CN105234386B - Method for preparing sintered neodymium iron boron through grain boundary diffusion of heavy rare earth - Google Patents
Method for preparing sintered neodymium iron boron through grain boundary diffusion of heavy rare earth Download PDFInfo
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- CN105234386B CN105234386B CN201510306946.5A CN201510306946A CN105234386B CN 105234386 B CN105234386 B CN 105234386B CN 201510306946 A CN201510306946 A CN 201510306946A CN 105234386 B CN105234386 B CN 105234386B
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Abstract
The invention provides a method for preparing sintered neodymium iron boron through grain boundary diffusion of heavy rare earth. The method comprises the steps that heavy rear earth matter and organic solvent are mixed to prepare turbid liquid; the turbid liquid is subjected to dispersion treatment in neodymium iron boron alloy powder, and neodymium iron boron powder is obtained; and after being heated, cooled and sieved, the neodymium iron boron powder is subjected to compression molding, sintering and aging treatment, and the sintered neodymium iron boron is obtained. According to the method, the heavy rear earth matter and the neodymium iron boron alloy powder are sintered, so that the heavy rear earth matter and the neodymium iron boron powder are mixed evenly, the preparation process is simple, the using amount of the heavy rear earth matter is small, and the utilization rate of the heavy rear earth matter is high; meanwhile, the coercivity and temperature resistance of the sintered neodymium iron boron are improved, and the consistency of properties of the sintered neodymium iron boron is guaranteed.
Description
Technical field
The present invention relates to a kind of grain boundary decision heavy rare earth prepares the processing technique of sintered NdFeB, sintering neodymium is particularly improved
The grain boundary diffusion process of ferrum boron, the composition of overall improvement sintered NdFeB, raising sintered NdFeB coercivity and heat resistance
Technique.
Background technology
Sintered NdFeB is the permanent magnet material of current most cost performance, there is the title of " magnetic king ".Compared with other permanent magnets, burn
The Curie temperature of knot neodymium iron boron is low, and this is the principal element for restricting it in commercial Application.In order to improve the heatproof of sintered NdFeB
Performance, people have attempted various methods, and in existing conclusion, the characteristic of the antiferromagnetic coupling of heavy rare earth can offset light rare earth
The low problem of the Curie temperature that brings after ferromagnetic coupling, but heavy rare earth is few in nature storage, excessively asks for unfavorable to heavy rare earth
In the core value of sustainable development.Reducing the service efficiency for using and improving heavy rare earth of heavy rare earth becomes current sintering neodymium
The important brainstorm subject of ferrum boron.
Numerous scholars have done numerous studies to this, and explore optimal coercivity model.Japanese scholars are developed earliest
The model of grain boundary decision, by applying and heavy rare earth is diffused into magnet and is shown by heat-treating methods, makes coercivity and heatproof
Performance is improved significantly, and it has the disadvantage it will be evident that because material surface can only be coated to, thus its diffusion depth is only limited
In micron order, this results in the technique and is only capable of processing laminar permanent magnet material, and limited to block rare earth permanent magnetic action；Domestic one
The method that a little research institutions have studied dual alloy mixing, but the effect for mixing is unsatisfactory, is mainly manifested in heavy rare earth compound
The powder fluidity of itself bad dispersibility, in particular up to Nano grade is poor, easy conglomeration, and it has high fusing point, in height
Can not be sintered together with Fe-Nd-B very well during temperature sintering, the defects such as hole, sand holes occur, cause magnetic property low and squareness
Difference；Additionally, simple powder mixing method cannot also accomplish high efficiency dispersion, it is impossible to give full play to the effect of heavy rare earth.
The content of the invention
It is an object of the invention to solve at least the above and/or defect, and provide at least will be described later excellent
Point.
This method by way of atomization it is also an object that by the way that heavy rare earth material is prepared into into suspension, be added to
In Nd Fe B alloys powder and mixed；Then it is brilliant from crystal boundary to principal phase at high temperature during vacuum-sintering after shaping
Grain diffusion, ultimately forms preferable neodymium iron boron coercivity model, improves coercivity and heat resistance.
A kind of method that grain boundary decision heavy rare earth prepares sintered NdFeB, heavy rare earth material and organic solvent are mixed
Suspension, obtains neodymium iron boron powder a in decentralized processing to Nd Fe B alloys powder, it is heat-treated, cool down, sieve after pressed
Make type, sintering and Ageing Treatment.
Preferably, the preparation method of the suspension is as follows：First by 100 weight portion heavy rare earth materials and 5-20 weight portions
Organic solvent is transferred to ball mill ball milling and makes jelly, and Ball-milling Time is 2-5h, is drawn off and adds 30-80 weight portions to have
Machine solvent, stirring 0.5-3h obtains the suspension.
Preferably, the decentralized processing refers to that the suspension is added in Nd Fe B alloys powder Jing after atomization, and
Mix 30min-180min in mixed powder machine under inert atmosphere protection and obtain the neodymium iron boron powder a, the inert atmosphere is
Noble gases or nitrogen.
Preferably, the heat treated refers to be placed in neodymium iron boron powder a and adds in heat container that evacuation is simultaneously heated to
30-70 DEG C, insulation 1-5h obtains neodymium iron boron powder b.
Preferably, the organic solvent is the alcohols, one or more of ketone or ethers that boiling point is 60-100 DEG C
Mixture.
Preferably, the heavy rare earth material be nanoscale, its be the oxide and/or fluoride of Dy, Tb, Ho wherein
A kind of compound or various mixture.
Preferably, the mass fraction that the consumption of the heavy rare earth material accounts for the Nd Fe B alloys powder consumption is
0.5%-3%.
Preferably, the Nd Fe B alloys powder is to carry out melting, hydrogen under vacuum by Nd Fe B alloys to crush,
Then it is milled into using air-flow, wherein the smelting temperature is 1450-1550 DEG C, the broken desorption temperature of the hydrogen is 350-600
DEG C, temperature retention time is 2-10h, and the particle mean size of the Nd Fe B alloys powder is 3-5 microns.
Preferably, by the neodymium iron boron powder b it is compressing in Magnetic field press, in vacuum sintering furnace sintering and when
Effect, wherein, the sintering temperature of the vacuum-sintering is 1050-1100 DEG C, and sintering time is 3-5h, and the timeliness is divided into twice,
First time timeliness is incubated 2-5h at 880-920 DEG C, and second timeliness is incubated 2-4h at 470-600 DEG C.
The present invention at least includes following beneficial effect：
1st, after heavy rare earth material is mixed with organic solvent, ball mill grinding is put into, organic solvent is then added again
And heavy rare earth suspension is made in stirring, is become aerosol and is added in neodymium iron boron powder.Stable heavy rare earth is prepared first
Dispersion, in the way of being atomized neodymium iron boron powder surface is sprayed onto so that neodymium iron boron powder can be good at mixing, contributes to weight
Rare earth is evenly distributed in neodymium iron boron crystal boundary, realizes improving the coercitive purpose of sintered NdFeB；Reduce heavy rare earth simultaneously
Usage amount, improve the utilization ratio of heavy rare earth, saved cost；In addition, the method need not to purchase magnetron sputtering etc. high-end
Equipment, with splendid using effect and convenience, easily realizes.
2nd, what is selected is lower boiling organic solvent, after heavy rare earth material and neodymium iron boron powder are sufficiently mixed, is transferred to
Plus in heat container, just organic solvent can be removed under the auxiliary of evacuation, using low-temperature heat, both reach dispersion weight dilute
Soil material purpose, turn avoid organic solvent and molding neodymium iron boron, magnetic property is had undesirable effect.
3rd, under an inert atmosphere, heavy rare earth material and neodymium iron boron powder are mixed, are prevented from neodymium iron boron powder and are oxidized,
And then part neodymium iron boron powder can be avoided to be oxidized the inhomogeneities for causing sintered NdFeB magnetic.
Specific embodiment
Embodiment of the present invention is further illustrated below in conjunction with embodiment, but does not limit the practical range of the present invention.
Embodiment 1
Add Dy in Nd Fe B alloys melting, wherein, the consumption of Dy accounts for the mass fraction of Nd Fe B alloys consumption and is
0.5%；Then it is compressing in Magnetic field press, sintering and timeliness in vacuum sintering furnace, wherein, the burning of the vacuum-sintering
Junction temperature is 1065 DEG C, and sintering time is 4h, and the timeliness is divided into twice, and first time timeliness is incubated 5h at 920 DEG C, second
Timeliness is incubated 4h at 470 DEG C.
Embodiment 2
Fe-Nd-B alloy powder is mixed into 30min with the fluoride of Dy in mixed powder machine, the fluoride consumption of wherein Dy is accounted for
The mass fraction of Nd Fe B alloys consumption is 0.5%；Then it is compressing in Magnetic field press, in vacuum sintering furnace sintering and
Timeliness, wherein, the sintering temperature of the vacuum-sintering is 1065 DEG C, and sintering time is 4h, and the timeliness is divided into twice, for the first time
Timeliness is incubated 5h at 920 DEG C, and second timeliness is incubated 4h at 470 DEG C.
Embodiment 3
A kind of method that grain boundary decision heavy rare earth prepares sintered NdFeB, heavy rare earth material and organic solvent are mixed
Suspension, obtains neodymium iron boron powder a in decentralized processing to Nd Fe B alloys powder, it is heat-treated, cool down, sieve after pressed
Make type, sintering and Ageing Treatment.
Wherein, the preparation method of the suspension is as follows：First 100 weight portion heavy rare earth materials and 5 parts by weight of ethanol are turned
Move on to ball mill ball milling and make jelly, Ball-milling Time is 2h, be drawn off and add 80 parts by weight of ethanol, stirring 3h to obtain institute
State suspension；Wherein, the heavy rare earth material is the fluoride of Dy；After heavy rare earth material is mixed with organic solvent, put into
Ball mill grinding, then adds again organic solvent and heavy rare earth suspension is made in stirring, is become aerosol and is added to neodymium
In ferrum boron powder.Stable heavy rare earth dispersion is prepared first, is sprayed onto neodymium iron boron powder surface in the way of being atomized so that neodymium
Ferrum boron powder can be good at mixing, contributes to heavy rare earth and is evenly distributed in around neodymium iron boron crystal boundary, realize improving sintering neodymium
The coercitive purpose of ferrum boron；Reduce the usage amount of heavy rare earth simultaneously, improve the utilization ratio of heavy rare earth, saved into
This；In addition, the method need not purchase the high-end devices such as magnetron sputtering, with splendid using effect and convenience, easily realize.
Wherein, the decentralized processing refers to that the suspension is added in Nd Fe B alloys powder, and lazy Jing after atomization
Property atmosphere protection under mix 30min in mixed powder machine and obtain the neodymium iron boron powder a, the inert atmosphere is nitrogen；In inertia
Under atmosphere, heavy rare earth material and neodymium iron boron powder are mixed, be prevented from neodymium iron boron powder and be oxidized, and then part can be avoided
Neodymium iron boron powder is oxidized the inhomogeneities for causing sintered NdFeB magnetic.
Wherein, the heat treated refer to by neodymium iron boron powder a be placed in plus heat container in, evacuation is simultaneously heated to 70 DEG C,
Insulation 5h obtains neodymium iron boron powder b.
Wherein, the heavy rare earth material is nanoscale.
Wherein, the mass fraction that the consumption of the heavy rare earth material accounts for the Nd Fe B alloys powder consumption is 0.5%.
Wherein, the Nd Fe B alloys powder is to carry out melting, hydrogen under vacuum by Nd Fe B alloys to crush, then
It is milled into using air-flow, wherein the smelting temperature is 1550 DEG C, the broken desorption temperature of the hydrogen is 350 DEG C, and temperature retention time is
10h, the granularity of described Nd Fe B alloys powder is 5 microns.
Wherein, the neodymium iron boron powder b is cooled to into room temperature, is suppressed in Magnetic field press after sieving in 80 mesh sieving machines
Molding, in vacuum sintering furnace sintering and timeliness, wherein, the sintering temperature of the vacuum-sintering is 1065 DEG C, and sintering time is
4h, the timeliness is divided into twice, and first time timeliness is incubated 5h at 920 DEG C, and second timeliness is incubated 4h at 470 DEG C.
Embodiment 4
A kind of method that grain boundary decision heavy rare earth prepares sintered NdFeB, heavy rare earth material and organic solvent are mixed
Suspension, obtains neodymium iron boron powder a in decentralized processing to Nd Fe B alloys powder, it is heat-treated, cool down, sieve after pressed
Make type, sintering and Ageing Treatment.
Wherein, the preparation method of the suspension is as follows：First by 100 parts of heavy rare earth materials and 10 parts by weight of ethanol and 10 weights
Amount part acetone is transferred to ball mill ball milling and makes jelly, and Ball-milling Time is 5h, be drawn off and add 20 parts by weight of ethanol and
10 pbw acetones, stirring 0.5h obtains the suspension；Wherein, described heavy rare earth material is the oxide of 50 weight portion Dy
With 50 weight portion Tb fluorides.
Wherein, the decentralized processing refers to that the suspension is added in Nd Fe B alloys powder, and lazy Jing after atomization
Property atmosphere protection under mix 180min in mixed powder machine and obtain the neodymium iron boron powder a, the inert atmosphere is helium.
Wherein, the heat treated refer to by neodymium iron boron powder a be placed in plus heat container in, evacuation is simultaneously heated to 50 DEG C,
Insulation 1h obtains neodymium iron boron powder b.
Wherein, the heavy rare earth material is nanoscale.
Wherein, the mass fraction that the consumption of the heavy rare earth material accounts for the Nd Fe B alloys powder consumption is 3%.
Wherein, the Nd Fe B alloys powder is to carry out melting, hydrogen under vacuum by Nd Fe B alloys to crush, then
It is milled into using air-flow, wherein the smelting temperature is 1450 DEG C, the broken desorption temperature of the hydrogen is 600 DEG C, and temperature retention time is
2h, the granularity of the Nd Fe B alloys powder is 3 microns.
Wherein, the neodymium iron boron powder b is cooled to into room temperature, is suppressed in Magnetic field press after sieving in 80 mesh sieving machines
Molding, in vacuum sintering furnace sintering and timeliness, wherein, the sintering temperature of the vacuum-sintering is 1100 DEG C, and sintering time is
5h, the timeliness is divided into twice, and first time timeliness is incubated 2h at 880 DEG C, and second timeliness is incubated 4h at 600 DEG C.
Embodiment 5
A kind of method that grain boundary decision heavy rare earth prepares sintered NdFeB, heavy rare earth material and organic solvent are mixed
Suspension, obtains neodymium iron boron powder a in decentralized processing to Nd Fe B alloys powder, it is heat-treated, cool down, sieve after pressed
Make type, sintering and Ageing Treatment.
Wherein, the preparation method of the suspension is as follows：First by 100 parts of heavy rare earth materials and 5 parts by weight Methanol, 8 weight
Part butanone and 3 weight portion glycol dimethyl ethers are transferred to ball mill ball milling and make jelly, and Ball-milling Time is 3h, is drawn off simultaneously
10 parts by weight Methanol, 30 weight portion butanone and 18 weight portion glycol dimethyl ethers, stirring 2h are added to obtain the suspension；Its
In, the heavy rare earth material is the fluoride of the oxide of 50 weight portion Dy, the oxide of 30 weight portion Tb and 20 weight portion Ho.
Wherein, the decentralized processing refers to that the suspension is added in Nd Fe B alloys powder, and lazy Jing after atomization
Property atmosphere protection under mix 90min in mixed powder machine and obtain the neodymium iron boron powder a, the inert atmosphere is neon.
Wherein, the heat treated refer to by neodymium iron boron powder a be placed in plus heat container in, evacuation is simultaneously heated to 30 DEG C,
Insulation 4h obtains neodymium iron boron powder b.
Wherein, the heavy rare earth material is nanoscale.
Wherein, the mass fraction that the consumption of the heavy rare earth material accounts for the Nd Fe B alloys powder consumption is 1%.
Wherein, the Nd Fe B alloys powder is to carry out melting, hydrogen under vacuum by Nd Fe B alloys to crush, then
It is milled into using air-flow, wherein the smelting temperature is 1500 DEG C, the broken desorption temperature of the hydrogen is 400 DEG C, and temperature retention time is
5h, the granularity of the Nd Fe B alloys powder is 4.5 microns.
Wherein, the neodymium iron boron powder b is cooled to into room temperature, is suppressed in Magnetic field press after sieving in 80 mesh sieving machines
Molding, in vacuum sintering furnace sintering and timeliness, wherein, the sintering temperature of the vacuum-sintering is 1050 DEG C, and sintering time is
3h, the timeliness is divided into twice, and first time timeliness is incubated 4h at 900 DEG C, and second timeliness is incubated 3.5h at 550 DEG C.
It is (hard according to GB/T3217 permanent magnetism by by sintering in above-described embodiment 1-5 after the neodymium iron boron magnetic body surface grinding that obtains
Magnetic) magnetism of material test method carries out performance detection, and the magnetic for measuring is as follows：
As seen from the above table, add heavy rare earth material in the way of being atomized, improve the using effect of heavy rare earth, significantly improve
The coercivity of sintered NdFeB；With increasing for heavy rare earth addition, remanent magnetism and maximum magnetic energy product are basically unchanged, but coercivity
It is improved significantly；Data also show that the method can obtain the good product of concordance (HK/Hcj is good).
Although embodiment of the present invention is disclosed as above, it is not restricted to listed in description and embodiment
With.It can be applied to completely various suitable the field of the invention.For those skilled in the art, can be easily
Realize other modification.Therefore under the general concept limited without departing substantially from claim and equivalency range, the present invention is not limited
In specific details and shown here as the embodiment with description.
Claims (7)
1. a kind of method that grain boundary decision heavy rare earth prepares sintered NdFeB, it is characterised in that heavy rare earth material is molten with organic
Agent is mixed and made into suspension, and neodymium iron boron powder a, heat-treated, cooling, mistake are obtained in decentralized processing to Nd Fe B alloys powder
It is pressed after sieve, sinters and Ageing Treatment；
The preparation method of the suspension is as follows：First 100 weight portion heavy rare earth materials and 5-20 weight parts organic solvents are shifted
Jelly is made to ball mill ball milling, Ball-milling Time is 2-5h, be drawn off and add 30-80 weight parts organic solvents, stirred
0.5-3h obtains the suspension；
The decentralized processing refers to that the suspension is added in Nd Fe B alloys powder, and in inert atmosphere protection Jing after atomization
Under mix 30min-180min in mixed powder machine and obtain the neodymium iron boron powder a, the inert atmosphere is noble gases or nitrogen.
2. the method that grain boundary decision heavy rare earth as claimed in claim 1 prepares sintered NdFeB, it is characterised in that the heating
Process refer to by neodymium iron boron powder a be placed in plus heat container in, evacuation is simultaneously heated to 30-70 DEG C, and insulation 1-5h obtains neodymium iron boron
Powder b.
3. the method that grain boundary decision heavy rare earth as claimed in claim 2 prepares sintered NdFeB, it is characterised in that described organic
Solvent is the mixture of one or more of the alcohols that boiling point is 60-100 DEG C, ketone or ethers.
4. the method that grain boundary decision heavy rare earth as claimed in claim 1 prepares sintered NdFeB, it is characterised in that described heavy dilute
Soil material is nanoscale, and it is the one of which compound or various mixture of the oxide of Dy, Tb, Ho and/or fluoride.
5. the method that grain boundary decision heavy rare earth as claimed in claim 4 prepares sintered NdFeB, it is characterised in that described heavy dilute
It is 0.5%-3% that the consumption of soil material accounts for the mass fraction of the Nd Fe B alloys powder consumption.
6. the method that grain boundary decision heavy rare earth as claimed in claim 1 prepares sintered NdFeB, it is characterised in that the neodymium ferrum
Boron alloy powder is to carry out melting, hydrogen under vacuum by Nd Fe B alloys to crush, and is then milled into using air-flow, wherein institute
Smelting temperature is stated for 1450-1550 DEG C, the broken desorption temperature of the hydrogen is 350-600 DEG C, and temperature retention time is 2-10h, described
The particle mean size of Nd Fe B alloys powder is 3-5 microns.
7. the method that grain boundary decision heavy rare earth as claimed in claim 2 prepares sintered NdFeB, it is characterised in that by the neodymium
Ferrum boron powder b is compressing in Magnetic field press, sintering and timeliness in vacuum sintering furnace, wherein, the burning of the vacuum-sintering
Junction temperature is 1050-1100 DEG C, and sintering time is 3-5h, and the timeliness is divided into twice, and first time timeliness is protected at 880-920 DEG C
Warm 2-5h, second timeliness is incubated 2-4h at 470-600 DEG C.
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Families Citing this family (4)
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| CN106158205A (en) * | 2016-08-29 | 2016-11-23 | 京磁材料科技股份有限公司 | A kind of preparation method of neodymium iron boron magnetic body |
| CN106205926B (en) * | 2016-09-23 | 2019-05-24 | 北京中科三环高技术股份有限公司 | A kind of preparation method of rare-earth magnet |
| CN107492429A (en) * | 2017-08-09 | 2017-12-19 | 江西金力永磁科技股份有限公司 | A kind of high temperature resistant neodymium iron boron magnetic body and preparation method thereof |
| CN108511180B (en) * | 2018-03-26 | 2020-03-31 | 廊坊京磁精密材料有限公司 | Preparation method of anti-oxidation neodymium iron boron magnet |
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