CN1083257A - The preparation method of powder of permanent-magnet material - Google Patents
The preparation method of powder of permanent-magnet material Download PDFInfo
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- CN1083257A CN1083257A CN 93107808 CN93107808A CN1083257A CN 1083257 A CN1083257 A CN 1083257A CN 93107808 CN93107808 CN 93107808 CN 93107808 A CN93107808 A CN 93107808A CN 1083257 A CN1083257 A CN 1083257A
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Abstract
The invention belongs to the preparation field of permanent magnetic material.Be specially adapted to the preparation method of rare earth-filtering metal-interstitial atom type permanent-magnet powder.Adopting the inventive method to prepare samarium iron nitrogen magnetic is samarium cast iron casting ingot to be carried out the homogenizing processing after carry out static pressurized hydrogen heat treatment and static pressurized nitrogen heat treatment again after being crushed to powder particle＜30 μ m earlier, carries out ball milling at last again and makes particle size at 1-3 μ m.Adopting the inventive method to produce the permanent magnetism powder, to have technology compared with prior art simple, characteristics such as the with short production cycle and comprehensive magnetic property height of magnetic.
Description
The invention belongs to the preparation field of permanent magnetic material.Be specially adapted to the preparation method of rare earth-transition metal-interstitial atom type permanent magnetic material.
At present rare earth permanent-magnetic material has been found multiplely, and samarium iron nitrogen permanent magnetic material is one of the most promising rare earth permanent-magnetic material continue neodymium iron boron after, also is that current magnetics circle is both at home and abroad made great efforts the field developed.Main research direction is to improve the preparation method of magnetic property and magnet powder.What the preparation method of rare earth permanent-magnet powder was at present main has four kinds, and 1 is mechanical alloying method; 2 is the HDDR method; 3 is melt-quenching method.Though adopt the magnetic of method for preparing that higher coercive force is arranged, remanent magnetism is very low.Therefore magnetic energy product is also lower, and the preparation technology of magnetic is also complicated.Nearest Japanese TDK company introduction a kind of prior powder metallurgy legal system be equipped with samarium iron nitrogen permanent-magnet powder, though higher magnetic property is arranged by the prepared Magnaglo of this method, Br=13KG, iHc=10.4KOe, (BH) amx=30MGOe, its technology is: 1, carried out hydrogenation treatment in 4 hours 250 ℃ of insulations under high-purity flowing hydrogen; 2, under high-purity flowing nitrogen, carried out nitrogen treatment in 63 hours 450 ℃ of insulations; 3, under high-purity mobile argon gas, carried out annealing in process in 3 hours 450 ℃ of insulations.And then adopt ball milling to make powder fining.The main shortcoming of said method is a complex process, and the production cycle is long and uneconomical etc.
The objective of the invention is to propose a kind of method for preparing high-performance rare-earth-transition metal-interstitial atom type powder of permanent-magnet material, this method has characteristics such as production technology is simple, economic and with short production cycle.
According to the preparation method of the high-performance rare-earth permanent-magnetic powder that the object of the invention proposed, at the characteristic of samarium iron permanent-magnet material powder, details are as follows for this preparation method that we adopted.At first the samarium ferroalloy ingot after the melting is carried out homogenizing annealing and handle under 1050 ℃～1150 ℃ high temperature, the annealing in process time is 8～16 hours, adopts mechanical or manual method alloy pig to be crushed to＜particle of 30 μ m then.Hydrogen heat processing in the methods of the invention is to adopt high-purity static pressuring method, and treatment temperature is 200 ℃～300 ℃, and temperature retention time is 2～4 hours.Nitrogenize heat treatment adopts high-purity static pressurized nitrogen to heat-treat, and its heating-up temperature is 470 ℃～550 ℃ and is incubated 2～6 hours.In high-purity static pressurized hydrogen that is adopted in the methods of the invention and the nitrogen Technology for Heating Processing each gas pressure all＞1bar.Carry out ball milling again after waiting this material to handle, make the permanent-magnet powder granularity at last at 1-3 μ m.Samarium iron nitrogen permanent magnetic material adopts above-mentioned preparation method's production, can obtain very high magnetic property economically, and its performance is Br=12.2～12.8KG, iHc=5-9KOe, (BH) max=23-25MGOe.Its reason is that the alloy pig after high-temperature homogenization is handled has uniform interior tissue, carrying out K cryogenic treatment after the alloy pig fragmentation in the hydrogen of＞1bar expands samarium iron compound unit cell volume, particle cracks, very important to the absorption and the diffusion that promote nitrogen-atoms in the subsequent technique, suitably improve nitriding temperature in addition and also be the approach that shortens nitridation time, adopt static atmosphere under the pressure of＞1bar, to help absorption and the diffusion of material hydrogen, nitrogen-atoms.Because hydrogen, nitrogen all are reducibility gas.Hydrogen, nitrogen-atoms will just require the gas concentration of alloy surface and pressure will have enough greatly toward alloy internal penetration and diffusion, can strengthen the affinity of gas atom and alloy like this, reach gas atom diffusion and the purpose of permeating.
The method that adopts the present invention to prepare the rare earth permanent-magnetic material powder has following characteristics compared with prior art.Because the inventive method is still used original equipment.Therefore production equipment does not need reinvestment, and production technology is simple, and is with short production cycle, and the properties of product height.This technology is a kind of preparation method of economical production samarium iron nitrogen high performance permanent magnetic materials powder.
Embodiment
The embodiment of the invention is that the Sm2Fe17 alloy pig is handled under 1050 ℃ of temperature, and temperature retention time 12 hours then through Mechanical Crushing, makes alloy material granularity＜30 μ m.Each technological parameter of the embodiment of the inventive method sees Table 1.Magnetic property by the prepared samarium iron nitrogen magnetic of said method sees Table 2.Can find out that from table 1, table 2 it is simple, with short production cycle that the samarium iron nitrogen magnetic that adopts the inventive method to produce has technology, and advantage such as the comprehensive magnetic property of magnetic is good.
In an embodiment, table 1 is static pressurized hydrogen, heat treated each technological parameter of alloy under the blanket of nitrogen.Table 2 is by prepared each the magnetic property data of samarium iron nitrogen magnetic of the inventive method.
Table 1
| The technology sequence number | Hydrogen treat | Nitrogen treatment | Ball milling | ||||
| Temperature ℃ | Time hour | Air pressure bar | Temperature ℃ | Time hour | Air pressure bar | Hour | |
| 1 | 280 | 2.5 | 1.1 | 470 | 4 | 1.1 | 3 |
| 2 | 230 | 4 | 1.7 | 520 | 2 | 1.3 | 1.5 |
| 3 | 250 | 3 | 1.2 | 480 | 3 | 1.2 | 2 |
Table 2
| The performance sequence number | Br?KGs | iHc?KOe | (BH)max?MGOe |
| 1 | 12.2 | 7.9 | 23.2 |
| 2 | 12.8 | 5.2 | 24 |
| 3 | 12.5 | 6.3 | 23.6 |
Claims (5)
1, a kind of method for preparing rare earth-transition metal-interstitial atom type permanent-magnet powder, be specially adapted to the preparation method of samarium iron nitrogen permanent magnetic alloy powder, after it is characterized in that earlier samarium cast iron casting ingot being carried out high-temperature homogenization handles, broken again ingot casting is to the particle of＜30 μ m, and under static state pressurization atmosphere, carry out hydrogen heat and handle and nitrogen heat treatment, carry out the powder ball milling after to be heated again, making powder particle is 1-3 μ m.
2, according to the described method of claim 1, the temperature that it is characterized in that the homogenizing processing of steel ingot is 1040 ℃-1080 ℃ insulations 8-16 hour.
3,, it is characterized in that the heat treated temperature of static pressurized hydrogen is at 2-4 hour 200 ℃ of-300 ℃ of temperature retention times according to the described method of claim 1.
4,, it is characterized in that the heat treated temperature of static pressurized nitrogen is at 2-6 hour 470 ℃ of-550 ℃ of temperature retention times according to the described method of claim 1.
5, according to claim 1,3,4 described methods, it is characterized in that static state adds to depress carries out hydrogen and nitrogen heat treatment, each gas pressure all＞1bar.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93107808 CN1083257A (en) | 1993-07-08 | 1993-07-08 | The preparation method of powder of permanent-magnet material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93107808 CN1083257A (en) | 1993-07-08 | 1993-07-08 | The preparation method of powder of permanent-magnet material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1083257A true CN1083257A (en) | 1994-03-02 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93107808 Pending CN1083257A (en) | 1993-07-08 | 1993-07-08 | The preparation method of powder of permanent-magnet material |
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| CN (1) | CN1083257A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100565117C (en) * | 2002-07-19 | 2009-12-02 | 内山工业株式会社 | Magnetic coder |
| CN102101120A (en) * | 2009-12-21 | 2011-06-22 | 上海爱普生磁性器件有限公司 | Method for recycling boned neodymium iron boron permanent magnet defective product |
| CN104384493A (en) * | 2014-10-22 | 2015-03-04 | 浙江工业大学 | Method for preparing Sm2Fe17Nx magnetic powder by taking ammonium carbonate as nitrogen source positive pressure samarium iron nitride alloy |
-
1993
- 1993-07-08 CN CN 93107808 patent/CN1083257A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100565117C (en) * | 2002-07-19 | 2009-12-02 | 内山工业株式会社 | Magnetic coder |
| CN102101120A (en) * | 2009-12-21 | 2011-06-22 | 上海爱普生磁性器件有限公司 | Method for recycling boned neodymium iron boron permanent magnet defective product |
| CN104384493A (en) * | 2014-10-22 | 2015-03-04 | 浙江工业大学 | Method for preparing Sm2Fe17Nx magnetic powder by taking ammonium carbonate as nitrogen source positive pressure samarium iron nitride alloy |
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