.000 claims description 6
- 229910052758 niobium Inorganic materials 0.000 claims description 6
- 229910052771 Terbium Inorganic materials 0.000 claims description 4
- 239000000696 magnetic material Substances 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 239000000314 lubricant Substances 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 3
- 238000003723 Smelting Methods 0.000 abstract 3
- 230000001112 coagulating effect Effects 0.000 abstract 3
- 239000006247 magnetic powder Substances 0.000 abstract 3
- 238000010902 jet-milling Methods 0.000 abstract 2
- 239000002245 particle Substances 0.000 abstract 2
- 238000003483 aging Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 239000011261 inert gas Substances 0.000 abstract 1
- 230000001681 protective effect Effects 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 9
- 229910052796 boron Inorganic materials 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 229910052761 rare earth metal Inorganic materials 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000005984 hydrogenation reaction Methods 0.000 description 4
- 238000007670 refining Methods 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 230000005389 magnetism Effects 0.000 description 3
- 230000005290 antiferromagnetic effect Effects 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000005275 alloying Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
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- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The invention discloses a method for preparing high-magnetic energy product high-coercive force low-cost sintered neodymium iron boron (NdFeB). The method comprises the following steps of: throwing raw materials into a rapid coagulating furnace and smelting in the protective atmosphere of inert gases or nitrogen, and pouring smelting liquid onto a copper roller at a roller speed of 2 to 4m/s to form a rapid coagulating thin strip with the mean thickness of 0.1 to 0.3mm; performing hydrogen breaking and jet milling to obtain magnetic powder with the superficial area mean particle size of 1.5 to 3 mu m, and orientating and molding the magnetic powder in a magnetic field to obtain a blank; and finally, sintering, cooling and ageing to obtain a sintered NdFeB magnet with the mean grain size of 5 to 6 mu m. Compared with the conventional preparation method, by optimizing the rapid coagulating process and combining the adjustment of raw materials, the preparation method makes NdFeB columnar crystals reduced during smelting; therefore, the superficial area mean particle size of the magnetic powder is reduced in the process of performing jet milling, the mean grain size of the sintered NdFeB magnet is reduced finally, and the coercive force of the sintered NdFeB magnet is improved. Therefore, the preparation method is suitable for preparing a high-magnetic energy product and low-cost high-coercive force magnet.
Description
Technical field
The present invention relates to technical field of magnetic materials, relate in particular to a kind of preparation method who prepares high energy product, high-coercive force, low-cost sintered NdFeB.
Background technology
Sintered nd-fe-b magnet is because its excellent magnetism can have been served as extremely important role in our life of today.Sintered neodymium iron boron material is mainly used in the mainstay industry and the new high-tech industry in the whole world, as computer industry, automotive industry, communication information industry, health care industry, transportation industries, stereo set, video recording video reproduction industry and office automation and household electrical appliances industry etc.
Along with the requirement of energy-saving and emission-reduction, high-grade magnet applications mainly is the high-coercive force magnet, and the anti-demagnetization capability of high-coercive force magnet is strong, has high temperature stability and low coercive force temperature coefficient.The coercive force of sintered NdFeB is relevant with anisotropy field, and anisotropy field is big more, and the coercive force of magnet is high more.Nd
2Fe
14B, Dy
2Fe
14B and Tb
2Fe
14The anisotropy field of B is respectively 5810kA/m, and therefore 11940kA/m and 17572kA/m, generally improve coercive force by adding heavy rare earth element Dy and Tb, and the addition of heavy rare earth element is too much in the present domestic high-coercive force magnet, especially Tb.But,, therefore will significantly increase the cost of this magnet by the coercive force that adds heavy rare earth element raising neodymium iron boron magnetic body because heavy rare earth element costs an arm and a leg.Simultaneously,, thereby cause the magnetic flux Bs of neodymium iron boron magnetic body and remanent magnetism Br to descend, the magnetic property of high-coercive force neodymium iron boron magnetic body is reduced because heavy rare earth element and iron dust antiferromagnetic coupling reduce the iron atom magnetic moment.
At present, the production technique of preparation high-performance Ne-Fe-B is to adopt the rapid hardening thin slice, secondly by the broken technology of hydrogen rapid-hardening flake is broken into meal, make fine powder by airflow milling then, the surface mean size of fine powder is generally at 3.2 microns~4.0 microns, surface mean size is lower or high more all can to cause coercive force to reduce, the lower generation transgranular fracture of surface mean size and coercive force is reduced, and surface mean size improves because the mean grain size of magnet becomes ambassador's coercive force reduces.
Summary of the invention
The technical problem to be solved in the present invention is at the above-mentioned state of the art, and a kind of method for preparing high energy product, high-coercive force, low-cost sintered NdFeB is provided.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of method for preparing high energy product, high-coercive force, low-cost sintered NdFeB comprises the steps:
Step 1: according to the ingredient formula (PrNd) of sintered NdFeB
aFe
100%-a-b-cB
bM
cShown component and mass percentage content preparation raw material, wherein M be in Dy, Tb, Nb, Co, Ga, Zr, Al and the Cu element one or more, a, b and c represent the mass percent of each corresponding element respectively, and 20%≤a≤32%, 0.9%≤b≤1.2%, 0%≤c≤6%;
Step 2: the raw material of step 1 preparation is dropped into the rapid hardening stove, carry out melting in rare gas element or nitrogen protection atmosphere, after the melting melting liquid is watered roller speed on the copper roller of 2m/s~4m/s, getting rid of into mean thickness is the rapid hardening strip of 0.1mm~0.3mm;
Step 3: the rapid hardening strip that step 2 is obtained carries out the broken technology of hydrogen, and the broken laggard capable airflow milling of hydrogen obtains the magnetic that surface mean size is 1.5 μ m~3 μ m, with magnetic oriented moulding in magnetic field, obtains molded blank;
Step 4: the molded blank that step 3 is obtained carries out sintering, carry out dehydrogenation venting in the sintering process, regulate sintering temperature to 1040 ℃~1110 ℃ then, be incubated 2 hours~5 hours postcooling, carry out ageing treatment at last, obtaining mean grain size is the Sintered NdFeB magnet of 5 μ m~6 μ m.
In order to optimize technique scheme, the measure of taking also comprises:,
Each component and content in the step 1 are:
PrNd alloying element 20%~32%;
Fe element 55%~70%;
B element 0.9%~1.1%;
Dy element 0~8%;
Tb element 0~5%;
Co element 0~2%;
Cu element 0~0.2%;
Ga element 0~0.2%;
Al element 0~1%;
Zr element 0~1%;
Nb element 0~1%.
Roller speed in the step 2 is preferably 2.5m/s~4m/s.
The mean thickness of the rapid hardening strip in the step 2 is preferably 0.1mm~0.2mm.
The density of molded blank is 4.0g/cm in the step 3
3More than.
The interpolation mass percentage content is 0.1%~2% lubricant in the magnetic in the step 3, helps the raising of orientation degree.
Dehydrogenation venting in the step 4 is between 300 ℃~800 ℃ several temperature spots to be set, and is incubated 1 hour respectively at each corresponding temperature point~carried out the dehydrogenation venting in 3 hours, and three temperature spots preferably are set between 300 ℃~800 ℃.
The magneticstrength in magnetic field is 1.5T~2T in the step 3.
A kind of preparation high energy product of the present invention, high-coercive force, the method of low-cost sintered NdFeB is by the optimization of rapid hardening technology, and the adjustment of combined formulation, reduced the surface mean size of airflow milling magnetic, thereby reduced the mean grain size of sintered Nd-Fe-B permanent magnetic material, than present technology of preparing: the surface mean size of airflow milling magnetic is controlled at 3.2 μ m~4.0 μ m, the average crystal grain of magnet is controlled at 10 μ m~15 μ m behind the sintering, that have even bigger, preparation method of the present invention can make the magnetic surface mean size be controlled at 1.5 μ m~3 μ m, the mean grain size of magnet can reach 5 μ m~6 μ m behind the sintering, finally improves the coercive force of Sintered NdFeB magnet.At present, the coercitive method that improves neodymium iron boron magnetic body mainly is by adding heavy rare earths Dy or Tb, the Dy price is six or seven times of Nd price, and the Tb price is 12 times of the Nd price, in addition, because heavy rare earth element and iron dust are in antiferromagnetic coupling, remanent magnetism is reduced greatly, the present invention is by optimizing rapid hardening technology, the mean grain size of neodymium iron boron column crystal reduces when making melting, thereby the surface mean size of magnetic reduces when making airflow milling, and coercive force improves, and therefore preparation method of the present invention is fit to preparation high energy product, high-coercive force magnet cheaply.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1: the Nd-Fe-Bo permanent magnet material in the present embodiment follows these steps to produce:
Step 1: according to the expression component of Nd-Fe-B alloys and the ingredient formula of mass percentage content: (PrNd)
30%Fe
66.9%B
1.0%Dy
1.0%Cu
0.1%Al
0.2%Nb
0.2%Co
0.6%Preparation raw material;
Step 2: confected materials is dropped in the rapid hardening stove, in vacuum tightness 2 * 10
-2Add heat drying furnace under the vacuum of Pa, charge into Ar gas then and carry out melting, after the refining molten steel is watered roller speed on the copper roller of 2.5m/s, getting rid of into mean thickness is the rapid hardening strip of 0.25mm;
Step 3: the rapid hardening strip packed into carry out the broken technology of hydrogen in the hydrogenation furnace, powder after hydrogen is broken carries out airflow milling, the magnetic surface mean size is controlled at 2.5 μ m during airflow milling, is oriented moulding in the magnetic field of 2T in magneticstrength, and the density of molded blank is more than the 4.0gg/cm3;
Step 4: the sintering oven of the blank after the moulding being put into high vacuum carries out sintering, is incubated 2 hours respectively at 300 ℃, 560 ℃ and 800 ℃ in the sintering process and carries out the dehydrogenation venting; Regulate sintering temperature to 1050 ℃, be incubated and charge into high-purity Ar gas after 4 hours and be cooled to below 100 ℃, carry out ageing treatment at 900 ℃ then and carried out ageing treatment 4 hours in 4 hours and 500 ℃.
Embodiment 2: the Nd-Fe-Bo permanent magnet material in the present embodiment follows these steps to produce:
Step 1: according to the expression component of Nd-Fe-B alloys and the ingredient formula of mass percentage content: (PrNd)
30%Fe
66.9%B
1.0%Dy
1.0%Cu
0.1%Al
0.2%Nb
0.2%Co
0.6%Preparation raw material;
Step 2: confected materials is dropped in the rapid hardening stove, in vacuum tightness 2 * 10
-2Add heat drying furnace under the vacuum of Pa, charge into Ar gas then and carry out melting, after the refining molten steel is watered roller speed on the copper roller of 4.0m/s, getting rid of into mean thickness is the rapid hardening strip of 0.16mm;
Step 3: the rapid hardening strip packed into carry out the broken technology of hydrogen in the hydrogenation furnace, powder after hydrogen is broken carries out airflow milling, the surface mean size of magnetic is controlled at 1.5 μ m during airflow milling, is oriented moulding in the magnetic field of 2T in magneticstrength, and the density of molded blank is more than the 4.0g/cm3;
Step 4: the sintering oven of the blank after the moulding being put into high vacuum carries out sintering, is incubated 2 hours respectively at 300 ℃, 560 ℃ and 800 ℃ in the sintering process and carries out the dehydrogenation venting; Regulate sintering temperature to 1035 ℃, be incubated and charge into high-purity Ar gas after 4 hours and be cooled to below 100 ℃, carry out ageing treatment at 890 ℃ then and carried out ageing treatment 4 hours in 4 hours and 460 ℃.
Embodiment 3: the Nd-Fe-Bo permanent magnet material in the present embodiment follows these steps to produce:
Step 1: according to the expression component of Nd-Fe-B alloys and the ingredient formula of mass percentage content: (PrNd)
28%Fe
66.9%B
1.0%Dy
3.0%Cu
0.1%Al
0.2%Nb
0.2%Co
0.6%Preparation raw material;
Step 2: confected materials is dropped in the rapid hardening stove, in vacuum tightness 2 * 10
-2Add heat drying furnace under the vacuum of Pa, charge into Ar gas then and carry out melting, after the refining molten steel is watered roller speed on the copper roller of 3.0m/s, getting rid of into mean thickness is the rapid hardening strip of 0.20mm;
Step 3: the rapid hardening strip packed into carry out the broken technology of hydrogen in the hydrogenation furnace, powder after hydrogen is broken carries out airflow milling, the surface-area of magnetic on average is controlled at 2.0 μ m during airflow milling, is oriented moulding in the magnetic field of 2T in magneticstrength, and the density of molded blank is more than the 4.0g/cm3;
Step 4: the sintering oven of the blank after the moulding being put into high vacuum carries out sintering, is incubated 2 hours respectively at 300 ℃, 560 ℃ and 800 ℃ in the sintering process and carries out the dehydrogenation venting; Regulate sintering temperature to 1065 ℃, be incubated and charge into high-purity Ar gas after 4 hours and be cooled to below 100 ℃, carry out ageing treatment at 900 ℃ then and carried out ageing treatment 4 hours in 4 hours and 450 ℃.
Embodiment 4: the Nd-Fe-Bo permanent magnet material in the present embodiment follows these steps to produce:
Step 1: according to the expression component of Nd-Fe-B alloys and the ingredient formula of mass percentage content: (PrNd)
28%Fe
66.9%B
1.0%Dy
3.0%Cu
0.1%Al
0.2%Nb
0.2%Co
0.6%Preparation raw material;
Step 2: confected materials is dropped in the rapid hardening stove, in vacuum tightness 2 * 10
-2Add heat drying furnace under the vacuum of Pa, charge into Ar gas then and carry out melting, after the refining molten steel is watered roller speed on the copper roller of 4.0m/s, getting rid of into mean thickness is the rapid hardening strip of 0.13mm;
Step 3: the rapid hardening strip packed into carry out the broken technology of hydrogen in the hydrogenation furnace, powder after hydrogen is broken carries out airflow milling, the surface mean size of magnetic is controlled at 1.5 μ m during airflow milling, is oriented moulding in the magnetic field of 2T in magneticstrength, and the density of molded blank is more than the 4.0g/cm3;
Step 4: the sintering oven of the blank after the moulding being put into high vacuum carries out sintering, is incubated 2 hours respectively at 300 ℃, 560 ℃ and 800 ℃ in the sintering process and carries out the dehydrogenation venting; Regulate sintering temperature to 1055 ℃, be incubated and charge into high-purity Ar gas after 4 hours and be cooled to below 100 ℃, carry out ageing treatment at 890 ℃ then and carried out ageing treatment 4 hours in 4 hours and 430 ℃.
Each parameter of the neodymium iron boron magnetic body that embodiment 1 to embodiment 4 makes is as shown in the table, and comparative example wherein is in order to compare with embodiment 1, each corresponding parameter value of the sintered NdFeB that the raw material among the embodiment 1 is prepared according to prior preparation method.
As can be seen from the above table, relative prior preparation method, utilize preparation method of the present invention to reduce the granularity of airflow milling magnetic, thereby reduced the mean grain size of neodymium iron boron magnetic body behind the sintering, finally improved the coercive force and the maximum magnetic energy product of Sintered NdFeB magnet.
Claims (8)
1. a method for preparing high energy product, high-coercive force, low-cost sintered NdFeB comprises the steps:
Step 1: according to the ingredient formula (PrNd) of sintered NdFeB
aFe
100%-a-b-cB
bM
cShown component and mass percentage content preparation raw material, wherein M be in Dy, Tb, Nb, Co, Ga, Zr, Al and the Cu element one or more, a, b and c represent the mass percent of each corresponding element respectively, and 20%≤a≤32%, 0.9%≤b≤1.2%, 0%≤c≤6%;
Step 2: the raw material of step 1 preparation is dropped into the rapid hardening stove, carry out melting in rare gas element or nitrogen protection atmosphere, after the melting melting liquid is watered roller speed on the copper roller of 2m/s~4m/s, getting rid of into mean thickness is the rapid hardening strip of 0.1mm~0.3mm;
Step 3: the rapid hardening strip that step 2 is obtained carries out the broken technology of hydrogen, and the broken laggard capable airflow milling of hydrogen obtains the magnetic that surface mean size is 1.5 μ m~3 μ m, with magnetic oriented moulding in magnetic field, obtains molded blank;
Step 4: the molded blank that step 3 is obtained carries out sintering, carry out dehydrogenation venting in the sintering process, regulate sintering temperature to 1040 ℃~1110 ℃ then, be incubated 2 hours~5 hours postcooling, carry out ageing treatment at last, obtaining mean grain size is the sintered NdFeB of 5 μ m~6 μ m.
2. a kind of method for preparing high energy product, high-coercive force, low-cost sintered NdFeB according to claim 1 is characterized in that: the roller speed in the described step 2 is 2.5m/s~4m/s.
3. a kind of method for preparing high energy product, high-coercive force, low-cost sintered NdFeB according to claim 1 is characterized in that: the mean thickness of the rapid hardening strip in the described step 2 is 0.1mm~0.2mm.
4. a kind of method for preparing high energy product, high-coercive force, low-cost sintered NdFeB according to claim 1 is characterized in that: the density of molded blank is 4.0g/cm in the described step 3
3More than.
5. a kind of method for preparing high energy product, high-coercive force, low-cost sintered NdFeB according to claim 1 is characterized in that: the interpolation mass percent is 0.1%~2% lubricant in the magnetic in the described step 3.
6. a kind of method for preparing high energy product, high-coercive force, low-cost sintered NdFeB according to claim 1, it is characterized in that: the dehydrogenation venting in the described step 4 is between 300 ℃~800 ℃ several temperature spots to be set, and is incubated 1 hour respectively at each corresponding temperature point~carried out dehydrogenation and exit in 3 hours.
7. a kind of method for preparing high energy product, high-coercive force, low-cost sintered NdFeB according to claim 6 is characterized in that: three temperature spots are set in the described step 4.
8. according to the preparation method of the described a kind of sintered Nd-Fe-B permanent magnetic material of arbitrary claim in the claim 1 to 7, it is characterized in that: the magneticstrength in magnetic field is 1.5T~2T in the described step 3.
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CN103093914A (en) * | 2013-01-25 | 2013-05-08 | 宁波同创强磁材料有限公司 | High-performance neodymium-iron-boron magnet and preparation method thereof |
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CN103940642A (en) * | 2013-01-17 | 2014-07-23 | 中国科学院宁波材料技术与工程研究所 | Standard sample for Nd-Fe-B magnetic material quantitative analysis and XRF analysis method |
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