CN110289161B - Preparation method of neodymium iron boron magnet with low rare earth content - Google Patents
Preparation method of neodymium iron boron magnet with low rare earth content Download PDFInfo
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- CN110289161B CN110289161B CN201910639719.2A CN201910639719A CN110289161B CN 110289161 B CN110289161 B CN 110289161B CN 201910639719 A CN201910639719 A CN 201910639719A CN 110289161 B CN110289161 B CN 110289161B
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- iron boron
- neodymium iron
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 112
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 29
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 29
- 238000005245 sintering Methods 0.000 claims abstract description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 62
- 239000000843 powder Substances 0.000 claims description 62
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims description 48
- 238000005496 tempering Methods 0.000 claims description 46
- 238000005266 casting Methods 0.000 claims description 42
- 229910045601 alloy Inorganic materials 0.000 claims description 39
- 239000000956 alloy Substances 0.000 claims description 39
- 238000003723 Smelting Methods 0.000 claims description 35
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 33
- 229910052786 argon Inorganic materials 0.000 claims description 31
- 238000002156 mixing Methods 0.000 claims description 30
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 26
- 238000001816 cooling Methods 0.000 claims description 22
- 239000010949 copper Substances 0.000 claims description 21
- 239000010936 titanium Substances 0.000 claims description 21
- 229910052719 titanium Inorganic materials 0.000 claims description 21
- 229910052726 zirconium Inorganic materials 0.000 claims description 21
- 239000012768 molten material Substances 0.000 claims description 20
- 229910052802 copper Inorganic materials 0.000 claims description 19
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 15
- 229910052779 Neodymium Inorganic materials 0.000 claims description 15
- 229910052796 boron Inorganic materials 0.000 claims description 15
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 14
- 239000001257 hydrogen Substances 0.000 claims description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims description 14
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 14
- 229910052742 iron Inorganic materials 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 12
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000000465 moulding Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- 238000005086 pumping Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims 6
- RZJQYRCNDBMIAG-UHFFFAOYSA-N [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] Chemical class [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] RZJQYRCNDBMIAG-UHFFFAOYSA-N 0.000 claims 1
- 229910052771 Terbium Inorganic materials 0.000 abstract description 16
- 229910052692 Dysprosium Inorganic materials 0.000 abstract description 15
- 229910000881 Cu alloy Inorganic materials 0.000 abstract description 4
- 229910001069 Ti alloy Inorganic materials 0.000 abstract description 4
- 229910001093 Zr alloy Inorganic materials 0.000 abstract description 4
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 abstract description 3
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 4
- 230000005389 magnetism Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0266—Moulding; Pressing
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
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- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
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- C22C—ALLOYS
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- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
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- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
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- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0573—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes obtained by reduction or by hydrogen decrepitation or embrittlement
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- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0576—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together pressed, e.g. hot working
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- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
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- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
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Abstract
The invention discloses a preparation method of a neodymium iron boron magnet with low rare earth content, which belongs to the technical field of magnet preparation. In the preparation process of the preparation method, dysprosium and terbium are not used, and Cu, Zr and Ti alloys are added and are matched with high-temperature sintering at the temperature higher than 1100 ℃, so that the movement of the grain boundary of the main phase is limited by the grain boundary of the Cu, Zr and Ti alloys, the growth of grains in the main phase is hindered, and the magnetic exchange among the grains in the main phase is blocked. And then the coercive force and the working temperature of the neodymium iron boron magnet are improved, the preparation of the magnet with high thermal stability is facilitated, meanwhile, rare earth metals Dy and Tb are not used, and the preparation cost of the magnet is greatly reduced.
Description
Technical Field
The invention belongs to the technical field of magnet preparation, and particularly relates to a preparation method of a neodymium iron boron magnet with low rare earth content.
Background
Neodymium magnet (Neodymium magnet), also known as Neodymium-iron-boron magnet (NdFeB magnet), is made of Neodymium, iron, boron (Nd)2Fe14B) The tetragonal system crystal is formed. The neodymium iron boron magnet has the characteristics of small volume, light weight, strong magnetism and the like. Neodymium iron boron magnets have been used in the fields of automobiles, computers, information, aviation, and the like since their discovery. However, the curie temperature of the ndfeb magnet is low, and the magnetism of the ndfeb magnet is weakened along with the increase of the casting with high working temperature. In order to change the characteristics of the Nd-Fe-B magnet, the prior art usesDysprosium (Dy) and terbium (Tb) are added to improve the coercivity of a neodymium magnet and improve the thermal stability and magnetism at high temperature.
Both Dy and Tb are rare earth metals with lower contents than other metals, and with the recent widespread use of neodymium-iron-boron magnets, the mining amount of Dy and Tb is continuously increasing, making Dy and Tb expensive raw materials. If the using amount of Dy and Tb can be reduced or Dy and Tb are not used in the preparation process of the neodymium iron boron magnet, the cost of the neodymium iron boron magnet can be greatly reduced. In the prior art, although a preparation method for improving the neodymium iron boron magnet by adding cobalt (Co) exists, the problem of reduced magnetism is caused by adding Co.
Disclosure of Invention
In order to overcome the defects of the prior art, the technical problems to be solved by the invention are as follows: provides a preparation method of a neodymium iron boron magnet which does not use dysprosium and terbium and has higher working temperature and low rare earth content.
In order to solve the technical problems, the invention adopts the technical scheme that: a preparation method of a neodymium iron boron magnet with low rare earth content comprises the following steps:
step 1, mixing materials of 1.5-3% of zirconium, 0.5-2% of titanium and the balance of copper according to weight percentage, then repeatedly smelting for many times under the protection of argon, and rapidly solidifying and casting the molten materials during the last smelting to obtain alloy cast pieces;
step 2, mixing 10-15% of praseodymium, 13-18% of neodymium, 0.8-1.5% of boron and the balance of iron according to the weight percentage, then smelting under the protection of argon, and rapidly solidifying and casting the molten material to obtain a main phase casting sheet;
step 3, respectively carrying out hydrogen fracturing on the alloy casting sheet and the main phase casting sheet to obtain alloy powder and main phase powder;
step 4, adding 2-5% of alloy powder into the main phase powder, fully and uniformly mixing, and crushing into neodymium iron boron powder with the particle size of 2.5-3.8 microns by using an airflow mill;
and 5, pressing and molding the neodymium iron boron powder in an oriented magnetic field of 2.1T to obtain a pressed compact, sintering the pressed compact at 1110-1120 ℃ for 7-9h at the heating rate of 8-10 ℃/min, and then performing primary tempering and secondary tempering to obtain the neodymium iron boron magnet.
The invention has the beneficial effects that: according to the preparation method of the neodymium iron boron magnet with low rare earth content, Dy and Tb are not added in the preparation process, and Cu, Zr and Ti alloys are added and are matched with high-temperature sintering at the temperature higher than 1100 ℃, so that the movement of the grain boundary of the main phase is limited by the alloy grain boundary of Cu, Zr and Ti, the growth of crystal grains in the main phase is hindered, and the magnetic exchange among the crystal grains in the main phase is blocked. And then the coercive force and the working temperature of the neodymium iron boron magnet are improved, the preparation of the magnet with high thermal stability is facilitated, meanwhile, rare earth metals Dy and Tb are not used, and the preparation cost of the magnet is greatly reduced.
Detailed Description
In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.
The most key concept of the invention is as follows: and the alloy of Cu, Zr and Ti is used for replacing Dy and Tb, so that the coercive force and the working temperature of the neodymium iron boron magnet are improved.
The invention provides a preparation method of a neodymium iron boron magnet with low rare earth content, which comprises the following steps:
step 1, mixing materials of 1.5-3% of zirconium, 0.5-2% of titanium and the balance of copper according to weight percentage, then repeatedly smelting for many times under the protection of argon, and rapidly solidifying and casting the molten materials during the last smelting to obtain alloy cast pieces;
step 2, mixing 10-15% of praseodymium, 13-18% of neodymium, 0.8-1.5% of boron and the balance of iron according to the weight percentage, then smelting under the protection of argon, and rapidly solidifying and casting the molten material to obtain a main phase casting sheet;
step 3, respectively carrying out hydrogen fracturing on the alloy casting sheet and the main phase casting sheet to obtain alloy powder and main phase powder;
step 4, adding 2-5% of alloy powder into the main phase powder, fully and uniformly mixing, and crushing into neodymium iron boron powder with the particle size of 2.5-3.8 microns by using an airflow mill;
and 5, pressing and molding the neodymium iron boron powder in an oriented magnetic field of 2.1T to obtain a pressed compact, sintering the pressed compact at 1110-1120 ℃ for 7-9h at the heating rate of 8-10 ℃/min, and then performing primary tempering and secondary tempering to obtain the neodymium iron boron magnet.
From the above description, the beneficial effects of the present invention are: according to the preparation method of the neodymium iron boron magnet with low rare earth content, Dy and Tb are not added in the preparation process, and Cu, Zr and Ti alloys are added and are matched with high-temperature sintering at the temperature higher than 1100 ℃, so that the movement of the grain boundary of the main phase is limited by the alloy grain boundary of Cu, Zr and Ti, the growth of crystal grains in the main phase is hindered, and the magnetic exchange among the crystal grains in the main phase is blocked. And then the coercive force and the working temperature of the neodymium iron boron magnet are improved, the preparation of the magnet with high thermal stability is facilitated, meanwhile, rare earth metals Dy and Tb are not used, and the preparation cost of the magnet is greatly reduced.
Further, in the step 1, the content of zirconium is 2%, and the content of titanium is 0.8%.
Further, in the step 2, the content of praseodymium is 14%, the content of neodymium is 18%, and the content of boron is 0.9%.
Furthermore, the smelting times in the step 1 are 3-6 times. The uniformity of mixing is ensured by multiple melting.
Further, after the hydrogen breaking in the step 3 is finished, vacuumizing and dehydrogenation treatment is further included, wherein the dehydrogenation treatment temperature is 680 ℃, and the dehydrogenation time is 4.5 hours.
Further, the time of the first-stage tempering in the step 5 is 4 hours, and the temperature is 950 ℃; the time of the secondary tempering is 4 hours, the temperature is 600 ℃, and argon is filled for cooling during cooling.
Example 1:
the preparation method of the neodymium iron boron magnet with low rare earth content specifically comprises the following steps:
step 1, mixing materials of 2% of zirconium, 0.8% of titanium and the balance of copper according to the weight percentage, then repeatedly smelting for 4 times under the protection of argon, and rapidly solidifying the molten materials to obtain alloy cast pieces during the last smelting;
step 2, mixing materials including 15% of praseodymium, 16% of neodymium, 1.5% of boron and the balance of iron according to the weight percentage, then smelting under the protection of argon, and rapidly solidifying and casting the molten materials to obtain a main phase casting sheet;
step 3, performing hydrogen breaking and vacuum pumping dehydrogenation treatment on the alloy casting sheet and the main phase casting sheet respectively to obtain alloy powder and main phase powder; wherein, the dehydrogenation treatment temperature is 680 ℃, and the dehydrogenation time is 4.5 h;
step 4, adding alloy powder accounting for 5 percent of the total weight of the main phase powder into the main phase powder, fully and uniformly mixing, and crushing the mixture into neodymium iron boron powder with the particle size of 2.5-3.8 mu m by an airflow mill;
step 5, pressing and molding neodymium iron boron powder in an oriented magnetic field of 2.1T to obtain a pressed compact, sintering the pressed compact at 1120 ℃ for 8h at a heating rate of 8-10 ℃/min, and then performing primary tempering and secondary tempering to obtain a neodymium iron boron magnet A; wherein, the time of the first-stage tempering is 4h, and the temperature is 950 ℃; the time of the secondary tempering is 4 hours, the temperature is 600 ℃, and argon is filled for cooling during cooling.
The remanence Br of the neodymium iron boron magnet a is as follows: 13.58 KGs; coercivity Hcb is: 12.93 KOe; the magnetic energy product BH (max) is: 40.23 MGOe.
Example 2:
the preparation method of the neodymium iron boron magnet with low rare earth content specifically comprises the following steps:
step 1, mixing 2.5 percent of zirconium, 2 percent of titanium and the balance of copper according to the weight percentage, then repeatedly smelting for 3 times under the protection of argon, and rapidly solidifying the molten material to obtain an alloy cast sheet during the last smelting;
step 2, mixing materials of 14% of praseodymium, 18% of neodymium, 0.9% of boron and the balance of iron according to the weight percentage, then smelting under the protection of argon, and rapidly solidifying and casting the molten materials to obtain a main phase casting sheet during smelting;
step 3, performing hydrogen breaking and vacuum pumping dehydrogenation treatment on the alloy casting sheet and the main phase casting sheet respectively to obtain alloy powder and main phase powder; wherein, the dehydrogenation treatment temperature is 680 ℃, and the dehydrogenation time is 4 h;
step 4, adding alloy powder accounting for 3 percent of the total weight of the main phase powder into the main phase powder, fully and uniformly mixing, and crushing the mixture into neodymium iron boron powder with the particle size of 2.5-3.8 mu m by an airflow mill;
step 5, pressing and molding neodymium iron boron powder in an oriented magnetic field of 2.1T to obtain a pressed compact, sintering the pressed compact at 1115 ℃ for 9 hours at a heating rate of 8-10 ℃/min, and then performing primary tempering and secondary tempering to obtain a neodymium iron boron magnet B; wherein, the time of the first-stage tempering is 3.5h, and the temperature is 980 ℃; the time of the secondary tempering is 3 hours, the temperature is 620 ℃, and argon is filled for cooling during cooling.
The remanence Br of the neodymium iron boron magnet B is: 12.81 KGs; coercivity Hcb is: 12.20 KOe; the magnetic energy product BH (max) is: 38.64 MGOe.
Example 3:
the preparation method of the neodymium iron boron magnet with low rare earth content specifically comprises the following steps:
step 1, mixing 3% of zirconium, 1.5% of titanium and the balance of copper according to the weight percentage, then repeatedly smelting for 6 times under the protection of argon, and rapidly solidifying the molten material to obtain an alloy cast sheet during the last smelting;
step 2, mixing materials of 10% of praseodymium, 15% of neodymium, 1.2% of boron and the balance of iron according to the weight percentage, then smelting under the protection of argon, and rapidly solidifying and casting the molten materials to obtain a main phase casting sheet;
step 3, performing hydrogen breaking and vacuum pumping dehydrogenation treatment on the alloy casting sheet and the main phase casting sheet respectively to obtain alloy powder and main phase powder; wherein the dehydrogenation treatment temperature is 660 ℃, and the dehydrogenation time is 3 h;
step 4, adding alloy powder accounting for 5 percent of the total weight of the main phase powder into the main phase powder, fully and uniformly mixing, and crushing the mixture into neodymium iron boron powder with the particle size of 2.5-3.8 mu m by an airflow mill;
step 5, pressing and molding neodymium iron boron powder in an oriented magnetic field of 2.1T to obtain a pressed compact, sintering the pressed compact at 1110 ℃ for 7 hours at a heating rate of 8-10 ℃/min, and then performing primary tempering and secondary tempering to obtain a neodymium iron boron magnet C; wherein, the time of the first-stage tempering is 4h, and the temperature is 950 ℃; the time of the secondary tempering is 3.5h, the temperature is 600 ℃, and argon is filled for cooling during cooling.
The remanence Br of the neodymium iron boron magnet C is: 12.62 KGs; coercivity Hcb is: 12.07 KOe; the magnetic energy product BH (max) is: 36.82 MGOe.
Example 4:
the preparation method of the neodymium iron boron magnet with low rare earth content specifically comprises the following steps:
step 1, mixing materials of 1.8 percent of zirconium, 0.5 percent of titanium and the balance of copper according to weight percentage, then repeatedly smelting for 6 times under the protection of argon, and rapidly solidifying the molten materials to obtain alloy cast pieces during the last smelting;
step 2, mixing materials of praseodymium accounting for 12 percent of the weight percentage, neodymium accounting for 14 percent of the weight percentage, boron accounting for 0.8 percent of the weight percentage and iron accounting for the rest, then smelting under the protection of argon, and rapidly solidifying and casting the molten materials to obtain a main phase casting sheet during smelting;
step 3, performing hydrogen breaking and vacuum pumping dehydrogenation treatment on the alloy casting sheet and the main phase casting sheet respectively to obtain alloy powder and main phase powder; wherein, the dehydrogenation treatment temperature is 680 ℃, and the dehydrogenation time is 4 h;
step 4, adding alloy powder accounting for 5 percent of the total weight of the main phase powder into the main phase powder, fully and uniformly mixing, and crushing the mixture into neodymium iron boron powder with the particle size of 2.5-3.8 mu m by an airflow mill;
step 5, pressing and molding neodymium iron boron powder in an oriented magnetic field of 2.1T to obtain a pressed compact, sintering the pressed compact at 1120 ℃ for 9 hours at a heating rate of 8-10 ℃/min, and then performing primary tempering and secondary tempering to obtain a neodymium iron boron magnet D; wherein, the time of the first-stage tempering is 4h, and the temperature is 900 ℃; the time of the secondary tempering is 4 hours, the temperature is 600 ℃, and argon is filled for cooling during cooling.
The remanence Br of the neodymium iron boron magnet D is: 13.24 KGs; coercivity Hcb is: 12.74 KOe; the magnetic energy product BH (max) is: 39.88 MGOe.
Example 5:
the preparation method of the neodymium iron boron magnet with low rare earth content specifically comprises the following steps:
step 1, mixing materials of 1.5 percent of zirconium, 1 percent of titanium and the balance of copper according to the weight percentage, then repeatedly smelting for 5 times under the protection of argon, and rapidly solidifying the molten materials to obtain alloy cast pieces during the last smelting;
step 2, mixing 13% of praseodymium, 13% of neodymium, 1% of boron and the balance of iron according to the weight percentage, then smelting under the protection of argon, and rapidly solidifying and casting the molten material to obtain a main phase casting sheet;
step 3, performing hydrogen breaking and vacuum pumping dehydrogenation treatment on the alloy casting sheet and the main phase casting sheet respectively to obtain alloy powder and main phase powder; wherein, the dehydrogenation treatment temperature is 680 ℃, and the dehydrogenation time is 4.5 h;
step 4, adding alloy powder accounting for 5 percent of the total weight of the main phase powder into the main phase powder, fully and uniformly mixing, and crushing the mixture into neodymium iron boron powder with the particle size of 2.5-3.8 mu m by an airflow mill;
step 5, pressing and molding neodymium iron boron powder in an oriented magnetic field of 2.1T to obtain a pressed compact, sintering the pressed compact at 1120 ℃ for 7h at a heating rate of 8-10 ℃/min, and then performing primary tempering and secondary tempering to obtain a neodymium iron boron magnet E; wherein, the time of the first-stage tempering is 4h, and the temperature is 950 ℃; the time of the secondary tempering is 4 hours, the temperature is 600 ℃, and argon is filled for cooling during cooling.
The remanence Br of the neodymium iron boron magnet E is: 13.06 KGs; coercivity Hcb is: 12.56 KOe; the magnetic energy product BH (max) is: 38.58 MGOe.
Comparative example 1:
the preparation method of the neodymium iron boron magnet with low rare earth content specifically comprises the following steps:
step 1, uniformly mixing 2% of zirconium, 0.8% of titanium and the balance of copper by weight;
step 2, mixing 15 wt% of praseodymium, 16 wt% of neodymium, 1.5 wt% of boron and the balance of iron materials to obtain a main phase mixture, adding an alloy mixture accounting for 5 wt% of the main phase mixture into the main phase mixture to obtain a neodymium iron boron mixture, repeatedly smelting the neodymium iron boron mixture for 4 times under the protection of argon gas, and rapidly solidifying and casting the molten material to obtain a neodymium iron boron cast sheet during the last smelting;
step 3, carrying out hydrogen breaking and vacuum pumping dehydrogenation treatment on the neodymium iron boron cast sheet, and then crushing the neodymium iron boron cast sheet into neodymium iron boron powder with the particle size of 2.5-3.8 microns through an airflow mill; wherein, the dehydrogenation treatment temperature is 680 ℃, and the dehydrogenation time is 4.5 h;
step 4, pressing and molding neodymium iron boron powder in an oriented magnetic field of 2.1T to obtain a pressed compact, sintering the pressed compact at 1120 ℃ for 8h at a heating rate of 8-10 ℃/min, and then performing primary tempering and secondary tempering to obtain a neodymium iron boron magnet F; wherein, the time of the first-stage tempering is 4h, and the temperature is 950 ℃; the time of the secondary tempering is 4 hours, the temperature is 600 ℃, and argon is filled for cooling during cooling.
The remanence Br of the neodymium iron boron magnet F is: 12.39 KGs; coercivity Hcb is: 11.70 KOe; the magnetic energy product BH (max) is: 36.31 MGOe.
Comparative example 2:
the preparation method of the neodymium iron boron magnet with low rare earth content specifically comprises the following steps:
step 1, mixing 14% of praseodymium, 18% of neodymium, 0.9% of boron and the balance of iron according to the weight percentage to obtain a main phase mixture, then adding 0.075% of zirconium in the total weight of the main phase mixture into the main phase mixture to obtain a neodymium iron boron mixture, repeatedly smelting the neodymium iron boron mixture for 3 times under the protection of argon, and rapidly solidifying and casting the molten material during the last smelting to obtain a neodymium iron boron casting sheet;
step 2, carrying out hydrogen breaking and vacuum pumping dehydrogenation treatment on the neodymium iron boron cast sheet, and then crushing the neodymium iron boron cast sheet into neodymium iron boron powder with the particle size of 2.5-3.8 microns through an airflow mill; wherein, the dehydrogenation treatment temperature is 680 ℃, and the dehydrogenation time is 4 h;
step 3, pressing and molding the neodymium iron boron powder in an oriented magnetic field of 2.1T to obtain a pressed compact, sintering the pressed compact at 1115 ℃ for 9 hours at a heating rate of 8-10 ℃/min, and then performing primary tempering and secondary tempering to obtain a neodymium iron boron magnet G; wherein, the time of the first-stage tempering is 3.5h, and the temperature is 980 ℃; the time of the secondary tempering is 3 hours, the temperature is 620 ℃, and argon is filled for cooling during cooling.
The remanence Br of the neodymium iron boron magnet G is: 11.57 KGs; coercivity Hcb is: 11.08 KOe; the magnetic energy product BH (max) is: 34.18 MGOe.
Comparative example 3:
the preparation method of the neodymium iron boron magnet with low rare earth content specifically comprises the following steps:
step 1, mixing 10% of praseodymium, 15% of neodymium, 1.2% of boron and the balance of iron according to the weight percentage to obtain a main phase mixture, adding 0.03% of titanium of the total weight of neodymium iron boron into the neodymium iron boron mixture to obtain a neodymium iron boron mixture, repeatedly smelting the neodymium iron boron mixture for 6 times under the protection of argon gas, and rapidly solidifying and casting the molten material during the last smelting to obtain a neodymium iron boron casting sheet;
step 3, carrying out hydrogen breaking and vacuum pumping dehydrogenation treatment on the neodymium iron boron cast sheet, and then crushing the neodymium iron boron cast sheet into neodymium iron boron powder with the particle size of 2.5-3.8 microns through an airflow mill; wherein the dehydrogenation treatment temperature is 660 ℃, and the dehydrogenation time is 3 h;
step 4, pressing and molding neodymium iron boron powder in an oriented magnetic field of 2.1T to obtain a pressed compact, sintering the pressed compact at 1110 ℃ for 7 hours at a heating rate of 8-10 ℃/min, and then performing primary tempering and secondary tempering to obtain a neodymium iron boron magnet H; wherein, the time of the first-stage tempering is 4h, and the temperature is 950 ℃; the time of the secondary tempering is 3.5h, the temperature is 600 ℃, and argon is filled for cooling during cooling.
The remanence Br of the neodymium iron boron magnet H is: 11.92 KGs; coercivity Hcb is: 11.16 KOe; the magnetic energy product BH (max) is: 35.86 MGOe.
Comparative example 4:
the preparation method of the neodymium iron boron magnet with low rare earth content specifically comprises the following steps:
step 1, mixing materials of praseodymium accounting for 12 weight percent, neodymium accounting for 14 weight percent, boron accounting for 0.8 weight percent and iron accounting for the balance to obtain a main phase mixture, adding copper accounting for 3.9 weight percent of the total weight of the main phase mixture into the main phase mixture to obtain a neodymium iron boron mixture, repeatedly smelting the neodymium iron boron mixture for 6 times under the protection of argon, and rapidly solidifying and casting the molten materials to obtain neodymium iron boron casting sheets;
step 2, carrying out hydrogen breaking and vacuum pumping dehydrogenation treatment on the neodymium iron boron cast sheet, and then crushing the neodymium iron boron cast sheet into neodymium iron boron powder with the particle size of 2.5-3.8 microns through an airflow mill; wherein, the dehydrogenation treatment temperature is 680 ℃, and the dehydrogenation time is 4 h;
step 3, pressing and molding neodymium iron boron powder in an oriented magnetic field of 2.1T to obtain a pressed compact, sintering the pressed compact at 1120 ℃ for 9 hours at a heating rate of 8-10 ℃/min, and then performing primary tempering and secondary tempering to obtain a neodymium iron boron magnet I; wherein, the time of the first-stage tempering is 4h, and the temperature is 900 ℃; the time of the secondary tempering is 4 hours, the temperature is 600 ℃, and argon is filled for cooling during cooling.
The remanence Br of the neodymium iron boron magnet I is as follows: 10.63 KGs; coercivity Hcb is: 9.84 KOe; the magnetic energy product BH (max) is: 32.47 MGOe.
Compared with the neodymium iron boron magnet with Cu, Zr and Ti added, the neodymium iron boron magnet with Cu, Zr and Ti added is obviously improved in magnetic force, and meanwhile, compared with the neodymium iron boron magnet prepared by directly adding Cu, Zr and Ti into raw materials, the neodymium iron boron magnet prepared by firstly preparing Cu, Zr and Ti into alloy is better in magnetic property.
In summary, according to the preparation method of the neodymium iron boron magnet with low rare earth content provided by the invention, Dy and Tb are not added in the preparation process, and the alloy grain boundary of Cu, Zr and Ti is added to be matched with high-temperature sintering at the temperature higher than 1100 ℃, so that the movement of the grain boundary of the main phase is limited by the alloy grain boundary of Cu, Zr and Ti, the growth of crystal grains in the main phase is hindered, and the magnetic exchange among the crystal grains in the main phase is blocked. And then the coercive force and the working temperature of the neodymium iron boron magnet are improved, the preparation of the magnet with high thermal stability is facilitated, meanwhile, rare earth metals Dy and Tb are not used, and the preparation cost of the magnet is greatly reduced.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or directly or indirectly applied to the related technical field are included in the scope of the present invention.
Claims (6)
1. The preparation method of the neodymium iron boron magnet with low rare earth content is characterized by comprising the following steps:
step 1, mixing materials prepared by 1.5-3% of zirconium, 0.5-2% of titanium and the balance of copper in percentage by weight, then repeatedly smelting for many times under the protection of argon, and rapidly solidifying and casting the molten material when smelting for the last time to obtain an alloy casting sheet;
step 2, mixing materials which are prepared according to the weight percentage of 10-15% of praseodymium, 13-18% of neodymium, 0.8-1.5% of boron and the balance of iron, then smelting under the protection of argon, and rapidly solidifying the molten materials to obtain a main phase alloy cast sheet;
step 3, respectively carrying out hydrogen fracturing on the alloy casting sheet and the main phase casting sheet to obtain alloy powder and main phase powder;
step 4, adding alloy powder accounting for 2-5% of the total weight of the main phase powder into the main phase powder, fully and uniformly mixing, and crushing the mixture into neodymium iron boron powder with the particle size of 2.5-3.8 microns through an airflow mill;
and 5, pressing and molding the neodymium iron boron powder in an oriented magnetic field of 2.1T to obtain a pressed compact, sintering the pressed compact at 1110-1120 ℃ for 7-9h at the heating rate of 8-10 ℃/min, and then performing primary tempering and secondary tempering to obtain the neodymium iron boron magnet.
2. The method for preparing a neodymium iron boron magnet with low rare earth content according to claim 1, wherein in the step 1, the content of zirconium is 2%, and the content of titanium is 0.8%.
3. The method of claim 1, wherein in the step 2, the content of praseodymium is 14%, the content of neodymium is 18%, and the content of boron is 0.9%.
4. The method for preparing a neodymium iron boron magnet with low rare earth content according to claim 1, wherein the smelting times in the step 1 are 3-6 times.
5. The method for preparing a neodymium-iron-boron magnet with low rare earth content according to claim 1, characterized in that after the hydrogen breaking in the step 3 is finished, the method further comprises a vacuum-pumping dehydrogenation treatment, wherein the dehydrogenation treatment temperature is 680 ℃, and the dehydrogenation time is 4.5 hours.
6. The method for preparing a neodymium-iron-boron magnet with low rare earth content according to claim 1, wherein the time of the primary tempering in the step 5 is 4 hours, and the temperature is 950 ℃; the time of the secondary tempering is 4 hours, the temperature is 600 ℃, and argon is filled for cooling during cooling.
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