CN110289161A - A kind of preparation method of the neodymium iron boron magnetic body of low content of rare earth - Google Patents
A kind of preparation method of the neodymium iron boron magnetic body of low content of rare earth Download PDFInfo
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- CN110289161A CN110289161A CN201910639719.2A CN201910639719A CN110289161A CN 110289161 A CN110289161 A CN 110289161A CN 201910639719 A CN201910639719 A CN 201910639719A CN 110289161 A CN110289161 A CN 110289161A
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- iron boron
- neodymium iron
- magnetic body
- preparation
- main phase
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 99
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 30
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 66
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 36
- 239000000956 alloy Substances 0.000 claims abstract description 36
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 26
- 239000010949 copper Substances 0.000 claims abstract description 24
- 229910052802 copper Inorganic materials 0.000 claims abstract description 23
- 239000010936 titanium Substances 0.000 claims abstract description 20
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 20
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 16
- 229910052796 boron Inorganic materials 0.000 claims abstract description 16
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 15
- 229910052742 iron Inorganic materials 0.000 claims abstract description 15
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims abstract description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 13
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 62
- 239000000203 mixture Substances 0.000 claims description 56
- 239000000463 material Substances 0.000 claims description 42
- 229910052786 argon Inorganic materials 0.000 claims description 31
- 239000007789 gas Substances 0.000 claims description 31
- 238000002844 melting Methods 0.000 claims description 31
- 230000008018 melting Effects 0.000 claims description 31
- 238000000137 annealing Methods 0.000 claims description 23
- FMGSKLZLMKYGDP-USOAJAOKSA-N dehydroepiandrosterone Chemical class C1[C@@H](O)CC[C@]2(C)[C@H]3CC[C@](C)(C(CC4)=O)[C@@H]4[C@@H]3CC=C21 FMGSKLZLMKYGDP-USOAJAOKSA-N 0.000 claims description 22
- 238000005496 tempering Methods 0.000 claims description 21
- 238000005266 casting Methods 0.000 claims description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- 239000001257 hydrogen Substances 0.000 claims description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims description 14
- 238000000748 compression moulding Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 11
- 238000003801 milling Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 4
- 229910052692 Dysprosium Inorganic materials 0.000 abstract description 16
- 229910052771 Terbium Inorganic materials 0.000 abstract description 16
- 239000013078 crystal Substances 0.000 abstract description 16
- 229910001069 Ti alloy Inorganic materials 0.000 abstract description 6
- 238000005245 sintering Methods 0.000 abstract description 6
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 abstract description 3
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 abstract description 3
- 229910000714 At alloy Inorganic materials 0.000 abstract description 2
- 230000005389 magnetism Effects 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- PJBVNQZYNLTGCM-UHFFFAOYSA-N [B].[Fe].[Nd].[B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd].[B].[Fe].[Nd] PJBVNQZYNLTGCM-UHFFFAOYSA-N 0.000 description 1
- 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
- 238000005516 engineering process Methods 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
- 239000002994 raw material Substances 0.000 description 1
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- 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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- 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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- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
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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
- H01F1/04—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 metals or alloys
- 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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- H01F1/057—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
- H01F1/0575—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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- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
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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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Abstract
The invention discloses a kind of preparation methods of the neodymium iron boron magnetic body of low content of rare earth, belong to magnet preparation technical field, the preparation method is using zirconium, titanium and copper at alloy powder, main phase powder is made using praseodymium, neodymium, boron and iron, neodymium iron boron magnetic body is made after then a certain amount of alloy powder is added in main phase powder.The preparation method is during the preparation process, without using dysprosium and terbium, by adding Cu, Zr, Ti alloy, cooperation is higher than 1100 DEG C of high temperature sintering, so that the alloy crystal boundary of Cu, Zr, Ti limit the movement of main phase crystal boundary, the growth of crystal grain in main phase is hindered, the magnetic in main phase between crystal grain has been blocked to exchange.And then the coercivity and operating temperature of neodymium iron boron magnetic body are improved, be conducive to that the high magnet of thermal stability is prepared, while not using rare earth metal Dy and Tb, significantly reduce the cost of magnet preparation.
Description
Technical field
The invention belongs to magnet preparation technical fields, and in particular to a kind of preparation side of the neodymium iron boron magnetic body of low content of rare earth
Method.
Background technique
Neodium magnet (Neodymium magnet) is also referred to as ndfeb magnet (NdFeB magnet), is by neodymium, iron, boron
(Nd2Fe14B) the tetragonal crystal formed.Ndfeb magnet has the characteristics that small in size, light-weight, magnetic strong.Neodymium-iron-boron
Since iron self-discovery, it is gradually applied to the fields such as automobile, computer, information, aviation.But the Curie temperature of ndfeb magnet compared with
Low, as the casting of work high temperature increases, magnetism can weaken.In order to change this characteristic of ndfeb magnet, the prior art
In by addition dysprosium (Dy) and terbium (Tb) Lai Tigao neodium magnet coercive force, improve the thermal stability and magnetism under its high temperature.
Dy and Tb is rare earth metal, and content is low compared with other metals, and answering extensively with ndfeb magnet in recent years
With the yield of Dy and Tb also persistently rise, so that Dy and Tb become expensive raw material.If in the preparation of ndfeb magnet
It can reduce the usage amount of Dy and Tb in the process or without using Dy and Tb, then the cost of ndfeb magnet can be greatly reduced.It is existing
Although there is the preparation method having in technology by adding cobalt (Co) Lai Tigao ndfeb magnet, the addition of Co will also result in magnetic
Property reduce the problem of.
Summary of the invention
In order to overcome the defects of the prior art described above, it is not used the technical problems to be solved by the present invention are: providing one kind
Dysprosium and terbium, and the preparation method of the neodymium iron boron magnetic body of the higher low content of rare earth of operating temperature.
In order to solve the above-mentioned technical problem, a kind of the technical solution adopted by the present invention are as follows: neodymium-iron-boron of low content of rare earth
The preparation method of body, comprising the following steps:
Step 1, the zirconium of percentage composition 1.5-3% by weight, 0.5-2% titanium, surplus be copper material mix, then exist
It carries out multiple melt back under the protection of argon gas, the material of fusing is subjected to rapid hardening slab when last time melting, is closed
Golden slab；
Step 2, the praseodymium of percentage composition 10-15% by weight, the neodymium of 13-18%, 0.8-1.5% boron, surplus is iron
Material mixing, then carries out melting under the protection of argon gas, and the material of fusing is carried out rapid hardening slab when melting, obtains main phase casting
Piece；
Alloy casting piece and main phase slab are carried out hydrogen respectively and break by step 3, obtain alloy powder and main phase powder；
Step 4, the alloy powder that 2-5% is added in main phase powder simultaneously mix well, then are broken for 2.5- through airflow milling
3.8 μm of neodymium iron boron powder；
Step 5, by the compression moulding in the alignment magnetic field of 2.1T of neodymium iron boron powder, green compact is obtained, by green compact in 1110-
1120 DEG C of sintering 7-9h, the rate of heat addition are 8-10 DEG C/min, then using level-one tempering and second annealing, obtain neodymium-iron-boron
Body.
The beneficial effects of the present invention are: the preparation method of the neodymium iron boron magnetic body of low content of rare earth provided by the invention,
Dy and Tb are not added in preparation process, by adding Cu, Zr, Ti alloy, cooperation is higher than 1100 DEG C of high temperature sintering, so that Cu,
The alloy crystal boundary of Zr, Ti limit the movement of main phase crystal boundary, hinder the growth of crystal grain in main phase, blocked in main phase crystal grain it
Between magnetic exchange.And then the coercivity and operating temperature of neodymium iron boron magnetic body are improved, be conducive to thermal stability is prepared high
Magnet, while rare earth metal Dy and Tb are not used, significantly reduce the cost of magnet preparation.
Specific embodiment
To explain the technical content, the achieved purpose and the effect of the present invention in detail, it is explained below in conjunction with embodiment.
The most critical design of the present invention is: replacing Dy and Tb using Cu, Zr, Ti alloy, rectifying for neodymium iron boron magnetic body is promoted
Stupid power and operating temperature.
The present invention provides a kind of preparation method of the neodymium iron boron magnetic body of low content of rare earth, comprising the following steps:
Step 1, the zirconium of percentage composition 1.5-3% by weight, 0.5-2% titanium, surplus be copper material mix, then exist
It carries out multiple melt back under the protection of argon gas, the material of fusing is subjected to rapid hardening slab when last time melting, is closed
Golden slab；
Step 2, the praseodymium of percentage composition 10-15% by weight, the neodymium of 13-18%, 0.8-1.5% boron, surplus is iron
Material mixing, then carries out melting under the protection of argon gas, and the material of fusing is carried out rapid hardening slab when melting, obtains main phase casting
Piece；
Alloy casting piece and main phase slab are carried out hydrogen respectively and break by step 3, obtain alloy powder and main phase powder；
Step 4, the alloy powder that 2-5% is added in main phase powder simultaneously mix well, then are broken for 2.5- through airflow milling
3.8 μm of neodymium iron boron powder；
Step 5, by the compression moulding in the alignment magnetic field of 2.1T of neodymium iron boron powder, green compact is obtained, by green compact in 1110-
1120 DEG C of sintering 7-9h, the rate of heat addition are 8-10 DEG C/min, then using level-one tempering and second annealing, obtain neodymium-iron-boron
Body.
As can be seen from the above description, the beneficial effects of the present invention are: the neodymium-iron-boron of low content of rare earth provided by the invention
The preparation method of body, does not add Dy and Tb during the preparation process, and by adding Cu, Zr, Ti alloy, cooperation is higher than 1100 DEG C of height
Temperature sintering, so that the alloy crystal boundary of Cu, Zr, Ti limit the movement of main phase crystal boundary, hinders the growth of crystal grain in main phase, blocks
Magnetic exchange in main phase between crystal grain.And then the coercivity and operating temperature of neodymium iron boron magnetic body are improved, be conducive to be prepared into
The magnet high to thermal stability, while rare earth metal Dy and Tb are not used, significantly reduce the cost of magnet preparation.
Further, the content of zirconium is 2% in the step 1, and the content of titanium is 0.8%.
Further, the content of praseodymium is 14% in the step 2, and the content of neodymium is 18%, and the content of boron is 0.9%.
Further, the number of melting is 3-6 times in the step 1.Guarantee the mixed uniformity by multiple melting.
It further, further include vacuumizing Dehydroepiandrosterone derivative after the hydrogen of the step 3 is broken, Dehydroepiandrosterone derivative temperature 680
DEG C, dehydrogenation time 4.5h.
Further, the time that level-one is tempered in the step 5 is 4h, and temperature is 950 DEG C；The time of second annealing is
4h, temperature are 600 DEG C, wherein are filled with argon gas when cooling and are cooled down.
Embodiment 1:
The preparation method of the neodymium iron boron magnetic body of low content of rare earth, specifically includes the following steps:
Step 1, the zirconium of percentage composition 2% by weight, 0.8% titanium, surplus be copper material mix, then in argon gas
The material of fusing is carried out rapid hardening slab when last time melting, obtains alloy casting piece by the lower melt back for carrying out 4 times of protection；
Step 2, the praseodymium of percentage composition 15% by weight, 16% neodymium, 1.5% boron, surplus are that the material of iron mixes, so
It carries out melting under the protection of argon gas afterwards, the material of fusing is subjected to rapid hardening slab when melting, obtains main phase slab；
Step 3, that alloy casting piece and main phase slab carry out to hydrogen respectively is broken and after vacuumizing Dehydroepiandrosterone derivative, obtains alloy powder
With main phase powder；Wherein, 680 DEG C of Dehydroepiandrosterone derivative temperature, dehydrogenation time 4.5h；
Step 4, the alloy powder that main phase powder total weight 5% is added in main phase powder simultaneously mix well, then through air-flow
Mill is broken for 2.5-3.8 μm of neodymium iron boron powder；
Step 5, by the compression moulding in the alignment magnetic field of 2.1T of neodymium iron boron powder, green compact is obtained, by green compact at 1120 DEG C
It is sintered 8h, the rate of heat addition is 8-10 DEG C/min, then using level-one tempering and second annealing, obtains neodymium iron boron magnetic body A；Its
In, the time of level-one tempering is 4h, and temperature is 950 DEG C；The time of second annealing is 4h, and temperature is 600 DEG C, wherein when cooling
Argon gas is filled with to be cooled down.
The remanent magnetism Br of above-mentioned neodymium iron boron magnetic body A are as follows: 13.58KGs；Coercivity H b are as follows: 12.93KOe；Magnetic energy product BH (max)
Are as follows: 40.23MGOe.
Embodiment 2:
The preparation method of the neodymium iron boron magnetic body of low content of rare earth, specifically includes the following steps:
Step 1, the zirconium of percentage composition 2.5% by weight, 2% titanium, surplus be copper material mix, then in argon gas
The material of fusing is carried out rapid hardening slab when last time melting, obtains alloy casting piece by the lower melt back for carrying out 3 times of protection；
Step 2, the praseodymium of percentage composition 14% by weight, 18% neodymium, 0.9% boron, surplus are that the material of iron mixes, so
It carries out melting under the protection of argon gas afterwards, the material of fusing is subjected to rapid hardening slab when melting, obtains main phase slab；
Step 3, that alloy casting piece and main phase slab carry out to hydrogen respectively is broken and after vacuumizing Dehydroepiandrosterone derivative, obtains alloy powder
With main phase powder；Wherein, 680 DEG C of Dehydroepiandrosterone derivative temperature, dehydrogenation time 4h；
Step 4, the alloy powder that main phase powder total weight 3% is added in main phase powder simultaneously mix well, then through air-flow
Mill is broken for 2.5-3.8 μm of neodymium iron boron powder；
Step 5, by the compression moulding in the alignment magnetic field of 2.1T of neodymium iron boron powder, green compact is obtained, by green compact at 1115 DEG C
It is sintered 9h, the rate of heat addition is 8-10 DEG C/min, then using level-one tempering and second annealing, obtains neodymium iron boron magnetic body B；Its
In, the time of level-one tempering is 3.5h, and temperature is 980 DEG C；The time of second annealing is 3h, and temperature is 620 DEG C, wherein cooling
When be filled with argon gas and cooled down.
The remanent magnetism Br of above-mentioned neodymium iron boron magnetic body B are as follows: 12.81KGs；Coercivity H b are as follows: 12.20KOe；Magnetic energy product BH (max)
Are as follows: 38.64MGOe.
Embodiment 3:
The preparation method of the neodymium iron boron magnetic body of low content of rare earth, specifically includes the following steps:
Step 1, the zirconium of percentage composition 3% by weight, 1.5% titanium, surplus be copper material mix, then in argon gas
The material of fusing is carried out rapid hardening slab when last time melting, obtains alloy casting piece by the lower melt back for carrying out 6 times of protection；
Step 2, the praseodymium of percentage composition 10% by weight, 15% neodymium, 1.2% boron, surplus are that the material of iron mixes, so
It carries out melting under the protection of argon gas afterwards, the material of fusing is subjected to rapid hardening slab when melting, obtains main phase slab；
Step 3, that alloy casting piece and main phase slab carry out to hydrogen respectively is broken and after vacuumizing Dehydroepiandrosterone derivative, obtains alloy powder
With main phase powder；Wherein, 660 DEG C of Dehydroepiandrosterone derivative temperature, dehydrogenation time 3h；
Step 4, the alloy powder that main phase powder total weight 5% is added in main phase powder simultaneously mix well, then through air-flow
Mill is broken for 2.5-3.8 μm of neodymium iron boron powder；
Step 5, by the compression moulding in the alignment magnetic field of 2.1T of neodymium iron boron powder, green compact is obtained, by green compact at 1110 DEG C
It is sintered 7h, the rate of heat addition is 8-10 DEG C/min, then using level-one tempering and second annealing, obtains neodymium iron boron magnetic body C；Its
In, the time of level-one tempering is 4h, and temperature is 950 DEG C；The time of second annealing is 3.5h, and temperature is 600 DEG C, wherein cooling
When be filled with argon gas and cooled down.
The remanent magnetism Br of above-mentioned neodymium iron boron magnetic body C are as follows: 12.62KGs；Coercivity H b are as follows: 12.07KOe；Magnetic energy product BH (max)
Are as follows: 36.82MGOe.
Embodiment 4:
The preparation method of the neodymium iron boron magnetic body of low content of rare earth, specifically includes the following steps:
Step 1, the zirconium of percentage composition 1.8% by weight, 0.5% titanium, surplus be copper material mix, then in argon gas
Protection under carry out 6 melt backs, the material of fusing is subjected to rapid hardening slab when last time melting, obtains alloy casting
Piece；
Step 2, the praseodymium of percentage composition 12% by weight, 14% neodymium, 0.8% boron, surplus are that the material of iron mixes, so
It carries out melting under the protection of argon gas afterwards, the material of fusing is subjected to rapid hardening slab when melting, obtains main phase slab；
Step 3, that alloy casting piece and main phase slab carry out to hydrogen respectively is broken and after vacuumizing Dehydroepiandrosterone derivative, obtains alloy powder
With main phase powder；Wherein, 680 DEG C of Dehydroepiandrosterone derivative temperature, dehydrogenation time 4h；
Step 4, the alloy powder that main phase powder total weight 5% is added in main phase powder simultaneously mix well, then through air-flow
Mill is broken for 2.5-3.8 μm of neodymium iron boron powder；
Step 5, by the compression moulding in the alignment magnetic field of 2.1T of neodymium iron boron powder, green compact is obtained, by green compact at 1120 DEG C
It is sintered 9h, the rate of heat addition is 8-10 DEG C/min, then using level-one tempering and second annealing, obtains neodymium iron boron magnetic body D；Its
In, the time of level-one tempering is 4h, and temperature is 900 DEG C；The time of second annealing is 4h, and temperature is 600 DEG C, wherein when cooling
Argon gas is filled with to be cooled down.
The remanent magnetism Br of above-mentioned neodymium iron boron magnetic body D are as follows: 13.24KGs；Coercivity H b are as follows: 12.74KOe；Magnetic energy product BH (max)
Are as follows: 39.88MGOe.
Embodiment 5:
The preparation method of the neodymium iron boron magnetic body of low content of rare earth, specifically includes the following steps:
Step 1, the zirconium of percentage composition 1.5% by weight, 1% titanium, surplus be copper material mix, then in argon gas
The material of fusing is carried out rapid hardening slab when last time melting, obtains alloy casting piece by the lower melt back for carrying out 5 times of protection；
Step 2, the praseodymium of percentage composition 13% by weight, 13% neodymium, 1% boron, surplus are that the material of iron mixes, then
It carries out melting under the protection of argon gas, the material of fusing is subjected to rapid hardening slab when melting, obtains main phase slab；
Step 3, that alloy casting piece and main phase slab carry out to hydrogen respectively is broken and after vacuumizing Dehydroepiandrosterone derivative, obtains alloy powder
With main phase powder；Wherein, 680 DEG C of Dehydroepiandrosterone derivative temperature, dehydrogenation time 4.5h；
Step 4, the alloy powder that main phase powder total weight 5% is added in main phase powder simultaneously mix well, then through air-flow
Mill is broken for 2.5-3.8 μm of neodymium iron boron powder；
Step 5, by the compression moulding in the alignment magnetic field of 2.1T of neodymium iron boron powder, green compact is obtained, by green compact at 1120 DEG C
It is sintered 7h, the rate of heat addition is 8-10 DEG C/min, then using level-one tempering and second annealing, obtains neodymium iron boron magnetic body E；Its
In, the time of level-one tempering is 4h, and temperature is 950 DEG C；The time of second annealing is 4h, and temperature is 600 DEG C, wherein when cooling
Argon gas is filled with to be cooled down.
The remanent magnetism Br of above-mentioned neodymium iron boron magnetic body E are as follows: 13.06KGs；Coercivity H b are as follows: 12.56KOe；Magnetic energy product BH (max)
Are as follows: 38.58MGOe.
Comparative example 1:
The preparation method of the neodymium iron boron magnetic body of low content of rare earth, specifically includes the following steps:
Step 1, the zirconium of percentage composition 2% by weight, 0.8% titanium, surplus be copper material be uniformly mixed；
Step 2, the praseodymium of percentage composition 15% by weight, 16% neodymium, 1.5% boron, surplus are that the material of iron mixes, and are obtained
To main phase mixture, the alloy mixture of main phase total weight of the mixture 5% is then added in main phase mixture, obtains neodymium iron boron
Neodymium iron boron mixture, is carried out 4 melt backs by mixture under the protection of argon gas, by the material of fusing when last time melting
Material carries out rapid hardening slab, obtains neodymium iron boron slab；
Step 3, that neodymium iron boron slab is carried out to hydrogen is broken and after vacuumizing Dehydroepiandrosterone derivative, then is broken for 2.5-3.8 μ through airflow milling
The neodymium iron boron powder of m；Wherein, 680 DEG C of Dehydroepiandrosterone derivative temperature, dehydrogenation time 4.5h；
Step 4, by the compression moulding in the alignment magnetic field of 2.1T of neodymium iron boron powder, green compact is obtained, by green compact at 1120 DEG C
It is sintered 8h, the rate of heat addition is 8-10 DEG C/min, then using level-one tempering and second annealing, obtains neodymium iron boron magnetic body F；Its
In, the time of level-one tempering is 4h, and temperature is 950 DEG C；The time of second annealing is 4h, and temperature is 600 DEG C, wherein when cooling
Argon gas is filled with to be cooled down.
The remanent magnetism Br of above-mentioned neodymium iron boron magnetic body F are as follows: 12.39KGs；Coercivity H b are as follows: 11.70KOe；Magnetic energy product BH (max)
Are as follows: 36.31MGOe.
Comparative example 2:
The preparation method of the neodymium iron boron magnetic body of low content of rare earth, specifically includes the following steps:
Step 1, the praseodymium of percentage composition 14% by weight, 18% neodymium, 0.9% boron, surplus are that the material of iron mixes, and are obtained
To main phase mixture, the zirconium of main phase total weight of the mixture 0.075% is then added in main phase mixture, obtains neodymium iron boron mixing
Neodymium iron boron mixture, is carried out 3 melt backs by object under the protection of argon gas, when last time melting by the material of fusing into
Scanning frequency coagulates slab, obtains neodymium iron boron slab；
Step 2, that neodymium iron boron slab is carried out to hydrogen is broken and after vacuumizing Dehydroepiandrosterone derivative, then is broken for 2.5-3.8 μ through airflow milling
The neodymium iron boron powder of m；Wherein, 680 DEG C of Dehydroepiandrosterone derivative temperature, dehydrogenation time 4h；
Step 3, by the compression moulding in the alignment magnetic field of 2.1T of neodymium iron boron powder, green compact is obtained, by green compact at 1115 DEG C
It is sintered 9h, the rate of heat addition is 8-10 DEG C/min, then using level-one tempering and second annealing, obtains neodymium iron boron magnetic body G；Its
In, the time of level-one tempering is 3.5h, and temperature is 980 DEG C；The time of second annealing is 3h, and temperature is 620 DEG C, wherein cooling
When be filled with argon gas and cooled down.
The remanent magnetism Br of above-mentioned neodymium iron boron magnetic body G are as follows: 11.57KGs；Coercivity H b are as follows: 11.08KOe；Magnetic energy product BH (max)
Are as follows: 34.18MGOe.
Comparative example 3:
The preparation method of the neodymium iron boron magnetic body of low content of rare earth, specifically includes the following steps:
Step 1, the praseodymium of percentage composition 10% by weight, 15% neodymium, 1.2% boron, surplus are that the material of iron mixes, and are obtained
To main phase mixture, the titanium of neodymium iron boron total weight 0.03% is added in neodymium iron boron mixture, obtains neodymium iron boron mixture, it will
Neodymium iron boron mixture carries out 6 melt backs under the protection of argon gas, and the material of fusing is carried out speed when last time melting
Solidifying slab, obtains neodymium iron boron slab；
Step 3, that neodymium iron boron slab is carried out to hydrogen is broken and after vacuumizing Dehydroepiandrosterone derivative, then is broken for 2.5-3.8 μ through airflow milling
The neodymium iron boron powder of m；Wherein, 660 DEG C of Dehydroepiandrosterone derivative temperature, dehydrogenation time 3h；
Step 4, by the compression moulding in the alignment magnetic field of 2.1T of neodymium iron boron powder, green compact is obtained, by green compact at 1110 DEG C
It is sintered 7h, the rate of heat addition is 8-10 DEG C/min, then using level-one tempering and second annealing, obtains neodymium iron boron magnetic body H；Its
In, the time of level-one tempering is 4h, and temperature is 950 DEG C；The time of second annealing is 3.5h, and temperature is 600 DEG C, wherein cooling
When be filled with argon gas and cooled down.
The remanent magnetism Br of above-mentioned neodymium iron boron magnetic body H are as follows: 11.92KGs；Coercivity H b are as follows: 11.16KOe；Magnetic energy product BH (max)
Are as follows: 35.86MGOe.
Comparative example 4:
The preparation method of the neodymium iron boron magnetic body of low content of rare earth, specifically includes the following steps:
Step 1, the praseodymium of percentage composition 12% by weight, 14% neodymium, 0.8% boron, surplus are that the material of iron mixes, and are obtained
To main phase mixture, the copper of main phase total weight of the mixture 3.9% is added in main phase mixture, obtains neodymium iron boron mixture, it will
Neodymium iron boron mixture carries out 6 melt backs under the protection of argon gas, and the material of fusing is carried out rapid hardening slab when melting, is obtained
To neodymium iron boron slab；
Step 2, that neodymium iron boron slab is carried out to hydrogen is broken and after vacuumizing Dehydroepiandrosterone derivative, then is broken for 2.5-3.8 μ through airflow milling
The neodymium iron boron powder of m；Wherein, 680 DEG C of Dehydroepiandrosterone derivative temperature, dehydrogenation time 4h；
Step 3, by the compression moulding in the alignment magnetic field of 2.1T of neodymium iron boron powder, green compact is obtained, by green compact at 1120 DEG C
It is sintered 9h, the rate of heat addition is 8-10 DEG C/min, then using level-one tempering and second annealing, obtains neodymium iron boron magnetic body I；Its
In, the time of level-one tempering is 4h, and temperature is 900 DEG C；The time of second annealing is 4h, and temperature is 600 DEG C, wherein when cooling
Argon gas is filled with to be cooled down.
The remanent magnetism Br of above-mentioned neodymium iron boron magnetic body I are as follows: 10.63KGs；Coercivity H b are as follows: 9.84KOe；Magnetic energy product BH (max)
Are as follows: 32.47MGOe.
The neodymium iron boron magnetic body of Cu, Zr, Ti alloy is added, compared to the neodymium iron boron magnetic body for being individually added into Cu, Zr, Ti, magnetic force
It is obviously improved, while compared to Cu, Zr, Ti addition are directly prepared into neodymium iron boron magnetic body in the feed, Cu, Zr, Ti first being made
It is standby at alloy the neodymium iron boron magnetic body being prepared it is magnetic more preferably.
In conclusion the preparation method of the neodymium iron boron magnetic body of low content of rare earth provided by the invention, during the preparation process not
Dy and Tb is added, by adding Cu, Zr, Ti alloy, cooperation is higher than 1100 DEG C of high temperature sintering, so that the alloy of Cu, Zr, Ti are brilliant
Boundary limits the movement of main phase crystal boundary, hinders the growth of crystal grain in main phase, and the magnetic in main phase between crystal grain has been blocked to exchange.Into
And the coercivity and operating temperature of neodymium iron boron magnetic body are improved, be conducive to that the high magnet of thermal stability is prepared, while not making
With rare earth metal Dy and Tb, the cost of magnet preparation is significantly reduced.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalents made by bright description are applied directly or indirectly in relevant technical field, are similarly included in this hair
In bright scope of patent protection.
Claims (6)
1. a kind of preparation method of the neodymium iron boron magnetic body of low content of rare earth, which comprises the following steps:
Step 1, the zirconium of percentage composition 1.5-3% by weight, 0.5-2% titanium, surplus be copper material mix, then in argon gas
Protection under carry out multiple melt back, the material of fusing is subjected to rapid hardening slab when last time melting, obtains alloy casting
Piece；
Step 2, the praseodymium of percentage composition 10-15% by weight, the neodymium of 13-18%, 0.8-1.5% boron, surplus be iron material
Mixing, then carries out melting under the protection of argon gas, and the material of fusing is carried out rapid hardening slab when melting, obtains main-phase alloy casting
Piece；
Alloy casting piece and main phase slab are carried out hydrogen respectively and break by step 3, obtain alloy powder and main phase powder；
Step 4, the alloy powder that main phase powder total weight 2-5% is added in main phase powder simultaneously mix well, then through airflow milling
It is broken for 2.5-3.8 μm of neodymium iron boron powder；
Step 5, by the compression moulding in the alignment magnetic field of 2.1T of neodymium iron boron powder, green compact is obtained, by green compact at 1110-1120 DEG C
It is sintered 7-9h, the rate of heat addition is 8-10 DEG C/min, then using level-one tempering and second annealing, obtains neodymium iron boron magnetic body.
2. the preparation method of the neodymium iron boron magnetic body of low content of rare earth according to claim 1, which is characterized in that the step
The content of zirconium is 2% in 1, and the content of titanium is 0.8%.
3. the preparation method of the neodymium iron boron magnetic body of low content of rare earth according to claim 1, which is characterized in that the step
The content of praseodymium is 14% in 2, and the content of neodymium is 18%, and the content of boron is 0.9%.
4. the preparation method of the neodymium iron boron magnetic body of low content of rare earth according to claim 1, which is characterized in that the step
The number of melting is 3-6 times in 1.
5. the preparation method of the neodymium iron boron magnetic body of low content of rare earth according to claim 1, which is characterized in that the step
It further include vacuumizing Dehydroepiandrosterone derivative after 3 hydrogen is broken, 680 DEG C of Dehydroepiandrosterone derivative temperature, dehydrogenation time 4.5h.
6. the preparation method of the neodymium iron boron magnetic body of low content of rare earth according to claim 1, which is characterized in that the step
The time that level-one is tempered in 5 is 4h, and temperature is 950 DEG C；The time of second annealing is 4h, and temperature is 600 DEG C, wherein when cooling
Argon gas is filled with to be cooled down.
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| CN117727520A (en) * | 2023-11-20 | 2024-03-19 | 山东上达稀土材料有限公司 | A highly magnetic and corrosion-resistant sintered cerium-rich permanent magnet and its preparation method |
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| CN117727520A (en) * | 2023-11-20 | 2024-03-19 | 山东上达稀土材料有限公司 | A highly magnetic and corrosion-resistant sintered cerium-rich permanent magnet and its preparation method |
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