CN103537684B - Production method for samarium cobalt alloy powder - Google Patents
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Abstract
The invention discloses a production method for samarium cobalt alloy powder. The production method for the samarium cobalt alloy powder comprises weighing samarium, cobalt, iron, copper, zirconium and heavy rare earth element metal salt in proportion, preparing a salt solution and a salt-mixture solution, adding a little acid or alkali to control a PH (Potential of Hydrogen) value to be between 4 and 9, simultaneously adding surface active agent and dispersing agent which account 1 to 5 % of the mass of the metal salt in the metal salt solution, performing spray drying at the temperature between 300 and 350 DEG C to produce composite powder precursor, performing low temperature calcine at the temperature between 200 and 300 DEG C, performing two-step restoring on the precursor under hydrogen atmosphere with the temperature between 400 to 800 DEG C, ball-milling the restored powder to obtain the samarium cobalt alloy powder. The samarium cobalt alloy powder produced through the production method has the advantages of being reasonable in powder size, uniform in crystal grain and component distribution, high in purity and low in oxygen content. The production method has the advantages of being simple in operation, low in energy consumption, high in production efficiency and suitable for continuous production.
Description
Technical field
The present invention relates to rare earth permanent-magnetic material preparation method, be specifically related to a kind of preparation method of samarium-cobalt alloy powder.
Background technology
Samarium cobalt permanent magnet alloy is a kind of high temperature permanent magnetic material of excellent performance, and because of its Curie temperature high (higher than 820 DEG C), temperature stability is good, corrosion resistance is strong and the advantage such as good in oxidation resistance has the effect do not replaced in permanent-magnet material.This material is widely used in microwave communication techniques, audio-visual technology, electrical engineering, instrumental technique, computing technique, automatic technology, communications and transportation, petrochemical industry, magnetization technology, magnetic separation technique, bioengineering and the field such as magnetic medical treatment and health and fitness facilities.
The method that tradition prepares samarium-cobalt alloy powder is the pure element metal adopting samarium, cobalt, iron, copper, zirconium and rare earth, in vacuum induction melting furnace, carries out high melt, then high temperature solution is carried out chilling and obtain alloy cast ingot.Conventional method relates in a lot of patent, and as 200910080120.6,201110457035.4, samarium-cobalt alloy powder prepared by this method has following shortcoming: needing to consume a large amount of electric energy, in order to prevent the oxidation of fusion process Raw, needing pumping high vacuum; For reducing the volatilization loss of alloying element in high melt process; applying argon gas is wanted to protect; and alloy cast ingot could take out after the cooling period; energy consumption is high, complicated operation, cycle are long, there is potential safety hazard to cause alloy cast ingot to prepare; because smelting temperature is high; ingot casting easily produces component segregation in condensation process, coarse grains, Grain size distribution are uneven, causes the decline of samarium-cobalt alloy performance, and the crystal grain of alloy powder and homogeneity of ingredients are the keys of preparation high-performance samarium-cobalt permanent-magnetic material.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art, provides a kind of preparation method of samarium-cobalt alloy powder.
In order to reach above-mentioned technical purpose, technical scheme provided by the invention is:
A preparation method for samarium-cobalt alloy powder, described samarium-cobalt alloy powder is made up of the element of following mass percentage content: samarium 24.5% ~ 26%, cobalt 52% ~ 56%, iron 7.5% ~ 12%, copper 6.5% ~ 8%, zirconium 2% ~ 4%, heavy rare earth element 0.5% ~ 1%; Described method comprises the steps:
(1) take the slaine of above-mentioned each element in the mass percentage content of samarium-cobalt alloy powder by above-mentioned each element; The slaine of above-mentioned each element is mixed with slaine mass percentage content be respectively the metal salt solution of 20% ~ 30% and mix, or is mixed with the metal salt solution that slaine mass percentage content is 20% ~ 30% after being mixed by the slaine of above-mentioned each element;
(2) add the surfactant accounting for slaine quality 1% ~ 5% in metal salt solution and account for slaine quality 1% ~ 5% dispersant; PH value is regulated to be 4 ~ 9;
(3) metal salt solution processed through step (2) is carried out spraying dry, prepare samarium-cobalt alloy powder presoma;
(4) samarium-cobalt alloy powder presoma is calcined in air under 200 DEG C ~ 300 DEG C conditions, decompose the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(5) the samarium-cobalt alloy powder after step (4) calcining is carried out twice reduction in 400 DEG C ~ 800 DEG C in a hydrogen atmosphere, often walking the recovery time is 30min ~ 120min;
(6) the samarium-cobalt alloy powder after step (5) reduction is milled to the samarium-cobalt alloy powder of 3 μm ~ 5 μm.
Wherein, described heavy rare earth element is one or more in gadolinium, dysprosium, holmium, praseodymium, er element.
The slaine of described samarium is samaric nitrate, samarium trichloride or acetic acid samarium; The slaine of described cobalt, iron, copper, zirconium is cobalt, iron, copper, the chlorate of zirconium, sulfate, nitrate or oxalates; The slaine of described heavy rare earth element is the nitrate of heavy rare earth element, chlorate or acetate.
Step (2) described surfactant is stearic acid, polyethylene glycol, urea, N, N-dimethyl formamide or dodecyl sodium sulfate; Described dispersant is triethyl group hexyl phosphoric acid, lauryl sodium sulfate, methyl anyl alcohol, cellulose derivative, polyacrylamide, guar gum or fatty acid polyethylene glycol ester.
Regulate metal salt solution pH value to be 4 ~ 9 by adding acid or alkali in step (2), described acid is HCl, HNO
3or oxalic acid, described alkali is NaOH, KOH or ammoniacal liquor.
Step (3) described spray drying condition is: temperature 300 DEG C ~ 350 DEG C, rate of drying 20000 ~ 30000 revs/min.
Described twice reduction of step (5) be by calcining after composite powder in a hydrogen atmosphere in 400 DEG C ~ 550 DEG C carry out first time reduce, recovery time 30min ~ 120min; Then the powder after first time reduction is carried out secondary reduction at 650 DEG C ~ 800 DEG C, recovery time 30min ~ 120min.
The present invention overcomes heritage answers method of smelting to prepare the shortcoming of samarium-cobalt alloy powder, adopts solution-spraying dry-calcining-hydrogen heat reduction-ball milling to prepare samarium-cobalt alloy powder.
Compared with prior art, beneficial effect of the present invention is:
(1) the ingot casting fragmentation preparation that the samarium-cobalt alloy powder that heritage answers method of smelting to prepare adopts copper condensation mould to cool fast, ingot casting easily produces component segregation in condensation process, coarse grains, Grain size distribution are uneven, easily cause the decline of samarium-cobalt alloy performance, and samarium-cobalt alloy powder prepared by the present invention adopts Liquid preparation methods, alloying element reaches the mixing of atom level level, component distributing is more even, and grain size is tiny and granularity concentrated.
(2) powder adopts solwution method preparation, first low temperature calcination in atmosphere, crystal salt is decomposed, and remove unnecessary adsorbed water and the crystallization water, then two step high temperature reductions under a hydrogen atmosphere, effectively eliminate the impurity oxygen in powder, the alloy powder purity of preparation is high, and after hydrogen reduction, in powder, remain part hydrogen, be conducive to preventing the oxidation in the follow-up use procedure of powder.
(3) heritage answers method of smelting to prepare samarium-cobalt alloy ingot casting needs to consume a large amount of electric energy, in order to prevent the oxidation of fusion process Raw, needs pumping high vacuum; For reducing the volatilization loss of alloying element in high melt process, applying argon gas to protect, and alloy cast ingot could take out after the cooling period, energy consumption is high, complicated operation, cycle are grown, there is potential safety hazard to cause alloy cast ingot to prepare.Samarium-cobalt alloy powder preparation method of the present invention adopts solwution method to prepare at normal temperatures, simple to operate, energy consumption is low, the cycle is short, production efficiency is high, safe and reliable, be applicable to continuous prodution.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, but is not limited in following examples.Percentage composition involved in embodiment 1 to 7 is mass percentage content.
Embodiment 1
To produce, composition is samarium 25.5%, the alloy powder of cobalt 52%, iron 10.5%, copper 8%, zirconium 4%.
Take the samaric nitrate Sm (NO of 57.05g
3)
3, 256.82g cobalt nitrate Co (NO
3)
26H
2o, 75.96g ferric nitrate Fe (NO
3)
39H
2o, 30.41g copper nitrate Cu (NO
3)
23H
2o, 18.82g zirconium nitrate Zr (NO
3)
45H
2o.
(1) metal salt solution that distilled water is mixed with metalline 30% respectively in described each slaine is added;
(2) each metal salt solution rapid mixing is stirred, add a small amount of HNO
3stir, controlling pH value is 4 ~ 6, obtains transparent mixed solution;
(3) add surfactant stearic acid and the 5g dispersant lauryl sodium sulfate of 10g, be fully uniformly mixed, to prevent from occurring precipitation in solution, make powder dispersibility good;
(4) then at 300 DEG C ~ 350 DEG C spraying dry, spraying dry speed is 20000 ~ 30000 revs/min, prepares samarium-cobalt alloy powder presoma;
(5) by presoma in air 200 DEG C ~ 300 DEG C calcinings, decompose the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(6) the samarium-cobalt alloy powder after calcining is once reduced in 400 DEG C ~ 550 DEG C in a hydrogen atmosphere, recovery time 30min ~ 120min;
(7) the samarium-cobalt alloy powder after first time reduction is carried out secondary reduction at 650 DEG C ~ 800 DEG C, recovery time 30min ~ 120min;
(8) last, the samarium-cobalt alloy powder after thermal reduction is carried out ball milling, obtains granularity at the samarium-cobalt alloy powder of 3 μm ~ 5 μm.
Embodiment 2
To produce, composition is samarium 24.5%, the alloy powder of cobalt 54.5%, iron 12%, copper 6.5%, zirconium 2.5%.
Take the samaric nitrate Sm (NO of 54.81g
3)
3, 269.17g cobalt nitrate Co (NO
3)
26H
2o, 86.81g ferric nitrate Fe (NO
3)
39H
2o, 24.71g copper nitrate Cu (NO
3)
23H
2o, 11.76g zirconium nitrate Zr (NO
3)
45H
2o.
(1) metal salt solution that distilled water is mixed with metalline 20% respectively in described each slaine is added;
(2) each metal salt solution rapid mixing is stirred, add a small amount of HNO
3stir, controlling pH value is 4 ~ 6, obtains transparent mixed solution;
(3) surfactant stearic acid and the 8g dispersant lauryl sodium sulfate of 15g is added, to prevent from occurring in solution that precipitation makes powder dispersibility good;
(4) then at 300 DEG C ~ 350 DEG C spraying dry, spraying dry speed is 20000 ~ 30000 revs/min, prepares samarium-cobalt alloy powder presoma;
(5) by presoma in air 200 DEG C ~ 300 DEG C calcinings, decompose the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(6) the samarium-cobalt alloy powder after calcining is once reduced in 400 DEG C ~ 550 DEG C in a hydrogen atmosphere, recovery time 30min ~ 120min;
(7) the samarium-cobalt alloy powder after first time reduction is carried out secondary reduction at 650 DEG C ~ 800 DEG C, recovery time 30min ~ 120min;
(8) last, the samarium-cobalt alloy powder after thermal reduction is carried out ball milling, obtains granularity at the samarium-cobalt alloy powder of 3 μm ~ 5 μm.
Embodiment 3
To produce, composition is samarium 25.5%, the alloy powder of cobalt 53%, iron 12%, copper 6.5%, zirconium 2.5%, praseodymium 0.5%.
Take the samaric nitrate Sm (NO of 57.05g
3)
3, 261.76g cobalt nitrate Co (NO
3)
26H
2o, 86.81g ferric nitrate Fe (NO
3)
39H
2o, 24.71g copper nitrate Cu (NO
3)
23H
2o, 11.76g zirconium nitrate Zr (NO
3)
45H
2o, 1.54g praseodymium nitrate Pr (NO
3)
36H
2o.
(1) metal salt solution that distilled water is mixed with metalline 25% respectively in described each slaine is added;
(2) each metal salt solution rapid mixing is stirred, add a small amount of HNO
3stir, controlling pH value is 4 ~ 6, obtains transparent mixed solution;
(3) add surfactant stearic acid and the 8g dispersant lauryl sodium sulfate of 15g, to prevent from occurring precipitation in solution, make powder dispersibility good;
(4) then at 300 DEG C ~ 350 DEG C spraying dry, spraying dry speed is 20000 ~ 30000 revs/min, prepares samarium-cobalt alloy powder presoma;
(5) by presoma in air 200 DEG C ~ 300 DEG C calcinings, decompose the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(6) the samarium-cobalt alloy powder after calcining is once reduced in 400 DEG C ~ 550 DEG C in a hydrogen atmosphere, recovery time 30min ~ 120min;
(7) the samarium-cobalt alloy powder after first time reduction is carried out secondary reduction at 650 DEG C ~ 800 DEG C, recovery time 30min ~ 120min;
(8) last, the samarium-cobalt alloy powder after thermal reduction is carried out ball milling, obtains granularity at the samarium-cobalt alloy powder of 3 μm ~ 5 μm.
Embodiment 4
To produce, composition is samarium 25.5%, the alloy powder of cobalt 53%, iron 12%, copper 6.5%, zirconium 2.5%, gadolinium 0.5%.
Take the samaric nitrate Sm (NO of 57.05g
3)
3, 261.76g cobalt nitrate Co (NO
3)
26H
2o, 86.81g ferric nitrate Fe (NO
3)
39H
2o, 24.71g copper nitrate Cu (NO
3)
23H
2o, 11.76g zirconium nitrate Zr (NO
3)
45H
2o, 1.44g gadolinium nitrate Gd (NO
3)
36H
2o.
(1) metal salt solution that distilled water is mixed with metalline 25% respectively in described each slaine is added;
(2) each metal salt solution rapid mixing is stirred, add a small amount of HNO
3stir, controlling pH value is 4 ~ 6, obtains transparent mixed solution;
(3) add surfactant stearic acid and the 8g dispersant lauryl sodium sulfate of 15g, to prevent from occurring precipitation in solution, make powder dispersibility good;
(4) then at 300 DEG C ~ 350 DEG C spraying dry, spraying dry speed is 20000 ~ 30000 revs/min, prepares samarium-cobalt alloy powder presoma;
(5) by presoma in air 200 DEG C ~ 300 DEG C calcinings, decompose the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(6) the samarium-cobalt alloy powder after calcining is once reduced in 400 DEG C ~ 550 DEG C in a hydrogen atmosphere, recovery time 30min ~ 120min;
(7) the samarium-cobalt alloy powder after first time reduction is carried out secondary reduction at 650 DEG C ~ 800 DEG C, recovery time 30min ~ 120min;
(8) last, the samarium-cobalt alloy powder after thermal reduction is carried out ball milling, obtains granularity at the samarium-cobalt alloy powder of 3 μm ~ 5 μm.
Embodiment 5
To produce, composition is samarium 25.5%, the alloy powder of cobalt 53%, iron 12%, copper 6.2%, zirconium 2.5%, dysprosium 0.8%.
Take the samaric nitrate Sm (NO of 57.05g
3)
3, 261.76g cobalt nitrate Co (NO
3)
26H
2o, 86.81g ferric nitrate Fe (NO
3)
39H
2o, 23.57g copper nitrate Cu (NO
3)
23H
2o, 11.76g zirconium nitrate Zr (NO
3)
45H
2o, 2.16g dysprosium nitrate D
y(NO
3)
35H
2o.
(1) metal salt solution that distilled water is mixed with metalline 25% respectively in described each slaine is added;
(2) each metal salt solution rapid mixing is stirred, add a small amount of HNO
3stir, controlling pH value is 4 ~ 6, obtains transparent mixed solution;
(3) add surfactant stearic acid and the 8g dispersant lauryl sodium sulfate of 15g, to prevent from occurring precipitation in solution, make powder dispersibility good;
(4) then at 300 DEG C ~ 350 DEG C spraying dry, spraying dry speed is 20000 ~ 30000 revs/min, prepares samarium-cobalt alloy powder presoma;
(5) by presoma in air 200 DEG C ~ 300 DEG C calcinings, decompose the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(6) the samarium-cobalt alloy powder after calcining is once reduced in 400 DEG C ~ 550 DEG C in a hydrogen atmosphere, recovery time 30min ~ 120min;
(7) the samarium-cobalt alloy powder after first time reduction is carried out secondary reduction at 650 DEG C ~ 800 DEG C, recovery time 30min ~ 120min;
(8) last, the samarium-cobalt alloy powder after thermal reduction is carried out ball milling, obtains granularity at the samarium-cobalt alloy powder of 3 μm ~ 5 μm.
Embodiment 6
To produce, composition is samarium 25.5%, the alloy powder of cobalt 53%, iron 12%, copper 6.2%, zirconium 2.5%, holmium 0.8%.
Take the samaric nitrate Sm (NO of 57.05g
3)
3, 261.76g cobalt nitrate Co (NO
3)
26H
2o, 86.81g ferric nitrate Fe (NO
3)
39H
2o, 23.57g copper nitrate Cu (NO
3)
23H
2o, 11.76g zirconium nitrate Zr (NO
3)
45H
2o, 1.54g holmium nitrate HoNO
35H
2o.
(1) each slaine mixing will taken, adds distilled water in the slaine of described mixing, is mixed with the metal salt solution of metalline 25%;
(2) in metal salt solution, a small amount of HNO is added
3stir, controlling pH value is 4 ~ 6, obtains transparent mixed solution;
(3) add surfactant stearic acid and the 8g dispersant lauryl sodium sulfate of 15g, to prevent from occurring precipitation in solution, make powder dispersibility good;
(4) then at 300 DEG C ~ 350 DEG C spraying dry, spraying dry speed is 20000 ~ 30000 revs/min, prepares samarium-cobalt alloy powder presoma;
(5) by presoma in air 200 DEG C ~ 300 DEG C calcinings, decompose the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(6) the samarium-cobalt alloy powder after calcining is once reduced in 400 DEG C ~ 550 DEG C in a hydrogen atmosphere, recovery time 30min ~ 120min;
(7) the samarium-cobalt alloy powder after first time reduction is carried out secondary reduction at 650 DEG C ~ 800 DEG C, recovery time 30min ~ 120min;
(8) last, the samarium-cobalt alloy powder after thermal reduction is carried out ball milling, obtains granularity at the samarium-cobalt alloy powder of 3 μm ~ 5 μm.
Embodiment 7
To produce, composition is samarium 25.5%, the alloy powder of cobalt 53%, iron 12%, copper 6%, zirconium 2.5%, erbium 1%.
Take the samaric nitrate Sm (NO of 57.05g
3)
3, 261.76g cobalt nitrate Co (NO
3)
26H
2o, 86.81g ferric nitrate Fe (NO
3)
39H
2o, 22.81g copper nitrate Cu (NO
3)
23H
2o, 11.76g zirconium nitrate Zr (NO
3)
45H
2o, 1.91g erbium nitrate ErNO
35H
2o.
(1) each slaine mixing will taken, adds distilled water in the slaine of described mixing, is mixed with the metal salt solution of metalline 25%;
(2) in metal salt solution, a small amount of HNO is added
3stir, controlling pH value is 4 ~ 6, obtains transparent mixed solution;
(3) surfactant stearic acid and the 8g dispersant lauryl sodium sulfate of 15g is added, to prevent from occurring in solution that precipitation makes powder dispersibility good;
(4) then at 300 DEG C ~ 350 DEG C spraying dry, spraying dry speed is 20000 ~ 30000 revs/min, prepares samarium-cobalt alloy powder presoma;
(5) by presoma in air 200 DEG C ~ 300 DEG C calcinings, decompose the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(6) the samarium-cobalt alloy powder after calcining is once reduced in 400 DEG C ~ 550 DEG C in a hydrogen atmosphere, recovery time 30min ~ 120min;
(7) the samarium-cobalt alloy powder after first time reduction is carried out secondary reduction at 650 DEG C ~ 800 DEG C, recovery time 30min ~ 120min;
(8) last, the samarium-cobalt alloy powder after thermal reduction is carried out ball milling, obtains granularity at the samarium-cobalt alloy powder of 3 μm ~ 5 μm.
The powder of preparation in embodiment 1 to 7 is carried out grain size analysis, BET specific surface, morphology analysis and chemical composition analysis:
Results of grain size analysis shows, powder agglomerates particle mean size 4.3 μm;
BET surface analysis granularity shows, BET powder size 3.6 μm;
ESEM morphology analysis result shows that powder in the form of sheets, and individual particle granularity is less than 5 μm;
Chemical composition analysis shows that powder oxygen content is 0.1%, each element powders distributed components.
Claims (7)
1. the preparation method of a samarium-cobalt alloy powder, it is characterized in that, described samarium-cobalt alloy powder is made up of the element of following mass percentage content: samarium 24.5% ~ 26%, cobalt 52% ~ 56%, iron 7.5% ~ 12%, copper 6.5% ~ 8%, zirconium 2% ~ 4%, heavy rare earth element 0.5% ~ 1%; Described method comprises the steps:
(1) take the slaine of above-mentioned each element in the mass percentage content of samarium-cobalt alloy powder by above-mentioned each element; The slaine of above-mentioned each element is mixed with slaine mass percentage content be respectively the metal salt solution of 20% ~ 30% and mix, or is mixed with the metal salt solution that slaine mass percentage content is 20% ~ 30% after being mixed by the slaine of above-mentioned each element;
(2) add the surfactant accounting for slaine quality 1% ~ 5% in metal salt solution and account for slaine quality 1% ~ 5% dispersant; PH value is regulated to be 4 ~ 9;
(3) metal salt solution processed through step (2) is carried out spraying dry, prepare samarium-cobalt alloy powder presoma;
(4) samarium-cobalt alloy powder presoma is calcined in air under 200 DEG C ~ 300 DEG C conditions, decompose the crystal salt in samarium-cobalt alloy powder presoma, remove unnecessary adsorbed water and the crystallization water, obtain samarium-cobalt alloy powder;
(5) the samarium-cobalt alloy powder after step (4) calcining is carried out twice reduction in 400 DEG C ~ 800 DEG C in a hydrogen atmosphere, each recovery time is 30min ~ 120min;
(6) the samarium-cobalt alloy powder after step (5) reduction is milled to the samarium-cobalt alloy powder of 3 μm ~ 5 μm.
2. the method for claim 1, is characterized in that, described heavy rare earth element is one or more in gadolinium, dysprosium, holmium, praseodymium, er element.
3. the method for claim 1, is characterized in that, the slaine of described samarium is samaric nitrate, samarium trichloride or acetic acid samarium; The slaine of described cobalt, iron, copper, zirconium is cobalt, iron, copper, the chlorate of zirconium, sulfate, nitrate or oxalates; The slaine of described heavy rare earth element is the nitrate of heavy rare earth element, chlorate or acetate.
4. the method for claim 1, is characterized in that, step (2) described surfactant is stearic acid, polyethylene glycol, urea, N, N-dimethyl formamide or dodecyl sodium sulfate; Described dispersant is triethyl group hexyl phosphoric acid, lauryl sodium sulfate, methyl anyl alcohol, cellulose derivative, polyacrylamide, guar gum or fatty acid polyethylene glycol ester.
5. the method for claim 1, is characterized in that, regulate metal salt solution pH value to be 4 ~ 9 by adding acid or alkali in step (2), described acid is HCl, HNO
3or oxalic acid, described alkali is NaOH, KOH or ammoniacal liquor.
6. the method for claim 1, is characterized in that, step (3) described spray drying condition is: temperature 300 DEG C ~ 350 DEG C, dry rotating speed 20000 ~ 30000 revs/min.
7. the method for claim 1, is characterized in that, described twice reduction of step (5) be by calcining after composite powder in a hydrogen atmosphere in 400 DEG C ~ 550 DEG C carry out first time reduce, recovery time 30min ~ 120min; Then the powder after first time reduction is carried out secondary reduction at 650 DEG C ~ 800 DEG C, recovery time 30min ~ 120min.
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| CN104319046B (en) * | 2014-10-11 | 2017-07-07 | 宁波科星材料科技有限公司 | A kind of samarium-cobalt permanent-magnetic material |
| CN108274016B (en) * | 2018-03-14 | 2021-05-07 | 浙江工业大学 | Method for directly preparing samarium-iron alloy powder by spray pyrolysis reduction method |
| CN108889943A (en) * | 2018-09-05 | 2018-11-27 | 河北工业大学 | A kind of preparation of copper iron compound powder body material and its forming method |
| CN112570724B (en) * | 2020-12-11 | 2022-11-25 | 江西理工大学 | Preparation method of rare earth tungsten copper composite powder |
| CN114799192B (en) * | 2022-04-20 | 2023-02-03 | 北京航空航天大学 | ZrCo alloy with porous structure and preparation method thereof |
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| JP2010027852A (en) * | 2008-07-18 | 2010-02-04 | Daido Steel Co Ltd | Method of manufacturing r-t-b based rare earth magnet |
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| JP2011210850A (en) * | 2010-03-29 | 2011-10-20 | Tdk Corp | Method of manufacturing rare-earth sintered magnet, and the rare-earth sintered magnet |
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Effective date of registration: 20160325 Address after: 410200 No. 1106, Jinxing North Road, Wangcheng Economic Development Zone, Hunan, Changsha (Hunan Aerospace Science and Technology Industrial Park) Patentee after: Hunan Aerospace Magnet & Magneto Co., Ltd. Address before: Three road 410205 in Hunan Province, Yuelu District City, No. 217 Changsha Fenglin Patentee before: Hunan Aerospace Industry General Corporation |