CN1953111A - Preparation method of sintered rare earth Fe-N permanent magnet - Google Patents
Preparation method of sintered rare earth Fe-N permanent magnet Download PDFInfo
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- CN1953111A CN1953111A CN200510021893.9A CN200510021893A CN1953111A CN 1953111 A CN1953111 A CN 1953111A CN 200510021893 A CN200510021893 A CN 200510021893A CN 1953111 A CN1953111 A CN 1953111A
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Abstract
The invention relates to a method for preparing sinter rare-earth iron nitrogen permanent-magnetic material. Wherein, the invention is characterized in that: first compressing the rare-earth iron nitrogen permanent-magnetic material into initial blank; putting it the space between two punching heads of electric field activate pressure auxiliary sinter device to be clamped; in vacuum or protective gas, at the pressure as 0-110MPa, and the sinter temperature-increase speed as 0-2000Deg. C/s, the sinter temperature as 300-550Deg. C, and the temperature-insulated time is 1-60mins, processing electric field sinter activation to obtain rare-earth iron nitrogen permanent-magnetic element. The invention has instant temperature increase, to sinter the powder into block with high pressure and short time, at low temperature, without damaging the micro organism and property of powder.
Description
Technical field
The present invention is a kind of sintered rare earth Fe-N permanent magnetic material preparation method.
Background technology
People such as nineteen ninety Coey find Sm
2Fe
17N
xThe type compound has excellent permanent magnetism performance, and meanwhile professor Yang Yingchang of China has also reported NdFe
12N
xThe type rare earth permanent-magnetic material is shown great attention to so the rare earth Fe-N permanent magnetic material has caused both at home and abroad.They have the following advantages: content of rare earth is low, Curie temperature is higher (Sm wherein
2Fe
17N
xCurie temperature be 476 ℃, exceed Nd
2Fe
14Nearly 160 ℃ of B), very high magnetocrystalline anisotropy field (14T), and good thermal stability, non-oxidizability and decay resistance, magnetic property and Nd
2Fe
14B is that rare earth permanent magnet is suitable, is the rare earth permanent-magnetic material of future generation of the tool potentiality of generally acknowledging, thereby has become Recent study and hot of research and development.
Japan takes the lead in having realized Sm in calendar year 2001
2Fe
17N
xThe industrialization of permanent magnetism powder, companies such as TDK, Hitachi, system steel institute have produced compression forming in succession, injection and calendering formation Sm
2Fe
17N
xRare-earth permanent magnet, and put on market; The NdFe of the Yang Yingchang professor independent research of China
12N
xThe type rare earth permanent magnet powder has also been realized suitability for industrialized production in succession, and compression molding, injection moulding neodymium Fe-N permanent magnet and neodymium iron nitrogen permanent magnetism powder have dropped into production application with the ferrite permanent-magnet complex.Bonding rare earth iron nitrogen permanent magnetic material has successfully been realized suitability for industrialized production.Compare with bonded permanent magnet as everyone knows, do not contain non magnetic phase in the sintered magnet, density is high thereby have high magnetic property and a mechanical property.In order to obtain high performance rare earth Fe-N permanent magnetic material permanent magnetic material, people have carried out a large amount of explorations at the sintered rare earth Fe-N permanent magnetic material.But nitrogen all can take place break away from lattice and decompose owing to the rare earth Fe-N permanent magnetic material is higher than 600 ℃ or low temperature long-time heating in temperature, cause material lose magnetism can, thereby sintered rare earth Fe-N permanent magnet prepares always, and difficulty has breakthrough.This defective has greatly limited the novel permanent magnetic material of this high performance-price ratio in industrial application.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of preparation method of novel sintered rare earth Fe-N permanent magnetic material is provided.
Technical scheme of the present invention is: at first will make by oneself or any one commercially available rare earth Fe-N permanent magnetic material is pressed into base just in advance; with between two drifts of its electric field activation pressure assisted sintering (the field-activated pressure-assisted synthesis (FAPAS)) equipment of packing into and clamp (see figure 1); after the operating room vacuumized; the high vacuum or backfill N2 or the inert protective gas that keep cavity; apply the pressure of 0-110MPa and carry out electric field burning activation knot, be cooled to room temperature after insulation a period of time and can obtain rare earth Fe-N permanent magnet.
It is 0-1750A that electric field activation pressure assisted sintering (the field-activated pressure-assisted synthesis (FAPAS)) equipment has pressure system, the direct current that uniaxial tension is 0-110MPa, and voltage is energy delivery system, vacuum systems and the cooling system of 10V.The heating rate scope of this equipment is 0-2000 ℃/s, and sintering range is 0-2000 ℃.Heating rate and sintering temperature are set the after-current size can load and regulate (typical sintering temperature curve is seen Fig. 2) automatically according to heating rate and sintering temperature, and its basic principle is exactly to make sample produce a large amount of heat (Q=I by logical big electric current under the booster action of pressure
2Rt) and sinter piece into.Thereby it has a moment and heats up, can be under lower temperature the piece that sinters into by high pressure and the powder of sintering realization in short-term, and can not destroy the microstructure of material and the characteristics of performance, be particularly suitable for the preparation of sintered rare earth Fe-N permanent magnetic material.
Above-mentioned sintering isotropism or anisotropic rare earth Fe-N permanent magnet, its sintering range is: 300-550 ℃.
Above-mentioned sintering isotropism or anisotropic rare earth Fe-N permanent magnet, its temperature retention time is: 1-60 minute.
Description of drawings:
Fig. 1. be the equipment schematic diagram of electric field activation pressure assisted sintering
Fig. 2. be typical electric field activated sintering process temperature time graph
Embodiment
Embodiment 1:
Adopt isotropic Sm of HDDR method preparation in the present embodiment
2Fe
17N
x(x≤3) magnetic is pressed into base just in advance on press, the density of first base is 3.3g/cm
3, formed body all is the sample of φ 10mm.Also clamp between two drifts with its electric field activation pressure assisted sintering equipment of packing into, to operating room's pumping high vacuum, and backfill N
2Gas carries out sintering then to 0.1MPa.Apply the pressure of 15MPa in the sintering process, sintering temperature is 500 ℃, and heating rate is 1200 ℃/s, and temperature retention time 5 minutes is cooled to room temperature and takes out magnet after sintering is finished.This sintering isotropism Sm
2Fe
17N
xThe density of magnet is 5.7g/cm
3, magnetic property is remanent magnetism Br=0.64T, magnetic strength coercive force H
Cb=410kA/m, HCJ H
Cj=1100kA/m, maximum magnetic energy product (BH)
m=61kJ/m
3
Embodiment 2:
In the present embodiment, adopt anisotropic NdFe
12N
x(x≤3) magnetic, the compression moulding on press of orientation back is first base, the density of first base is 4.3g/cm
3, formed body all is the sample of φ 10mm.NdFe
12N
xAfter just base is packed into, to operating room's pumping high vacuum, sintering in electric field activation pressure assisted sintering equipment, apply the pressure of 50MPa in the sintering process, sintering temperature is 450 ℃, and heating rate is 1000 ℃/s, temperature retention time 12 minutes is cooled to room temperature and takes out magnet after sintering is finished.This sintering anisotropy NdFe
12N
xThe density of magnet is 6.23g/cm
3, magnetic property is remanent magnetism Br=0.70T, magnetic strength coercive force H
Cb=285kA/m, HCJ H
Cj=390kA/m, maximum magnetic energy product (BH)
m=75kJ/m
3
Embodiment 3:
In the present embodiment, adopt anisotropic Sm
2Fe
17N
x(x≤3) magnetic, the compression moulding on press of orientation back is first base, the density of first base is 3.0g/cm
3, formed body all is the sample of φ 10mm.First base is packed in the electric field activation pressure assisted sintering equipment into backfill Ar behind operating room's pumping high vacuum
2Gas carries out sintering to 0.1MPa.Apply the pressure of 80MPa in the sintering process, sintering temperature is 400 ℃, and heating rate is 1500 ℃/s, and temperature retention time 30 minutes is cooled to room temperature and takes out magnet after sintering is finished.The anisotropic Sm of this sintering
2Fe
17N
xThe density of magnet is 6.5g/cm
3, magnetic property is remanent magnetism Br=0.74T, magnetic strength coercive force H
Cb=380kA/m, HCJ H
Cj=760kA/m, maximum magnetic energy product (BH)
m=82kJ/m
3
Claims (3)
1, a kind of sintered rare earth Fe-N permanent magnetic material preparation method, it is characterized in that processing step is as follows: also clamp between two drifts of the electric field of at first the first base of the prior compression moulding of rare earth Fe-N permanent magnetic material being packed into activation pressure assisted sintering equipment, at high vacuum or backfill backfill N
2Or after the inert protective gas, sample is applied the pressure of 0-110MPa and carries out electric field and burn activation and form rare earth Fe-N permanent magnet.
2, the described sintered rare earth Fe-N permanent magnetic material of claim 1 preparation method is characterized in that the heating rate of electric field activation pressure assisted sintering is 0-2000 ℃/s, moulding pressure 0-110MPa, and sintering range is 300-550 ℃, temperature retention time is 1-60 minute.
3, according to claim 1 and the described sintered rare earth Fe-N permanent magnetic material of claim 2 preparation method, it is characterized in that the sintered rare earth Fe-N permanent magnetic material for preparing comprises: self-control or any one commercially available samarium iron nitrogen are permanent-magnet powder, and self-control or any one commercially available neodymium iron nitrogen are at least a in the permanent-magnet powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200510021893.9A CN1953111A (en) | 2005-10-18 | 2005-10-18 | Preparation method of sintered rare earth Fe-N permanent magnet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200510021893.9A CN1953111A (en) | 2005-10-18 | 2005-10-18 | Preparation method of sintered rare earth Fe-N permanent magnet |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1953111A true CN1953111A (en) | 2007-04-25 |
Family
ID=38059374
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200510021893.9A Pending CN1953111A (en) | 2005-10-18 | 2005-10-18 | Preparation method of sintered rare earth Fe-N permanent magnet |
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|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102310196A (en) * | 2011-01-23 | 2012-01-11 | 四川大学 | Method for manufacturing micro parts by sintering under electric field action |
-
2005
- 2005-10-18 CN CN200510021893.9A patent/CN1953111A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102310196A (en) * | 2011-01-23 | 2012-01-11 | 四川大学 | Method for manufacturing micro parts by sintering under electric field action |
| CN102310196B (en) * | 2011-01-23 | 2012-10-31 | 四川大学 | Method for manufacturing micro parts by sintering under electric field action |
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| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |