CN1082097C - Process for preparing permanent-magnetic material of Sm-Fe-C compound - Google Patents
Process for preparing permanent-magnetic material of Sm-Fe-C compound Download PDFInfo
- Publication number
- CN1082097C CN1082097C CN99113092A CN99113092A CN1082097C CN 1082097 C CN1082097 C CN 1082097C CN 99113092 A CN99113092 A CN 99113092A CN 99113092 A CN99113092 A CN 99113092A CN 1082097 C CN1082097 C CN 1082097C
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- CN
- China
- Prior art keywords
- magnetic material
- pure
- hours
- ball milling
- carried out
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 150000001875 compounds Chemical class 0.000 title claims abstract description 11
- 239000000696 magnetic material Substances 0.000 title claims abstract description 9
- 229910017112 Fe—C Inorganic materials 0.000 title claims description 7
- 238000004519 manufacturing process Methods 0.000 title 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 6
- 239000010439 graphite Substances 0.000 claims abstract description 6
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- 238000005551 mechanical alloying Methods 0.000 claims abstract description 6
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 6
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 229910052786 argon Inorganic materials 0.000 claims abstract description 3
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 3
- 150000003624 transition metals Chemical class 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000007669 thermal treatment Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- 230000005389 magnetism Effects 0.000 abstract description 6
- 239000007789 gas Substances 0.000 abstract 1
- 239000004615 ingredient Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000000137 annealing Methods 0.000 description 9
- 239000000956 alloy Substances 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 229910052772 Samarium Inorganic materials 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- -1 rare-earth transition metal Chemical class 0.000 description 3
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 2
- 229910001172 neodymium magnet Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Landscapes
- Hard Magnetic Materials (AREA)
Abstract
The present invention relates to a method for preparing a permanent magnetic material with samarium-ferrum-carbon compounds. The related permanent magnetic material is represented as Sm [y](FeCOTi) [100-1.5y]C[0.5y], wherein 'y' is more than or equal to 8 and less than or equal to 20. Basic processes for preparing the permanent magnetic material comprise the following steps that pure rare earth, pure iron, pure transition metal and graphite based on ingredients of a compound are proportioned, the raw materials are mechanically alloyed in a ball milling manner for 3 to 20 hours, and heat treatment is carried out for 0.1 to 10 hours under a vacuum condition at the temperature of 650 to 950 DEG C. The method is characterized in that after mechanical alloying and heat treatment, ball milling under the protection of argon gas is carried out again for 0.3 to 4 hours, and vacuum heat treatment at the temperature of 300 to 650 DEG C is carried out for 0.3 to 30 hours. The method has a simple process, and produced Sm2Fe17C has good intrinsic magnetism and high thermal stability.
Description
The present invention relates to a kind of method for preparing rare-earth transition metal carbide permanent magnet material.
Although the Nd-Fe-B permanent magnet has good magnetic performance such as high saturated magnetic energy product, the weakness that its Curie temperature is low has limited the range of application of this material.The clear 62-170455 of patent JP of for example relevant Nd-Fe-B, the clear 62-151541 of JP, the clear 62-152108 of JP, the clear 62-149108 of JP, the clear 62-151542 of JP, the clear 62-158854 of JP, the clear 62-156248 of JP, the clear 62-124702 of JP, the clear 62-177149 of JP, the clear 62-174905 of JP etc.In recent years, the progress of exploring the novel permanent magnetic material in the world wide is rapid, but relevant work mainly concentrates on 2: 17,2: 14: 1 type ternary compounds, wherein the new way of exploring novel cpd has been opened up in the discovery of Sm-Fe-C (N) type compound, discover that carbon enters Curie temperature and the magnetocrystalline anisotropy that 2: 17 lattices can greatly improve compound as interstitial atom, owing to contain carboritride at pyrolytic decomposition, and special nitriding carbon process limited the application of Sm-Fe-C, and the research work of this respect remains a new breakthrough.
The object of the present invention is to provide a kind of method for preparing permanent-magnetic material of Sm-Fe-C compound, this method technology is simple, and the prepared Sm that goes out
2Fe
17C has good intrinsic magnetic properties and higher thermostability.
The invention provides a kind of method for preparing permanent-magnetic material of Sm-Fe-C compound, related permanent magnet material is Sm
y(FeCoTi)
100-1.5yC
0.5y, 8≤y≤20 wherein; The primary process of its preparation is that pure rare earth, pure iron, pure transition metal, graphite are prepared burden by the compound composition; mode with ball milling is carried out mechanical alloying; 3～20 hours ball milling time; thermal treatment is 0.1～10 hour under 650～950 ℃ of vacuum conditions; it is characterized in that: adopting above-mentioned mechanical alloying method to make powder diameter is 1～3 micron; it is carried out after the above-mentioned thermal treatment ball milling 0.3～4 hour under argon shield again, 300～650 ℃ of vacuum heat treatment 0.3～30 hour.
Because Sm
2Fe
14The direction of magnetization of C is easy face, Sm
2Fe
17Direction of magnetization also be easy face, when adopting common preparation method to prepare Sm
yFe
100-1.5yC
0.5y, during (8≤y≤20) alloy, formation be 2: 14: 1 phase Sm
2Fe
14C and Sm
2Fe
17, and the few Sm of content
2Fe
17So C is the permanent magnetism performance that alloy does not have.The reason that causes this consequence is that annealing temperature is too high among the common preparation method, studies show that, carbon just might enter 2: 17 interstitial sites in mutually and form the Sm with magnetic easy axis direction only when being lower than 650 ℃
2Fe
17C
x(0≤x≤3), this has just formed contradiction, and annealing temperature is crossed the low crystallization that is unfavorable for alloy again, can not prepare the alloy with good permanent magnetism performance equally.Method provided by the invention is by twice ball milling, and twice annealed technology has solved an above-mentioned difficult problem well.In a word, the present invention has overcome the weakness of carburization process, directly prepares the rare-earth transition metal carbide by the mechanical alloying method, and Zhi Bei rare-earth transition metal carbide not only has good intrinsic magnetic properties in this way, and has higher thermostability.
Below by embodiment in detail the present invention is described in detail.
Embodiment 1
Press standard component Sm with the powder of pure samarium, pure iron and graphite
14Fe
79C
7(atomic percent) batching is placed in the ball grinder, ratio of grinding media to material 23: 1, and 12 millimeters of spherical diameter, rotating speed 15 meter per seconds, 54 millimeters of jar diameters, 100 millimeters of jar rotating diameters, ball milling be after 5 hours, 1～3 micron of particle diameter; 800 ℃ of vacuum annealings, placed ball grinder again in 30 minutes, ground 1 hour, 550 ℃ of vacuum annealings 30 minutes, get final product to such an extent that principal phase is Sm
2Fe
17The permanent-magnet powder of C, its permanent magnetism performance is (BH)
Max=87.5KJ/m
3(11MGOe), M
e=11.8kGs, M
r=9.35kGs.
iH
c=215kA/m (2.7kOe) can prepare magnet by the powder bonded method, without secondary ball milling and annealed Sm
14Fe
79C
7Maximum magnetic energy product (BH)
Max=0.01MGOe, HCJ
iH
c=0.17kOe, (annealing 35 minutes for 800 ℃).
Embodiment 2
Powder with pure samarium, pure iron, pure titanium and graphite is pressed standard component Sm
14Fe
77Ti
2C
7(atomic percent) batching is placed in the ball grinder, grinds 5 hours, 850 ℃ of vacuum annealings, places ball grinder again in 30 minutes, grinds 1 hour, 600 ℃ of vacuum annealings 30 minutes, gets final product to such an extent that principal phase is Sm
2(Fe
17-zTi
z) C
xPermanent-magnet powder, its permanent magnetism performance is (BH)
Max=65.0kJ/m
3(8.17MGOe), M
e=1.02T, M
r=0.81T,
iH
c=207kA/m (2.60kOe) can prepare magnet by the powder bonded method.
Embodiment 3
Powder with pure samarium, pure iron, pure cobalt and graphite is pressed standard component Sm
14Fe
75Co
4C
7(atomic percent) batching is placed in the ball grinder, grinds 5 hours, 850 ℃ of vacuum annealings, places ball grinder again in 30 minutes, grinds 1 hour, 600 ℃ of vacuum annealings 30 minutes, gets final product to such an extent that principal phase is Sm
2(Fe
17-uCo
u) permanent-magnet powder of Cx, its permanent magnetism performance is (BH)
Max=51.6kJ/m
3(6.48MGOe) .M
e=1.14T, M
r=0.86T,
iH
c=135.3kA/m (1.70kOe) can prepare magnet by the powder bonded method.
Claims (1)
1, a kind of method for preparing permanent-magnetic material of Sm-Fe-C compound, related permanent magnet material is Sm
y(FeCoTi)
100-1.5yC
0.5y, 8≤y≤20 wherein; The primary process of its preparation is that pure rare earth, pure iron, pure transition metal, graphite are prepared burden by the compound composition; mode with ball milling is carried out mechanical alloying; 3～20 hours ball milling time; thermal treatment is 0.1～10 hour under 650～950 ℃ of vacuum conditions; it is characterized in that: adopting above-mentioned mechanical alloying method to make powder diameter is 1～3 micron; it is carried out after the above-mentioned thermal treatment ball milling 0.3～4 hour under argon shield again, 300～650 ℃ of vacuum heat treatment 0.3～30 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99113092A CN1082097C (en) | 1999-07-14 | 1999-07-14 | Process for preparing permanent-magnetic material of Sm-Fe-C compound |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99113092A CN1082097C (en) | 1999-07-14 | 1999-07-14 | Process for preparing permanent-magnetic material of Sm-Fe-C compound |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1281055A CN1281055A (en) | 2001-01-24 |
| CN1082097C true CN1082097C (en) | 2002-04-03 |
Family
ID=5276324
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99113092A Expired - Fee Related CN1082097C (en) | 1999-07-14 | 1999-07-14 | Process for preparing permanent-magnetic material of Sm-Fe-C compound |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1082097C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111933375A (en) * | 2020-07-09 | 2020-11-13 | 浙江工业大学 | Novel samarium-iron-carbon-based anisotropic magnetic powder |
| CN114682788A (en) * | 2021-12-21 | 2022-07-01 | 北京航空航天大学 | Samarium iron/graphene nano composite material for electromagnetic wave absorption and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62177149A (en) * | 1986-01-29 | 1987-08-04 | Sumitomo Special Metals Co Ltd | Production of permanent magnet material |
-
1999
- 1999-07-14 CN CN99113092A patent/CN1082097C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62177149A (en) * | 1986-01-29 | 1987-08-04 | Sumitomo Special Metals Co Ltd | Production of permanent magnet material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1281055A (en) | 2001-01-24 |
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