CN108346499A - A kind of method that organic light rare earth complex modification prepares high-coercivity manganese bismuth magnetic powder - Google Patents
A kind of method that organic light rare earth complex modification prepares high-coercivity manganese bismuth magnetic powder Download PDFInfo
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- CN108346499A CN108346499A CN201810120000.3A CN201810120000A CN108346499A CN 108346499 A CN108346499 A CN 108346499A CN 201810120000 A CN201810120000 A CN 201810120000A CN 108346499 A CN108346499 A CN 108346499A
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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
- H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
- H01F1/0045—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
- H01F1/0054—Coated nanoparticles, e.g. nanoparticles coated with organic surfactant
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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
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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
- H01F1/061—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 with a protective layer
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
Abstract
The invention discloses a kind of methods that organic light rare earth complex modified by nano particles prepares high-coercivity manganese bismuth magnetic powder, follow these steps to carry out：According to MnBi alloying component dispensings, obtains alloy cast ingot and fast quenching is at strip；MnBi fast quenching thin straps are subjected to vacuum heat and carry out the pre- ball milling of high energy to it, then organic light rare earth complex nano particle is added, and so that light rare earth complex nano particle is effectively coated MnBi magnetic powders by high-energy ball milling, finally obtain the high-coercivity manganese bismuth magnetic powder of organic light rare earth complex modified by nano particles.The present invention makes light rare earth ion be substituted into the molecular grating of MnBi alloys by high-energy ball milling, effectively promotes the magnetocrystalline anisotropy of MnBi phases, and the coercivity of the MnBi alloy magnetic powders of acquisition is made to improve 40 ~ 90%.Meanwhile present invention process process is simple, and it is easy to operate, cost is reduced, is conducive to application of the high-coercivity manganese bismuth magnetic powder in more permanent magnet devices, to meet the market demand.
Description
Technical field
The present invention relates to technical field of magnetic materials more particularly to a kind of organic light rare earth complex modified by nano particles systems
The method of standby high-coercivity manganese bismuth magnetic powder.
Background technology
In recent years, the great demand of rare earth permanent-magnetic material leads to consuming excessively for rare earth resources, novel low rare earth or without dilute
Native permanent-magnet material becomes research hotspot.Manganese bismuth alloy has higher intrinsic magnetic as a kind of novel no rare earth permanent-magnetic material
Characteristic, and there is positive coercive force temperature coefficient in a certain range, become the potential permanent-magnet material of high temperature application.But Mn-
Due to its unique phase composition and changing rule in alloy system between Bi binary metals, it is difficult to obtain pure single-phase MnBi, mainly
It is that Mn atoms are easy to from MnBi Liquid Phase Segregations when peritectic reaction occurs in 719 K due to manganese bismuth alloy, this limits manganese significantly
The acquisition of bismuth magnetic powder high magnetic characteristics.Therefore, the pure single-phase manganese bismuth alloy of high-performance how is obtained, while promoting the coercive of manganese bismuth alloy
Power reduces the room temperature coercive gap edge with the magnets such as neodymium iron boron and SmCo, become magnetic industry be badly in need of public relations key subject it
One.
In view of the above-mentioned problems, the present invention is proposed using " electric arc melting+fast quenching+heat treatment+high-energy ball milling " and is adulterated organic
Light rare earth complex nano particle inhibits the formation of MnBi high-temperature-phases and the segregation of Mn atoms, realizes organic light rare earth complex
The preparation of modified by nano particles high-coercivity manganese bismuth magnetic powder.
Invention content
For problems of the prior art, present invention aims at provide a kind of organic light rare earth complex nanometer
The modified method for preparing high-coercivity manganese bismuth magnetic powder of grain.
The present invention is realized by the following technical programs：
The method that a kind of organic light rare earth complex modified by nano particles prepares high-coercivity manganese bismuth magnetic powder, feature exist
In following these steps to carry out：
（1）Dispensing：According to nominal composition MnyBi100-y, molar fraction y=45 or 50 or 55 or 60, use purity be 99.99% with
On Mn, Bi alloy carry out weighing and burden；
（2）Melting：The raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting obtains
MnyBi100-yAlloy cast ingot；
（3）Fast quenching：By MnyBi100-yIn the quick quenching furnace of alloy cast ingot under protection of argon gas, fast quenching obtains MnyBi100-yAlloy is thin
Band；
（4）Vacuum heat：By step（3）Mn obtainedyBi100-yAlloy thin band carries out vacuum annealing heat treatment, obtains corresponding
Nanometer crystal alloy strip；
（5）High-energy ball milling：By step（4）Mn obtainedyBi100-yNanometer crystal alloy strip carries out high-energy ball milling, is added before ball milling
Weight is MnyBi100-yThe surfactant of nanometer crystal alloy strip weight 3 ~ 9%, ball milling 0.5 ~ 1 hour；Adding weight is
MnyBi100-yOrganic light rare earth complex nano particle of nanometer crystal alloy strip weight 10 ~ 50%, continues ball milling 1 ~ 4 hour；
（6）Drying and processing：By step（5）Ball milling material obtained is dried 0.5 ~ 1 hour for 50 ~ 100 DEG C under vacuum, and the present invention is made
High-coercivity manganese bismuth magnetic powder.
Further, step（3）Described in quick quenching furnace chamber pressure be 0.04 ~ 0.08 MPa, injection pressure difference be
The linear velocity of 0.09 MPa, roller are 10 ~ 50 m/s.
Further, step（4）Described in vacuum annealing heat treatment specific process parameter be：Vacuum degree better than 5 ×
10-4Pa, annealing temperature are 280 DEG C ~ 380 DEG C, and annealing time is 0.5 ~ 1 hour.
Further, step（5）Described in surfactant be polyethylene glycol.
Further, step（5）Described in organic light rare earth complex nano particle be organic light rare earth glutamic acid miaow
Azoles complex nano particle（Ln(Glu)3ImCl3）With organic light rare earth ternary organic coordination compound nano particle（Ln(acac)3phen）In one kind or two kinds of mixtures.
Further, organic light rare earth glutamic acid Imidazole complex nano particle and organic light rare earth ternary are organic
The mass ratio of complex nano particle is 1:0~1；Light rare earth ion is Ln=La, Ce, Pr, Nd, Sm, Pm or Eu.
Compared with prior art, the invention has the advantages that and advantageous effect：
（1）The present invention is using " electric arc melting+fast quenching+heat treatment+high-energy ball milling " and adulterates organic light rare earth complex nanometer
Grain method prepares high-coercivity manganese bismuth magnetic powder.Manganese bismuth fast quenching thin strap is first subjected to heat treatment and the pre- ball milling of high energy, then will be organic
Light rare earth complex nano particle, which is added in manganese-bismuth magnetic powder, carries out high-energy ball milling, due to light rare earth complex nanoparticle size
It is smaller, manganese-bismuth magnetic powder can be effectively coated, light rare earth ion is made smoothly to be substituted into the molecular grating of manganese bismuth alloy, is effectively promoted
The magnetocrystalline anisotropy of MnBi phases, coercivity are obviously improved, and increase rate can reach 40 ~ 90%；
（2）Compared with traditional directly manganese-bismuth magnetic powder of doped nanoparticle, present invention process process is simple, easy to operate, reduces
Cost is conducive to application of the high-coercivity manganese bismuth magnetic powder in more permanent magnet devices.
Specific implementation mode
With reference to embodiment and comparative example the present invention is further elaborated.
Embodiment 1
（1）Dispensing：Use purity for 99.99% or more Mn, Bi alloy, according to nominal composition Mn45Bi55Alloy weigh matching
Material；
（2）Melting：The raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting obtains
Mn45Bi55Alloy cast ingot；
（3）Fast quenching：By Mn45Bi55In the quick quenching furnace of alloy cast ingot under protection of argon gas, fast quenching obtains Mn45Bi55Alloy thin band.
Quick quenching furnace chamber pressure is 0.04 MPa, and injection pressure difference is 0.09 MPa, and the linear velocity of roller is 20 m/s；
（4）Vacuum heat：By step（3）Mn obtained45Bi55Alloy thin band carries out vacuum annealing heat treatment, obtains corresponding
Nanocrystalline M n45Bi55Alloy thin band, thermal anneal temperature are 300 DEG C, and annealing time is 0.5 hour；
（5）High-energy ball milling：By step（4）Mn obtained45Bi55Nanometer crystal alloy strip carries out high-energy ball milling, and weight is added before ball milling
Amount is Mn45Bi55The polyethylene glycol of nanometer crystal alloy strip weight 3%, ball milling 0.5 hour；It is Mn to add weight45Bi55Nanometer
Organic light rare earth glutamic acid Imidazole complex nano particle of peritectic alloy strip weight 10%（(La,Pr)(Glu)3ImCl3）, continue
Ball milling 1 hour；
（6）Drying and processing：By step（5）Ball milling material obtained is dried 1 hour for lower 80 DEG C in vacuum, and organic light rare earth is made and matches
Close the manganese-bismuth magnetic powder of object modified by nano particles.
Comparative example
For preparation process with embodiment 1, difference lies in do not add organic light rare earth glutamic acid Imidazole complex nano particle（(La,
Pr)(Glu)3ImCl3）.
Sample prepared by above two method is tested its magnetic property using vibrating specimen magnetometer.Comparison
The results are shown in Table 1.
Table 1
By table 1 as it can be seen that compared with the manganese-bismuth magnetic powder for not adding organic light rare earth complex nano particle, the present invention is used and is added with
The manganese-bismuth magnetic powder that machine light rare earth complex nano particle obtains, coercivity improve 4.1 kOe, and increase rate reaches 44%.
Embodiment 2
（1）Dispensing：Use purity for 99.99% or more Mn, Bi alloy, according to nominal composition Mn55Bi45Alloy weigh matching
Material；
（2）Melting：The raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting obtains
Mn55Bi45Alloy cast ingot；
（3）Fast quenching：By Mn55Bi45In the quick quenching furnace of alloy cast ingot under protection of argon gas, fast quenching obtains Mn55Bi45Alloy thin band.
Quick quenching furnace chamber pressure is 0.06 MPa, and injection pressure difference is 0.09 MPa, and the linear velocity of roller is 30m/s；
（4）Vacuum heat：By step（3）Mn obtained55Bi45Alloy thin band carries out vacuum annealing heat treatment, obtains corresponding
Nanocrystalline M n55Bi45Alloy thin band, thermal anneal temperature are 350 DEG C, and annealing time is 1 hour；
（5）High-energy ball milling：By step（4）Mn obtained55Bi45Nanometer crystal alloy strip carries out high-energy ball milling, and weight is added before ball milling
Amount is Mn55Bi45The polyethylene glycol of nanometer crystal alloy strip weight 6%, ball milling 1 hour；It is Mn to add weight55Bi45It is nanocrystalline
Organic light rare earth ternary organic coordination compound nano particle of alloy thin band weight 30%（(Ce,Eu)(acac)3phen）, continue ball
Mill 2 hours；
（6）Drying and processing：By step（5）Ball milling material obtained is dried 1 hour for lower 100 DEG C in vacuum, and organic light rare earth is made and matches
Close the manganese-bismuth magnetic powder of object modified by nano particles.
Comparative example
For preparation process with embodiment 2, difference lies in do not add organic light rare earth ternary organic coordination compound nano particle（(Ce,Eu)
(acac)3phen）.
Sample prepared by above two method is tested its magnetic property using vibrating specimen magnetometer.Comparison
The results are shown in Table 2.
Table 2
As can be seen from Table 2, compared with the manganese-bismuth magnetic powder for not adding organic light rare earth complex nano particle, the present invention is used and is added with
The manganese-bismuth magnetic powder that machine light rare earth complex nano particle obtains, coercivity improve 8.3 kOe, and increase rate reaches 79%.
Embodiment 3
（1）Dispensing：Use purity for 99.99% or more Mn, Bi alloy, according to nominal composition Mn55Bi45Alloy weigh matching
Material；
（2）Melting：The raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting obtains
Mn55Bi45Alloy cast ingot；
（3）Fast quenching：By Mn55Bi45In the quick quenching furnace of alloy cast ingot under protection of argon gas, fast quenching obtains Mn55Bi45Alloy thin band.
Quick quenching furnace chamber pressure is 0.08 MPa, and injection pressure difference is 0.09 MPa, and the linear velocity of roller is 45 m/s；
（4）Vacuum heat：By step（3）Mn obtained55Bi45Alloy thin band carries out vacuum annealing heat treatment, obtains corresponding
Nanocrystalline M n55Bi45Alloy thin band, thermal anneal temperature are 380 DEG C, and annealing time is 1 hour；
（5）High-energy ball milling：By step（4）Mn obtained55Bi45Nanometer crystal alloy strip carries out high-energy ball milling, and weight is added before ball milling
Amount is Mn55Bi45The polyethylene glycol of nanometer crystal alloy strip weight 9%, ball milling 1 hour；It is Mn to add weight55Bi45It is nanocrystalline
Organic light rare earth glutamic acid Imidazole complex nano particle of alloy thin band weight 50%（(Pr,Nd)(Glu)3ImCl3）With it is organic
Light rare earth ternary organic coordination compound nano particle（(Sm,Pm)(acac)3phen）Mixture, wherein their mass ratio be 1:
1, continue ball milling 4 hours；
（6）Drying and processing：By step（5）Ball milling material obtained is dried 1 hour for lower 100 DEG C in vacuum, and organic light rare earth is made and matches
Close the manganese-bismuth magnetic powder of object modified by nano particles.
Comparative example
For preparation process with embodiment 3, difference lies in do not add organic light rare earth glutamic acid Imidazole complex nano particle（(Pr,
Nd)(Glu)3ImCl3）With organic light rare earth ternary organic coordination compound nano particle（(Sm,Pm)(acac)3phen）Mixture.
Sample prepared by above two method is tested its magnetic property using vibrating specimen magnetometer.Comparison
The results are shown in Table 3.
Table 3
By table 3 as it can be seen that compared with the manganese-bismuth magnetic powder for not adding organic light rare earth complex nano particle, the present invention is used and is added with
The manganese-bismuth magnetic powder that machine light rare earth complex nano particle obtains, coercivity improve 6.8 kOe, and increase rate reaches 83%.
Claims (6)
1. a kind of method that organic light rare earth complex modified by nano particles prepares high-coercivity manganese bismuth magnetic powder, it is characterised in that packet
Include following steps：
（1）Dispensing：According to nominal composition MnyBi100-y, molar fraction y=45 or 50 or 55 or 60, use purity be 99.99% with
On Mn, Bi alloy carry out weighing and burden；
（2）Melting：The raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting obtains
MnyBi100-yAlloy cast ingot；
（3）Fast quenching：By MnyBi100-yIn the quick quenching furnace of alloy cast ingot under protection of argon gas, fast quenching obtains MnyBi100-yAlloy is thin
Band；
（4）Vacuum heat：By step（3）Mn obtainedyBi100-yAlloy thin band carries out vacuum annealing heat treatment, obtains corresponding
Nanometer crystal alloy strip；
（5）High-energy ball milling：By step（4）Mn obtainedyBi100-yNanometer crystal alloy strip carries out high-energy ball milling, is added before ball milling
Weight is MnyBi100-yThe surfactant of nanometer crystal alloy strip weight 3 ~ 9%, ball milling 0.5 ~ 1 hour；Adding weight is
MnyBi100-yOrganic light rare earth complex nano particle of nanometer crystal alloy strip weight 10 ~ 50%, continues ball milling 1 ~ 4 hour；
（6）Drying and processing：By step（5）Ball milling material obtained is dried 0.5 ~ 1 hour for 50 ~ 100 DEG C under vacuum, and the present invention is made
High-coercivity manganese bismuth magnetic powder.
2. preparing high-coercivity manganese bismuth magnetic powder according to organic light rare earth complex modified by nano particles described in claim 1
Method, it is characterised in that：Step（3）Described in quick quenching furnace chamber pressure be 0.04 ~ 0.08 MPa, injection pressure difference be 0.09
The linear velocity of MPa, roller are 10 ~ 50 m/s.
3. preparing high-coercivity manganese bismuth magnetic powder according to organic light rare earth complex modified by nano particles described in claim 1
Method, it is characterised in that：Step（4）Described in vacuum annealing heat treatment specific process parameter be：Vacuum degree better than 5 ×
10-4Pa, annealing temperature are 280 DEG C ~ 380 DEG C, and annealing time is 0.5 ~ 1 hour.
4. preparing high-coercivity manganese bismuth magnetic powder according to organic light rare earth complex modified by nano particles described in claim 1
Method, it is characterised in that：Step（5）Described in surfactant be polyethylene glycol.
5. preparing high-coercivity manganese bismuth magnetic powder according to organic light rare earth complex modified by nano particles described in claim 1
Method, it is characterised in that：Step（5）Described in organic light rare earth complex nano particle be organic light rare earth glutamic acid imidazoles
Complex nano particle（Ln(Glu)3ImCl3）With organic light rare earth ternary organic coordination compound nano particle（Ln(acac)3phen）
In one kind or two kinds of mixtures.
6. organic light rare earth complex modified by nano particles according to claim 5 prepares the side of high-coercivity manganese bismuth magnetic powder
Method, it is characterised in that：Organic light rare earth glutamic acid Imidazole complex nano particle and organic light rare earth ternary is organic matches
The mass ratio for closing object nano particle is 1:0~1；Light rare earth ion is Ln=La, Ce, Pr, Nd, Sm, Pm or Eu.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111230127A (en) * | 2020-02-25 | 2020-06-05 | 中国计量大学 | Preparation method of composite magnetic powder |
| CN112466652A (en) * | 2020-12-10 | 2021-03-09 | 泮敏翔 | Preparation method of high-coercivity manganese bismuth magnet |
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Application publication date: 20180731 |