CN107785141A - A kind of method that non-rare earth MnBi permanent-magnet alloy high-temperature stabilities are improved by discharge plasma sintering technique - Google Patents
A kind of method that non-rare earth MnBi permanent-magnet alloy high-temperature stabilities are improved by discharge plasma sintering technique Download PDFInfo
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- CN107785141A CN107785141A CN201710998957.3A CN201710998957A CN107785141A CN 107785141 A CN107785141 A CN 107785141A CN 201710998957 A CN201710998957 A CN 201710998957A CN 107785141 A CN107785141 A CN 107785141A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/059—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C22/00—Alloys based on manganese
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/06—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder
- H01F1/08—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
- H01F1/086—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together sintered
Abstract
The invention discloses a kind of method that non-rare earth MnBi permanent-magnet alloy high-temperature stabilities are improved by discharge plasma sintering technique, its step is：Match foundry alloy sample composition：According to MnBi phasors, proportioning atomic ratio is Mn60Bi40Alloy, wherein Mn elements are that sheet is electrolysed Mn, need argon arc melt back to there is the metallic luster just can sample；Melt-spun：Annealing heat-treats：Initial strip prepared by fast melt-quenching carries out annealing heat-treats；Surface adjuvant ball milling：Strip after annealing is prepared into uniformly tiny powder particle by ball milling；Discharge plasma sintering：Powder after ball milling is fitted into graphite jig, is sintered using plasma discharging system under 593 K/50 MPa/5 min sintering condition, you can the MnBi permanent magnets with excellent high temperature stability are made.The MnBi magnets being prepared by the method for the present invention, its under 650 K test temperatures coercivity still up to 12.04 kOe.
Description
Technical field
The present invention relates to the preparation of MnBi permanent-magnet alloys and its magnetic property to study, more particularly to one kind passes through plasma discharging
The method that sintering technology improves non-rare earth MnBi permanent-magnet alloy high-temperature stabilities.
Background technology
Permanent-magnet material has a wide range of applications in fields such as electromechanics, information, communication and medical treatment, especially using Nd-Fe-B as
The rare earth permanent-magnetic material of representative.But the Curie temperature of the rare earth permanent-magnetic material such as NdFeB is low, heat endurance is poor, by adding weight
Although dysprosium doping and terbium can improve NdFeB high-temperature stability to a certain extent, but heavy rare earth element belongs to rare
Strategic resource, being excessively used for heavy rare earth element substantially increase the cost of raw material, limit its application in high-temperature field.
MnBi has higher magnetocrystalline anisotropy, moderate saturation magnetization and positive rectified as a kind of non-rare earth permanent-magnetic material
Stupid power temperature coefficient, it has important potential using value in high temperature field.
Discharge plasma sintering has heating speed using electric discharge thermal sintering caused by Joule heat and electric discharge compared to conventional sintering
The features such as rate is fast, sintering time is short, the densification degree of magnet can be effectively improved.After surfactant is aided in ball milling by the present invention
MnBi powder MnBi block shaped magnets are prepared using discharge plasma sintering, the method phases of MnBi magnets is prepared with other method
Than such as anneal band or hot pressed samples, magnet prepared by discharge plasma sintering is in 650 K（Pertinent literature report low temperature MnBi
It is in mutually paramagnetism in 628 K）Excellent hard magnetic property is still maintained, is allowed to that there is potential application value in high-temperature field.
The content of the invention
Non- rare earth MnBi permanent magnetism is improved object of the present invention is to provide one kind by discharge plasma sintering technique to close
The method of golden high-temperature stability, it has the advantages that excellent high-temperature magnetic can be fine and close with height.
The present invention is achieved like this, and one kind improves non-rare earth MnBi permanent-magnet alloys by discharge plasma sintering technique
The method of high-temperature stability, method and step are：
（One）Match foundry alloy sample composition：According to MnBi phasors proportioning needed for alloy sample, use purity for 99.8% electrolysis
Mn, the Bi that purity is 99.99%, wherein electrolysis Mn needs melt back to there is the metallic luster can sample；
（Two）Melt-spun：The simple substance element that weighing has matched is put into water-cooled copper crucible, vacuum is evacuated to 1.0 × 10-3 Pa
It is filled with the high-purity argon gas of 1 standard atmospheric pressure behind left and right, need to first melts Zr blocks during melting, it is absorbed oxygen remaining in stove,
Melt back four to five times in arc-melting furnace by matched somebody with somebody sample, to improve its homogeneity of ingredients；Afterwards by ingot casting by machinery
Put into quartz ampoule after broken, under high-purity argon gas protective atmosphere induction melting and using air pressure official post its from the stone in 0.6 mm apertures
Sprayed in the English pipe mouth of pipe, the drop sprayed rapidly is dropped on the atwirl copper rollers of 30-50 m/s, and thin ribbon shaped is finally prepared
Sample；
（Three）Annealing heat-treats：The quartzy seal of tube of thin ribbon shaped sample that band obtains will be got rid of, is high vacuum state in it, uses electricity
Resistance stove is annealed the strip of the quartzy seal of tube under conditions of temperature is 540-673 K, the time is 30-60 min, you can
Obtain high-purity low temperature MnBi phase alloy strips；
（Four）Surface adjuvant ball milling：Using agate alms bowl and pestle in glove box by the strip coarse crushing after annealing to 100-300
μm or so, then using oleic acid, oleyl amine as surface adjuvant, normal heptane is solvent, by planetary ball mill, has carried out 200
Rpm, ratio of grinding media to material 15:1 ball milling experiment, Ball-milling Time is 0.5-8 h；
（Five）Discharge plasma sintering（SPS）：Powder after 10 g or so ball milling is fitted into graphite jig, using electric discharge etc. from
Sub- sintering system, under the conditions of 593 K/50 MPa/5 min high-vacuum sintering, you can cylindrical MnBi permanent magnets are made.
The quick cooling of the fast melt-quenching can suppress MnBi bianry alloys in 719 K because of peritectic reaction and caused by Mn
Phase segregation phenomenon, laid the foundation to obtain carbonyl iron magnetic low temperature MnBi phases after band annealing.
The surfactant auxiliary ball-milling technology can reduce intergranular agglomeration, and it is thin to obtain particle size uniformity
Small forerunner's sintered powder, so as to significantly lift the coercivity of magnet.
The discharge plasma sintering has compared to conventional sintering and risen using electric discharge thermal sintering caused by Joule heat and electric discharge
The features such as warm speed is fast, sintering time is short, the densification degree of magnet, and the MnBi magnetic prepared with other method can be effectively improved
Body phase ratio, magnet prepared by discharge plasma sintering is in 650 K（Pertinent literature report low temperature MnBi phases are in paramagnetism in 628 K）
Excellent hard magnetic property is still maintained, is allowed to more have potential application value in high-temperature field.
Step（One）The simple substance element orders gained by promise green wood in Beijing, and Bi elemental purities are 99.99%, Mn elements
Mn is electrolysed for 99.8% sheet, wherein electrolysis Mn needs melt back to there is metallic luster, can sample.
Step（Two）The melt-spun all needs vacuum being evacuated to 1.0 × 10-3 Pa or so, in the atmosphere of high-purity argon gas
Lower completion.During electric arc melting, electric current should not be too big and to adjust tungsten needle and the distance of sample, is splashed to prevent sample or the starting the arc is lost
Lose；When fast quenching gets rid of band, induced-current need to be slowly increased, when the sample is heated evenly to molten condition, by melt jet to rotating
Alloy thin band needed for the acquisition of copper roller.
Step（Three）The annealing heat-treats need that picking has metallic luster and the less alloy thin band of burr is put into one end
The internal diameter of closing is in 10mm quartz ampoule, after this quartz ampoule is evacuated into high vacuum state, with acetylene flame rapidly by elongated stone
English pipe blows；Then the quartz ampoule for being packaged with sample is put into resistance furnace and carries out annealing heat-treats.
Step（Four）The surface adjuvant ball milling precursor powder is obtained after being ground by agate alms bowl and pestle, will be broken
Powder after broken is placed in planetary ball mill ball grinder；When oleic acid and oleyl amine is added dropwise, it is necessary to be carried out in vent cabinet, hand is worn
Rubber gloves, wear mouth mask or breathing mask.
Step（Five）The discharge plasma sintering need to be completed under high vacuum state, and sintering temperature is by insertion graphite jig
In thermocouple monitoring, sintering pressure by mould therefor sectional area calculate obtain.
The solution have the advantages that：Non- rare earth MnBi permanent-magnet alloys prepared by the present invention, prepared compared to ordinary sinter
MnBi alloys, there is high compactness and excellent high-temperature stability, and excellent hard magnetic property is still presented in 650 K, this
The discharge plasma sintering MnBi magnets that invention obtains have very considerable application value in high-temperature field.
Brief description of the drawings
Fig. 1 discharge plasma sinterings Mn60Bi40The SEM figures of magnet, sintering condition is 593 K/50 MPa/5 min.
（（a）Back scattering SEM shape appearance figures,（b）Secondary electron SEM shape appearance figures）.
Mn prepared by the m/s of Fig. 2 3560Bi40Magnetic property of the annealing band at a temperature of 300-650 K.
Fig. 3 discharge plasma sinterings Mn60Bi40Magnetic property of the magnet at a temperature of 300-650 K.
Embodiment
（One）Match foundry alloy sample composition：According to alloy sample needed for MnBi phasors proportioning, purity is used as 99.8%
Mn is electrolysed, the Bi that purity is 99.99%, wherein electrolysis Mn needs melt back to there is the metallic luster can sample.
（Two）Melt-spun：The simple substance element that weighing has matched is put into water-cooled copper crucible, vacuum is evacuated to 1.0 × 10-3
It is filled with the high-purity argon gas of 1 standard atmospheric pressure after Pa or so, need to first melts Zr blocks during melting, it is absorbed oxygen remaining in stove
Gas, melt back four to five times in arc-melting furnace by matched somebody with somebody sample, to improve its homogeneity of ingredients；Ingot casting is passed through into machine afterwards
Put into quartz ampoule after tool is broken, under high-purity argon gas protective atmosphere induction melting and using air pressure official post its from 0.6 mm apertures
Sprayed in the quartz ampoule mouth of pipe, the drop sprayed rapidly is dropped on the atwirl copper rollers of 35 m/s, and thin ribbon shaped is finally prepared
Sample.
（Three）Annealing heat-treats：The quartzy seal of tube of thin ribbon shaped sample that band obtains will be got rid of, is high vacuum state in it, makes
The strip of the quartzy seal of tube is annealed under the conditions of 593 K/30 min with resistance furnace, high-purity low temperature MnBi phases can be obtained
Alloy thin band.
（Four）Surface adjuvant ball milling：Using agate alms bowl and pestle in glove box by the strip coarse crushing after annealing to 100-
300 μm or so, then using oleic acid, oleyl amine as surface adjuvant, normal heptane is solvent, using planetary ball mill, is carried out
200 rpm, ratio of grinding media to material 15:1 ball milling experiment, Ball-milling Time is 30 min.
（Five）Discharge plasma sintering（SPS）：Powder after 10 g or so ball milling is fitted into graphite jig, utilizes electric discharge
Plasma agglomeration system, under the conditions of 593 K/50 MPa/5 min high-vacuum sintering, you can cylindrical MnBi permanent magnetism is made
Body.
Accompanying drawing 1（a）With（b）Respectively above-mentioned discharge plasma sintering Mn60Bi40The back scattering of magnet and secondary electron SEM
Shape appearance figure.
Get rid of tape speed be 35 m/s, annealing conditions be magnetic of the 593 made bands of K/30 min at a temperature of 300-650 K
Performance data is shown in Table 1.Get rid of tape speed be 35 m/s, annealing conditions are 593 K/30 min, Ball-milling Time be 30 min, burn
Magnetic property data of the knot condition for the 593 made MnBi magnets of K/50 MPa/5 min at a temperature of 300-650 K refer to the institute of table 1
Show.
Table 1
With reference to table 1, accompanying drawing 2 and 3 as can be seen that getting rid of that tape speed is 35 m/s, annealing temperature is 593 K and annealing time is 30
The coercivity that annealing band prepared by min obtains in 500 K is 16.30 kOe, and its demagnetization under 650 K test temperatures is bent
Paramagnetism feature is presented in line.Get rid of tape speed be 35 m/s, annealing conditions are 593 K/30 min, Ball-milling Time be 30 min, burn
Knot condition is that coercivity of the 593 made MnBi magnets of K/50 MPa/5 min under 550 K test conditions is 25.37 kOe, and
In the case where 650 K test high temperature, coercivity is 14.2 emu/g still up to 12.04 kOe, remanent magnetism, and excellent permanent magnetism performance is presented.
Discharge plasma sintering technique can effectively improve its high-temperature stability in the application of MnBi alloy fields, therefore the present invention uses
Discharge plasma sintering technique can effectively improve the high-temperature stability of MnBi magnets.
Although introducing and describing the embodiment of the present invention, the invention is not limited in this, but can also
To be implemented except the other modes in the range of the technical scheme defined in appended claims, for example tune can also be passed through
Save the composition of alloy, get rid of the regulation and control of tape speed, annealing temperature and Ball-milling Time to discharge plasma sintering presoma performance, with uncommon
The magnetic property for the MnBi magnets that can change discharge plasma sintering preparation is hoped, while discharge plasma sintering work can also be adjusted
Skill, the further influence for exploring discharge plasma sintering process to MnBi magnet magnetic properties etc..
Claims (4)
1. a kind of method that non-rare earth MnBi permanent-magnet alloy high-temperature stabilities are improved by discharge plasma sintering technique, its feature
It is, the described method comprises the following steps：
（One）Match foundry alloy sample composition：According to MnBi phasors proportioning needed for alloy sample, use purity for 99.8% electrolysis
Mn, the Bi that purity is 99.99%, wherein electrolysis Mn needs melt back to there is the metallic luster can sample；
（Two）Melt-spun：The simple substance element that weighing has matched is put into water-cooled copper crucible, vacuum is evacuated to 1.0 × 10-3 Pa is left
It is filled with the high-purity argon gas of 1 standard atmospheric pressure behind the right side, need to first melts Zr blocks during melting, it is absorbed oxygen remaining in stove, will
Matched somebody with somebody sample melt back four to five times in arc-melting furnace, to improve its homogeneity of ingredients；It is afterwards that ingot casting is broken by machinery
Quartz ampoule is put into after broken, under high-purity argon gas protective atmosphere induction melting and using air pressure official post its from the quartz in 0.6 mm apertures
Sprayed in the pipe mouth of pipe, the drop sprayed rapidly is dropped on the atwirl copper rollers of 30-50 m/s, and thin ribbon shaped sample is finally prepared
Product；
（Three）Annealing heat-treats：The quartzy seal of tube of thin ribbon shaped sample that band is prepared will be got rid of, is high vacuum state in it, makes
The strip of the quartzy seal of tube is annealed under conditions of temperature is 540-673 K, the time is 30-60 min with resistance furnace,
High-purity low temperature MnBi phase strips can be obtained；
（Four）Surface adjuvant ball milling：Using agate alms bowl and pestle in glove box by the strip coarse crushing after annealing to 100-300
μm or so, then using oleic acid, oleyl amine as surface adjuvant, normal heptane is solvent, is 15 in ratio of grinding media to material:1st, rotating speed is 200 rpm
Under conditions of being 0.5-8 h with Ball-milling Time, discharge plasma sintering Precursor Powder is prepared by planetary ball mill；
（Five）Discharge plasma sintering：Powder after 10 g or so ball milling is fitted into graphite jig, burnt using plasma discharging
Clone is united, under the conditions of 593 K/50 MPa/5 min high-vacuum sintering, you can cylindrical MnBi permanent magnets are made.
It is steady that 2. one kind as claimed in claim 1 by discharge plasma sintering technique improves non-rare earth MnBi permanent-magnet alloy high temperature
Qualitatively method, it is characterised in that the quick cooling of the fast melt-quenching can suppress MnBi bianry alloys in 719 K because of peritectoid
React and caused Mn phase segregations phenomenon, laid the foundation to obtain carbonyl iron magnetic low temperature MnBi phases after band annealing.
It is steady that 3. one kind as claimed in claim 1 by discharge plasma sintering technique improves non-rare earth MnBi permanent-magnet alloy high temperature
Qualitatively method, it is characterised in that the surfactant auxiliary ball-milling technology can reduce intergranular agglomeration, obtain
The tiny forerunner's sintered powder of particle size uniformity, so as to significantly lift the coercivity of magnet.
It is steady that 4. one kind as claimed in claim 1 by discharge plasma sintering technique improves non-rare earth MnBi permanent-magnet alloy high temperature
Qualitatively method, it is characterised in that the discharge plasma sintering is compared using electric discharge thermal sintering caused by Joule heat and electric discharge
Conventional sintering has the characteristics that heating rate is fast, sintering time is short, can effectively improve the densification degree of magnet, and with its other party
MnBi magnets prepared by method are compared, and magnet prepared by discharge plasma sintering still maintains excellent hard magnetic property in 650 K, makes
More have potential application value in high-temperature field.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108723355A (en) * | 2018-05-31 | 2018-11-02 | 江苏大学 | Discharge plasma sintering prepares magnetism Sm2Co17The methods and applications of/Al-Ni-Co composite materials |
| CN109972027A (en) * | 2018-12-24 | 2019-07-05 | 南昌航空大学 | A method of mutually adding preparation anisotropy CeFeB permanent-magnet alloy by low melting point PrCu intergranular |
| CN110571038A (en) * | 2019-08-29 | 2019-12-13 | 杭州史宾纳科技有限公司 | Method for improving neodymium iron boron magnetism by driving Nd-Cu grain boundary diffusion through pressure heat treatment |
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| CN102240810A (en) * | 2011-06-24 | 2011-11-16 | 北京工业大学 | Method for preparing high-coercivity manganese bismuth magnetic powder |
| CN105321643A (en) * | 2014-07-29 | 2016-02-10 | Lg电子株式会社 | MNBI-based magnetic substance, preparation method thereof, mnbi-based sintered magnet and preparation method thereof |
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2017
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| CN102240810A (en) * | 2011-06-24 | 2011-11-16 | 北京工业大学 | Method for preparing high-coercivity manganese bismuth magnetic powder |
| CN105321643A (en) * | 2014-07-29 | 2016-02-10 | Lg电子株式会社 | MNBI-based magnetic substance, preparation method thereof, mnbi-based sintered magnet and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108723355A (en) * | 2018-05-31 | 2018-11-02 | 江苏大学 | Discharge plasma sintering prepares magnetism Sm2Co17The methods and applications of/Al-Ni-Co composite materials |
| CN109972027A (en) * | 2018-12-24 | 2019-07-05 | 南昌航空大学 | A method of mutually adding preparation anisotropy CeFeB permanent-magnet alloy by low melting point PrCu intergranular |
| CN110571038A (en) * | 2019-08-29 | 2019-12-13 | 杭州史宾纳科技有限公司 | Method for improving neodymium iron boron magnetism by driving Nd-Cu grain boundary diffusion through pressure heat treatment |
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Application publication date: 20180309 |