CN101045966A - Process of sintering and synthesizing RE permanent magnetic alloy - Google Patents
Process of sintering and synthesizing RE permanent magnetic alloy Download PDFInfo
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- CN101045966A CN101045966A CN 200610066463 CN200610066463A CN101045966A CN 101045966 A CN101045966 A CN 101045966A CN 200610066463 CN200610066463 CN 200610066463 CN 200610066463 A CN200610066463 A CN 200610066463A CN 101045966 A CN101045966 A CN 101045966A
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- magnetic alloy
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Abstract
The sintering synthesis process of producing RE permanent magnetic alloy includes setting permanent magnetic alloy blank inside a microwave sintering furnace; adding additive NH4F, NH4N3 and/or NH2NH2, getter Zr84Al16, RE elements of La, Ce, Pr, etc in 1-4 wt%; sintering at microwave frequency of 0.1-500 GHz and temperature of 550-1135 deg.c for 0.1-1.5 hr; ageing in a vacuum sintering electric furnace; cooling to room temperature, post-machining and magnetizing to obtain the RE permanent magnetic alloy. Compared with conventional technological process, the sintering synthesis process of the present invention has the advantages of high performance of the produced RE permanent magnetic alloy, high homogeneity, low power consumption and low production cost.
Description
Technical field
The present invention relates to a kind of synthetic method of RE permanent magnetic alloy, particularly relate to a kind of process of sintering and synthesizing of RE permanent magnetic alloy, belong to metal material field, specifically belong to RE permanent magnetic alloy.
Background technology
Material is the pillar and the milestone of civilization of human society, and permanent magnet material has become one of sign of weighing country's civilization and development degree.What the magnetic property up-to-date in the permanent magnet material, that performance is best was the highest is rare earth permanent-magnetic material.It is the intermetallic compound by combinations such as rare earth element especially Ce, Pr, Nd, Sm and magnesium-yttrium-transition metal: Co, Fe, Ni and Al, Cu, Nb, Ga and non-metallic element C, B, obtains after suitable processing treatment.
Synthesized SmCo in 1987
5Permanent magnet alloy because the valency of Co is expensive, partly replaces Part of Co with Cu, Fe, Zr again, forms Sm, (Co, Cu, Fe, Zr)
7-8Intermetallic compound.Add that for Co B forms the new intermetallic compound of rare-earth iron-boron with Fe again after nineteen eighty-three, become third generation rare earth permanent-magnetic material, through the development of two more than ten years, the rare earth permanent-magnetic material output of China has occupied position first of the world.
In the time of among permanent magnet material successfully is applied to computer, motor, electroacoustic apparatus, nuclear magnetic resonance analyser, engine, transformer, people extremely are concerned about the cost problem of material, promptly under the prerequisite of excellent performance, how to reduce cost also is one of research focus, material cost accounts for variable cost 86%, accounts for 45% of total production cost.When reducing cost, people consider how to reduce utilization rate of raw materials, improve homogeneity, the consistence of material, and this also is the several problems that exist in the current rare earth permanent-magnetic material development.
Summary of the invention
The present invention is directed to the problem in the existing above-mentioned synthesis technique, a kind of, new synthetic process of saving starting material, reducing cost lower than energy consumption in the traditional processing technology is provided.
New technological flow mainly comprises:
1. preparing raw material
The smelting of rare earth alloy difficulty is bigger, because rare earth metal is volatile, the material for preparing is inserted in the medium-frequency induction furnace, vacuumizes, when vacuum tightness reaches 10 again
-2Heat up again behind the Pa, adopt slowly during intensification and heat up, smelting temperature 1350-1450 ℃, be poured in the copper crucible of water-cooled, drop to room temperature.
2. powder process is in the pulverizer under the N gas shiled, by broken in thick, hydrogenation powder process, comminution by gas stream, fine grinding to 3-6 micron powder.
3. the powder of above-mentioned powder process is packed in the mould, make the blank piece at the magnetic field compacted under.
4. above-mentioned blank piece is inserted microwave agglomerating furnace.Use microwave 0.1-500GH
2The microwave oven of frequency adds Zr in stove
84Al
16Powder and Ce, La, Pr, Nd, Pm, Ho, Tm, Yb, Lu, Sc, Sm, Eu, Ga, Tb, Dy, one or more proportionings of Er, Y.Add-on can account for sintered material 1-4%, adds additive: NH again
4F, NH
4N
3, NH
4NH
2A kind of or two kinds, three kinds, addition is to account for the 1-4% that adds material.Blank and additive after getter, the permanent magnetic alloy powder moulding are put into microwave agglomerating furnace simultaneously, extract some out and contain the many gas of oxygen.Synthesis temperature 550-1135 ℃, be incubated 0.1-1.5 hour.Sintering is based on microwave electromagnetic field directly and the interaction of heated medium molecule in microwave agglomerating furnace, make under the effect of medium molecule in microwave electromagnetic field, produce fierce motion, form similar heat of friction, thereby the temperature that forms on the heating object macroscopic view raises.
The microwave power that the material of per unit volume can absorb can be write becomes following formula:
P＝KfE
2Drtgδ
P wherein---the microwave power that the unit material absorbs
K---coefficient
F---microwave frequency
E---microwave electric field intensity
The relative permittivity of Dr---material
Tg δ---loss tangent
Wherein f, E belong to the sign of microwave field characteristic, and Dr, tg δ are the sign that is heated material.
Compare with the vacuum electric furnace sintering with microwave oven sintering, its advantage has following points:
(1) owing to the internal heating characteristics of microwave oven, combustion wave is radially outwards to propagate from the sample center, and it is consistent with the effusion direction of gas, can effectively gas be flushed out, and therefore, sintered products compactness is good.
(2) combustion wave is propagated evenly.
(3) accelerating velocity is fast.
(4) impurity is reduced in the segregation degree of prosperous intergranular circle.
(5) possibility of secondary crystal obviously reduces.
(6) the present invention uses 0.1-500GH in addition except that above-mentioned advantage is arranged
2It is short that the microwave oven of scope has the high wavelength of frequency, and penetrativity is strong, all helps to change and improve the mechanical property of sintered products.
(7) because with this Technology sintering time shortening, so save a large amount of electric energy.
(8) volatilization of minimizing rare earth element, saving rare earths material reduce cost again.
5. timeliness: timeliness in vacuum sintering furnace, vacuum tightness are 10
-2-10
-3Pa, aging temp: 490-1090 ℃, time 1-2 hour.
6. sintering success, the product through overaging enters post-treatment again, the size that needs by the user, is processed into required product.
7. product magnetization is magnetized in the magnet charger greater than 4.5 Gausses.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
With purity is 99.5% metal Pr, Nd, and 99.8% electrical pure iron and boracic are lower than 20% ferro-boron, and chloride Dy at 0.001-2% contains 99.8% Al, Cu by Pr
1.5Nd
11.9Dy
0.5Fe
79.4Al
0.3Cu
0.3B
6.5Cl
0.1Prescription requires to prepare alloy 15kg, and alloy material is inserted in the medium-frequency induction furnace, is evacuated down to 10
-3Pa, roasting refining under argon shield, refining is after 8 minutes; cooling is cast in the crystallizer of water-cooled slightly, and alloy pig is inserted coarse crushing (under the N gas shiled); being crushed to the 3-6 micron through over hydrogenation powder process, chlorine stream, is moulding in the magnetic field of 1.2T in magnetic field, and forming pressure is 2T/cm
2, the blank after the moulding is put into microwave (480GH
2) in the sintering oven, put into getter around in the blank material, the getter total amount is to be sintered 2.5% of blank material.Getter is by Zr
86Al
14With La, Ce, Pr, Nd mishmetal powder constituent, addition is 315g, adds NH again
4F300g.Shut stove, 1090 ℃ of insulations 0.45 hour, behind the taking-up material, again it is inserted vacuum sintering furnace, 1058 ℃ are incubated 58 fens, drop to 585 ℃, 585 ℃ of aging temps, aging time 1.6 hours, drop to room temperature by the customer requirements post-treatment, magnetize under 4-5T magnetic field, obtain high performance permanent magnet material, measuring result is as follows: residual magnetic flux density Br=1.44T.Hci＝1000KA/m，(BH)
m＝397KJ/m
3。
Embodiment 2:
Nd
13Pr
0.4Dy
0.6Al
0.2B
6.5Fe
79.4Cl
0.1Prescription is joined 10kg, and the adding getter is Zr
86, Al
14With Ce, Pr, Sm, add 110g, additive is NH
4N
3, NH
4NH
2, adding 150g, other conditions and method are with embodiment 1.It is as follows that product is measured magnetic property: Br=1.45T, Hci=998KA/m, (BH) max=403KJ/m
3
Claims (5)
1. the process of sintering and synthesizing of a RE permanent magnetic alloy is characterized in that, adopts the permanent magnet alloy molded blank to place the microwave oven of getter and additive to carry out sintering and synthesizes, and places vacuum sintering electric furnace timeliness.
2. the process of sintering and synthesizing of a kind of RE permanent magnetic alloy according to claim 1 is characterized in that, adopts the blank of permanent magnet alloy to place microwave 0.1-500GH in the sintering of permanent magnet alloy
2Sintering in the microwave agglomerating furnace of frequency, 550-1135 ℃ of its sintering temperature is incubated 0.1-1.5 hour.
3. the process of sintering and synthesizing of a kind of RE permanent magnetic alloy according to claim 1 is characterized in that, the alloy that goes out with microwave oven sintering reinstalls and carries out timeliness in the vacuum sintering furnace, and vacuum tightness is 10
-2-10
-3Pa, aging temp are 490-1090 ℃, and soaking time is 1-2 hour.
4. the process of sintering and synthesizing of a kind of RE permanent magnetic alloy according to claim 1 is characterized in that, the additive of putting in the microwave agglomerating furnace is NH
4F, NH
4N
3, NH
4NH
2One or both, three kinds, add-on is for accounting for sinter amount 1-4%.
5. the process of sintering and synthesizing of a kind of RE permanent magnetic alloy according to claim 1 is characterized in that, places the getter Zr of microwave agglomerating furnace
84Al
16, add-on for account for sintered material 1-4% and rare-earth elements La, Le, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, Sc one or more, add-on is for accounting for sintered material 1-4%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100664633A CN100519792C (en) | 2006-03-31 | 2006-03-31 | Process of sintering and synthesizing rare earth permanent magnetic alloy |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100664633A CN100519792C (en) | 2006-03-31 | 2006-03-31 | Process of sintering and synthesizing rare earth permanent magnetic alloy |
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| Publication Number | Publication Date |
|---|---|
| CN101045966A true CN101045966A (en) | 2007-10-03 |
| CN100519792C CN100519792C (en) | 2009-07-29 |
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ID=38770884
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102189258A (en) * | 2011-04-22 | 2011-09-21 | 荆门金钻硬质合金有限责任公司 | Hard alloy online detection control sintering process |
| CN105551788A (en) * | 2016-02-02 | 2016-05-04 | 中磁科技股份有限公司 | Method for improving coercive force of rare earth permanent magnet |
| CN108555240A (en) * | 2017-11-30 | 2018-09-21 | 深圳粤网节能技术服务有限公司 | A kind of microwave casting method |
| CN111430143A (en) * | 2020-04-22 | 2020-07-17 | 安徽吉华新材料有限公司 | Preparation process of rare earth neodymium iron boron permanent magnet |
-
2006
- 2006-03-31 CN CNB2006100664633A patent/CN100519792C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102189258A (en) * | 2011-04-22 | 2011-09-21 | 荆门金钻硬质合金有限责任公司 | Hard alloy online detection control sintering process |
| CN102189258B (en) * | 2011-04-22 | 2014-03-19 | 荆门金钻硬质合金有限责任公司 | Hard alloy online detection control sintering process |
| CN105551788A (en) * | 2016-02-02 | 2016-05-04 | 中磁科技股份有限公司 | Method for improving coercive force of rare earth permanent magnet |
| CN108555240A (en) * | 2017-11-30 | 2018-09-21 | 深圳粤网节能技术服务有限公司 | A kind of microwave casting method |
| CN111430143A (en) * | 2020-04-22 | 2020-07-17 | 安徽吉华新材料有限公司 | Preparation process of rare earth neodymium iron boron permanent magnet |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100519792C (en) | 2009-07-29 |
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Assignee: Shenzhen Feller Magtech Corporation Assignor: Pan Shuming Contract record no.: 2010440000514 Denomination of invention: Process of sintering and synthesizing RE permanent magnetic alloy Granted publication date: 20090729 License type: Exclusive License Open date: 20071003 Record date: 20100518 |
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