CN102290181B - Low-cost sintered rear-earth permanent magnet with high coercive force and high magnetic energy product and preparation method thereof - Google Patents
Low-cost sintered rear-earth permanent magnet with high coercive force and high magnetic energy product and preparation method thereof Download PDFInfo
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- CN102290181B CN102290181B CN201110118478.0A CN201110118478A CN102290181B CN 102290181 B CN102290181 B CN 102290181B CN 201110118478 A CN201110118478 A CN 201110118478A CN 102290181 B CN102290181 B CN 102290181B
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- 238000002360 preparation method Methods 0.000 title claims description 18
- 238000004519 manufacturing process Methods 0.000 title description 3
- 239000010949 copper Substances 0.000 claims abstract description 6
- 239000010955 niobium Substances 0.000 claims abstract description 6
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 4
- 239000004411 aluminium Substances 0.000 claims abstract description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 4
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 4
- 239000010941 cobalt Substances 0.000 claims abstract description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052802 copper Inorganic materials 0.000 claims abstract description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 4
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 4
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 4
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims abstract description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract 2
- 229910052726 zirconium Inorganic materials 0.000 claims abstract 2
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 57
- 150000002910 rare earth metals Chemical class 0.000 claims description 55
- 229910052739 hydrogen Inorganic materials 0.000 claims description 25
- 239000001257 hydrogen Substances 0.000 claims description 25
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 19
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 16
- 239000000470 constituent Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 238000005245 sintering Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 150000002431 hydrogen Chemical class 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 238000005266 casting Methods 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 238000009766 low-temperature sintering Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 230000001737 promoting effect Effects 0.000 claims description 4
- 238000005496 tempering Methods 0.000 claims description 4
- 239000000284 extract Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 229910052692 Dysprosium Inorganic materials 0.000 abstract description 4
- 229910052771 Terbium Inorganic materials 0.000 abstract description 4
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 abstract description 4
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052691 Erbium Inorganic materials 0.000 abstract description 3
- 229910052688 Gadolinium Inorganic materials 0.000 abstract description 3
- 229910052689 Holmium Inorganic materials 0.000 abstract description 3
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 abstract description 3
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 abstract description 3
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 238000004891 communication Methods 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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Abstract
The invention discloses a low-cost sintered rear-earth permanent magnet with high coercive force and a high magnetic energy product, a molecular formula expressing the components of the sintered rear-earth permanent magnet and the content of each component by mass is LRaHRbMcBdFe100-a-b-c-d, wherein LR is at least one of neodymium, praseodymium, cerium and lanthanum, HR is at least one of gadolinium, terbium, dysprosium, holmium and erbium, M is at least one of cobalt, copper, aluminium, zirconium and niobium, moreover, a is larger than or equal to 29 and less than or equal to 32, b is larger than or equal to 0 and less than or equal to 0.2, c is larger than or equal to 1.2 and less than or equal to 3, and d is larger than or equal to 0.6 and less than or equal to 3. Compared with the prior art, the sintered rear-earth permanent magnet has the advantages that: the heavy rear earth in the sintered rear-earth permanent magnet is only less than 0.2 percent by mass, the coercive force reaches more than 15kOe, the magnetic energy product reaches more than 42MGOe, i.e., the sintered rear-earth permanent magnet has no heavy rear earth or extremely little heavy rear earth, high coercive force and a high magnetic energy product, and under the condition that high coercive force and a high magnetic energy product are obtained, the material cost of the sintered rear-earth permanent magnet is greatly reduced.
Description
Technical field
The present invention relates to technical field of magnetic materials, relate in particular to a kind of low-cost high-coercive force high energy product sintered rare-earth permanent magnetic body and preparation method thereof.
Background technology
Rare-earth permanent magnet has the feature of high remanent magnetism, high-coercive force and high energy product, is widely used in the fields such as power electronics, communication, information, motor, communications and transportation, office automation, medicine equipment, military affairs.Through 20 years of researches exploitations, the magnetic energy product of rare-earth permanent magnet is greatly improved, the space but the coercive force of rare-earth permanent magnet still improves a lot.
Adopt to add traditionally heavy rare earth element and obtain the sintering rare-earth permanent magnet of high-coercive force as terbium, dysprosium etc., but heavy rare earth reserves are less, price is very high, cause the cost of sintering rare-earth permanent magnet higher, particularly rare earth rise in price in the recent period, adds heavy rare earth element and causes magnet cost higher.Meanwhile, the deterioration that membership causes magnet remanent magnetism that adds due to heavy rare earth, is not easy to obtain high magnetic energy product.Therefore, in order to save heavy rare earth resource, reduce the production cost of magnet, exploitation is not one of very significant research topic at present containing heavy rare earth or heavy rare earth low content and the permanent magnet with high-coercive force high energy product simultaneously.
Summary of the invention
The technical problem to be solved in the present invention is for the above-mentioned existing state of the art, a kind of low-cost high-coercive force high energy product sintered rare-earth permanent magnetic body is provided, thereby change existing production technology, in order to improve sintered magnet coercive force, consume in a large number heavy rare earth, cause the present situation that magnet cost is higher.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of low-cost high-coercive force high energy product sintered rare-earth permanent magnetic body, the molecular formula that represents its component and each constituent mass content is LR
ahR
bm
cb
dfe
100-a-b-c-dwherein LR is at least one in neodymium (Nd), praseodymium (Pr), cerium (Ce) and lanthanum (La), HR is gadolinium (Gd), terbium (Tb), dysprosium (Dy), at least one in holmium (Ho) and erbium (Er), M is at least one in cobalt (Co), copper (Cu), aluminium (Al), zirconium (Zr) and niobium (Nb), and 29≤a≤32,0≤b≤0.2,1.2≤c≤3,0.6≤d≤3.
Wherein, preferred 0≤b≤0.1 of the content of described HR.
The preparation method of a kind of low-cost high-coercive force high energy product sintered rare-earth permanent magnetic body of the present invention comprises the steps:
Step 1, according to representing the component of sintered rare-earth permanent magnetic body and the molecular formula LR of each constituent mass content
ahR
bm
cb
dfe
100-a-b-c-dpreparation raw material, wherein LR is at least one in neodymium (Nd), praseodymium (Pr), cerium (Ce) and lanthanum (La), HR is gadolinium (Gd), terbium (Tb), dysprosium (Dy), at least one in holmium (Ho) and erbium (Er), M is at least one in cobalt (Co), copper (Cu), aluminium (Al), zirconium (Zr) and niobium (Nb), and and 29≤a≤32,0≤b≤0.2,1.2≤c≤3,0.6≤d≤3.
Step 2, employing strip casting are made rapid-hardening flake by above-mentioned raw materials, then carry out the broken technique of hydrogen, and control dehydrogenation air pressure, after making dehydrogenation, the broken powder hydrogen content of hydrogen is between 1500ppm～3000ppm, the broken laggard promoting the circulation of qi stream of hydrogen grinds magnetic, magnetic is obtained in magnetic field to molded blank after oriented moulding;
Step 3, molded blank is put under inert gas shielding to sintering furnace and carried out low-temperature sintering, sintering temperature, not higher than 980 ℃, is then cooled to room temperature, finally adopts second annealing technique to heat-treat, and obtains sintered rare-earth permanent magnetic body;
The broken technique of hydrogen in described step 2 is about to rapid-hardening flake, and to be placed in hydrogen broken furnace ventilation broken, and detailed process is rapid-hardening flake to be placed in to hydrogen broken furnace to be evacuated to vacuum degree be below 2Pa, at room temperature passes into hydrogen, keeps pressure 1 * 10
5pa～5 * 10
5pa, the time, at 1 hour～4 hours, is cooled to room temperature, then extracts remaining hydrogen out, starts the dehydrogenation that heats up, and dehydrogenating technology adopts 300 ℃～700 ℃ insulations 3 hours～7 hours, and dehydrogenation air pressure is during lower than 90Pa, and dehydrogenation finishes, and stops heating, and is cooled to room temperature.
Oriented moulding in the magnetic field that magnetic in described step 2 is 1.2T～2T in magnetic field intensity.
Sintering process in described step 3 is to heat up 300 ℃～800 ℃, is incubated 0.5 hour～6 hours dehydrogenation gas, is then warming up to 950 ℃～980 ℃ sintering, is incubated 1 hour～5 hours.
Second annealing technique in described step 3 is respectively 800 ℃～890 ℃ and 450 ℃～600 ℃ tempering heat treatments 2 hours～5 hours.
The sintered rare-earth permanent magnetic temperature that described step 3 obtains is that 20 ℃ of official report coercivity H i are more than 15kOe.
Compared with prior art, in sintered rare-earth permanent magnetic body of the present invention, heavy rare earth mass percentage content is only below 0.2%, more than coercive force reaches 15kOe, more than magnetic energy product reaches 42MGOe, realize the sintered rare-earth permanent magnetic body without heavy rare earth or extremely low heavy rare earth, high-coercive force, high energy product, under the condition that obtains high-coercive force high energy product, greatly reduced the cost of material of sintered rare-earth permanent magnetic body.
Embodiment
Following specific embodiment is described in further detail the present invention.
Embodiment 1:
The molecular formula that represents sintered rare-earth permanent magnetic body component and each constituent mass content is Nd
20pr
10co
1cu
0.2al
0.6b
1.2fe
bal, be below the concrete preparation process of this sintered rare-earth permanent magnetic body:
(1) according to molecular formula Nd
20pr
10co
1cu
0.2al
0.6b
1.2fe
balthe component and each constituent mass content preparation raw material that represent;
(2) adopt strip casting that above-mentioned raw materials is made to rapid-hardening flake, then carry out the broken technique of hydrogen, and control dehydrogenation air pressure, making the broken powder hydrogen content of hydrogen after dehydrogenation is 1500ppm, the broken laggard promoting the circulation of qi stream of hydrogen grinds magnetic, magnetic is obtained in magnetic field to molded blank after oriented moulding;
(3) molded blank is put under inert gas shielding to sintering furnace and carried out low-temperature sintering; sintering temperature is 975 ℃; then be cooled to room temperature, finally adopt second annealing technique to heat-treat, tempering heat treatment temperature is 800 ℃ and obtains sintered rare-earth permanent magnetic body with 500 ℃.
The above-mentioned sintered rare-earth permanent magnetic body preparing is processed into Φ 10mm * 10mm small column and tests, test result is as shown in table 1.
Table 1: embodiment 1 magnet properties of sample
Embodiment 2:
The molecular formula that represents sintered rare-earth permanent magnetic body component and each constituent mass content is Nd
30.3c0
1.5cu
0.4al
0.2b
0.9fe
bal, be below the concrete preparation process of this sintered rare-earth permanent magnetic body:
(1) according to molecular formula Nd
30.3co
1.5cu
0.4al
0.2b
0.9fe
balthe component and each constituent mass content preparation raw material that represent;
(2) adopt strip casting that above-mentioned raw materials is made to rapid-hardening flake, then carry out the broken technique of hydrogen, and control dehydrogenation air pressure, making the broken powder hydrogen content of hydrogen after dehydrogenation is 3000ppm, the broken laggard promoting the circulation of qi stream of hydrogen grinds magnetic, magnetic is obtained in magnetic field to molded blank after oriented moulding;
(3) molded blank is put under inert gas shielding to sintering furnace and carried out low-temperature sintering; sintering temperature is 980 ℃; then be cooled to room temperature, finally adopt second annealing technique to heat-treat, tempering heat treatment temperature is 850 ℃ and obtains sintered rare-earth permanent magnetic body with 480 ℃.
The above-mentioned sintered rare-earth permanent magnetic body preparing is processed into Φ 10mm * 10mm small column and tests, test result is as shown in table 2:
Table 2: embodiment 2 magnet properties of sample
Embodiment 3:
The molecular formula that represents sintered rare-earth permanent magnetic body component and each constituent mass content is Nd
20pr
10gd
0.1co
1cu
0.2al
0.6b
1.2fe
bal, be below the preparation process of this sintered rare-earth permanent magnetic body:
(1) according to molecular formula Nd
20pr
10gd
0.1co
1cu
0.2al
0.6b
1.2fe
balthe component and each constituent mass content preparation raw material that represent;
(2) identical with the step (2) in embodiment 1;
(3) identical with the step (3) in embodiment 2.
The above-mentioned sintered rare-earth permanent magnetic body preparing is processed into Φ 10mm * 10mm small column and tests, test result shows that the HCJ Hcj of this sintered rare-earth permanent magnetic body is more than 15kOe, and magnetic energy product is more than 42MGOe.
Embodiment 4:
The molecular formula that represents sintered rare-earth permanent magnetic body component and each constituent mass content is Nd
20pr
10gd
0.1tb
0.1co
1cu
0.2al
0.6b
1.2fe
bal, be below the preparation process of this sintered rare-earth permanent magnetic body:
(1) according to molecular formula Nd
20pr
10gd
0.1tb
0.1co
1cu
0.2al
0.6b
1.2fe
balthe component and each constituent mass content preparation raw material that represent;
(2) identical with the step (2) in embodiment 1;
(3) identical with the step (3) in embodiment 2.
The above-mentioned sintered rare-earth permanent magnetic body preparing is processed into Φ 10mm * 10mm small column and tests, test result shows that the HCJ Hcj of this sintered rare-earth permanent magnetic body is more than 15kOe, and magnetic energy product is more than 42MGOe.
Embodiment 5:
The molecular formula that represents sintered rare-earth permanent magnetic body component and each constituent mass content in the present embodiment, and the preparation method of this sintered rare-earth permanent magnetic body is basic identical with embodiment 4, difference is to replace the Gd element in embodiment 3 with Dy element, and preparing molecular formula is Nd
20pr
10dy
0.1co
1cu
0.2al
0.6b
1.2fe
balsintered rare-earth permanent magnetic body, the HCJ Hcj of this sintered rare-earth permanent magnetic body is more than 10kOe, magnetic energy product is more than 42MGOe.
Embodiment 6:
The molecular formula that represents sintered rare-earth permanent magnetic body component and each constituent mass content in the present embodiment, and the preparation method of this sintered rare-earth permanent magnetic body is basic identical with embodiment 1, difference is to replace the Pr element in embodiment 2 with Ce element, and preparing molecular formula is Nd
20ce
10co
1cu
0.2al
0.6b
1.2fe
balsintered rare-earth permanent magnetic body, the HCJ Hcj of this sintered rare-earth permanent magnetic body is more than 10kOe, magnetic energy product is more than 42MGOe.
Embodiment 7:
The molecular formula that represents sintered rare-earth permanent magnetic body component and each constituent mass content in the present embodiment, and the preparation method of this sintered rare-earth permanent magnetic body is basic identical with embodiment 2, difference is to replace the Nd element in embodiment 2 with La element, and preparing molecular formula is La
30.3co
1.5cu
0.4al
0.2b
0.9fe
balsintered rare-earth permanent magnetic body, the HCJ Hcj of this sintered rare-earth permanent magnetic body is more than 10kOe, magnetic energy product is more than 42MGOe.
Claims (4)
1. low-cost high-coercive force high energy product sintered permanent magnet, is characterized in that: the molecular formula that represents its component and each constituent mass content is LR
am
cb
dfe
100-a-b-c-d, wherein LR is at least one in neodymium, praseodymium, cerium and lanthanum, M is at least one in cobalt, copper, aluminium, zirconium and niobium, and 29≤a≤32,1.2≤c≤3,0.6≤d≤3;
Its HCJ is more than 15kOe, and magnetic energy product is more than 42MGOe;
Its preparation method comprises the steps:
Step 1, according to representing the component of this sintered permanent magnet and the molecular formula LR of each constituent mass content
am
cb
dfe
100-a-b-c-dpreparation raw material;
Step 2, employing strip casting are made rapid-hardening flake by above-mentioned raw materials, then carry out the broken technique of hydrogen, and control dehydrogenation air pressure, after making dehydrogenation, the broken powder hydrogen content of hydrogen is between 1500ppm～3000ppm, the broken laggard promoting the circulation of qi stream of hydrogen grinds magnetic, magnetic is obtained in magnetic field to molded blank after oriented moulding;
Step 3, molded blank is put under inert gas shielding to sintering furnace and carried out low-temperature sintering, sintering temperature, not higher than 980 ℃, is then cooled to room temperature, finally adopts second annealing technique to heat-treat, and obtains sintered rare-earth permanent magnetic body.
2. low-cost high-coercive force high energy product sintered permanent magnet according to claim 1, it is characterized in that: the broken technique of hydrogen in described step 2 is rapid-hardening flake to be placed in to hydrogen broken furnace to be evacuated to vacuum degree be below 2Pa, at room temperature pass into hydrogen, keep pressure 1 * 10
5pa～5 * 10
5pa, the time, at 1 hour～4 hours, is cooled to room temperature, then extracts remaining hydrogen out, starts the dehydrogenation that heats up, dehydrogenating technology adopts 300 ℃～700 ℃ insulations 3 hours～7 hours, dehydrogenation air pressure during lower than 90Pa dehydrogenation finish, stop heating, be cooled to room temperature.
3. low-cost high-coercive force high energy product sintered permanent magnet according to claim 1, it is characterized in that: the sintering process in described step 3 is to heat up 300 ℃～800 ℃, be incubated 0.5 hour～6 hours dehydrogenation gas, be then warming up to 950 ℃～980 ℃ sintering, be incubated 1 hour～5 hours.
4. low-cost high-coercive force high energy product sintered permanent magnet according to claim 1, is characterized in that: the second annealing technique in described step 3 is respectively 800 ℃～890 ℃ and 450 ℃～600 ℃ tempering heat treatments 2 hours～5 hours.
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|---|---|---|---|
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| CN1557005A (en) * | 2002-09-30 | 2004-12-22 | Tdk株式会社 | R-T-B based rare earth element permanent magnet |
| CN1557004A (en) * | 2002-09-30 | 2004-12-22 | Tdk��ʽ���� | R-T-B based rare earth element permanent magnet and magnet composition |
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| CN1557005A (en) * | 2002-09-30 | 2004-12-22 | Tdk株式会社 | R-T-B based rare earth element permanent magnet |
| CN1557004A (en) * | 2002-09-30 | 2004-12-22 | Tdk��ʽ���� | R-T-B based rare earth element permanent magnet and magnet composition |
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