CN108133818A - Sintered NdFeB anti-oxidation processing method - Google Patents
Sintered NdFeB anti-oxidation processing method Download PDFInfo
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- CN108133818A CN108133818A CN201711285945.2A CN201711285945A CN108133818A CN 108133818 A CN108133818 A CN 108133818A CN 201711285945 A CN201711285945 A CN 201711285945A CN 108133818 A CN108133818 A CN 108133818A
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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
- H01F41/026—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 protecting methods against environmental influences, e.g. oxygen, by surface treatment
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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
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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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
- H01F41/0266—Moulding; Pressing
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Abstract
The invention discloses sintered NdFeB anti-oxidation processing method, step includes：In airflow milling crushing process, pure oxygen is injected in airflow mill, the amount of filling into of pure oxygen is 1.0~15L/h, and the concentration of pure oxygen is not less than 99.9%, and oxygen content is 5~15ppm in airflow milling crushing system.Along with the micro oxygen uptake of particle surface while powder particle of the present invention crushes in airflow mill, form uniform passivation film, effective the avoids the direct adsorption and oxidation of air and steam, not only improves the appearance yield of magnet after sintering, improves the magnetic property of Sintered NdFeB magnet.
Description
Technical field
The invention belongs to permanent magnet preparing technical fields more particularly to one kind to change sintered NdFeB anti-oxidation processing method.
Background technology
Permanent magnet, that is, hard magnetic body, the magnet that can keep it magnetic for a long time, is not easy loss of excitation, is not easy to be magnetized.Thus, nothing
By being in industrial production or in daily life one of most common muscle material of hard magnetic body.Neodymium iron boron magnetic body is also referred to as neodymium
Magnet (Neodymium magnet), chemical formula Nd2Fe14B is a kind of artificial permanent magnet, is low by iron and price
It is honest and clean, resourceful, can stable supplying neodymium and boron element be composed, can inexpensively manufacture, while the magnetic energy product of neodymium iron boron
It can reach ferritic 10 times or more, thus, neodymium iron boron magnetic body is since its cost performance is excellent, small density is high, has excellent performance
And it is widely used in the fields such as wind-powered electricity generation, motor, VCM, unmanned plane, and with the development of electric vehicle, have in future very big
Development opportunity.At present, high-performance Ne-Fe-B permanent magnet is mainly prepared by sintering process, and wherein Zhou Shouzeng etc. exists《Sintered NdFeB is dilute
Native permanent-magnet material and technology》In disclose the fabrication processing of sintered Nd-Fe-B permanent magnet, mainly melting, powder processed, compacting
Five molding, isostatic pressed and sintering steps, specifically include dispensing, melting, hydrogen crush, the compression moulding of powder processed, powder orientation, etc. it is quiet
Pressure, vacuum-sintering.Neodymium iron boron magnetic body main phase is Nd2Fe14B, and grain boundary is mutually rich-Nd phase, rich Nd Grain-Boundary Phases current potential
Less than basic phase Nd2Fe14B and richness B phases, it is mutually very active that this will appear as rich neodymium, was fabricated in entire neodymium iron boron magnetic body
Different degrees of oxidation always occurs for Cheng Zhong, reduces the content of rare earth of magnet, high particularly with the low rare earth quickly grown at present
Performance sintered NdFeB product, manufacturing process is very strict, and the properties of product stability of production is poor, limits Nd-Fe-B materials
The application of material.Thus, how by the improvement in Sintered NdFeB magnet powder preparing processes, strengthen the anti-oxidant of powder
Property, improves the magnetic property of magnet, widens its application range, is always forward-looking manufacturer and technical staff's extensive concern
Focus.
Invention content
The goal of the invention of the present invention is a kind of sintered NdFeB anti-oxidation processing method of body, can effectively avoid sky
The direct adsorption and oxidation of gas and steam improves the magnetic property of Sintered NdFeB magnet, it is steady to solve Sintered NdFeB magnet performance
The technical issues of qualitative difference.
The problem of for being previously mentioned, the present invention provides a kind of sintered NdFeB anti-oxidation processing method, step includes：
In airflow milling crushing process, pure oxygen is injected in airflow mill, the amount of filling into of pure oxygen is 1.0~15L/h, pure oxygen
Concentration not less than 99.9%, oxygen content is 5~15ppm in airflow milling crushing system.
Preferred embodiment is：In airflow milling crushing process, gas pressure is 0.45~0.65Mpa, gas flow for 10~
25m3/ min, the disperse gas pressure of airflow mill bottom is 0.2~0.4Mpa, and gas dispersion flow is 4~8m3/min。
Preferred embodiment is：By the powder made by airflow milling through overmulling powder machine after mixing, it magnetizes in mo(u)ldenpress
Orientation is pressed into density as 3.9~4.2g/cm3Green compact, the green compact are then subjected to isostatic cool pressing, the pressure of isostatic cool pressing is
115~300MPa, time are 45~200s, and isostatic cool pressing green compact are obtained after release.
Preferred embodiment is：Isostatic cool pressing green compact are packed into sintering furnace, vacuum degree is no more than 0.3Pa, institute in the sintering furnace
It is as follows to state sintering furnace temperature-rise period：
After the sintering furnace is warming up to 250~420 DEG C, 1~3h is kept the temperature；
After the sintering furnace is warming up to 450~550 DEG C, 2~4h is kept the temperature；
After the sintering furnace is warming up to 750~850 DEG C, 1~3h is kept the temperature；
After the sintering furnace is warming up to 1020~1050 DEG C, 1~2h is kept the temperature.
Preferred embodiment is：After sintering, be filled in argon gas to the sintering furnace, in the sintering furnace air pressure for 85~
100Kpa, and the sintering furnace is cooled down simultaneously to 60~80 DEG C.
Preferred embodiment is：Before the airflow milling crushes, need neodymium iron boron raw material being broken into coarse powder, by coarse powder and first
Antioxidant mixes, and the additive amount of first antioxidant accounts for 0.03~5wt% of coarse powder weight.
Preferred embodiment is：First antioxidant includes 0.08~6 part of benzotriazole, petroleum ether 80 in parts by weight
5~20 parts of~120 parts, 5~20 parts of thymol and triphenylcarbinol.
Preferred embodiment is：In airflow milling crushing process, the second antioxidant is injected into airflow mill in a manner of spraying
In, second antioxidant includes in parts by weight：0.1~0.8 part of polyethylene oxide alkyl ethers, electrometer 0.05~
0.15 part, 10~30 parts of ethyl alcohol, 0.01~0.09 part of 1- hexadecanols.
Beneficial effects of the present invention are as follows：
1st, it along with the micro oxygen uptake of particle surface while powder particle of the present invention crushes in airflow mill, is formed uniform
Passivation film, effective the avoids the direct adsorption and oxidation of air and steam, and the appearance for not only improving magnet after sintering is qualified
Rate improves the magnetic property of Sintered NdFeB magnet.
2nd, the present invention is magnetized orientation compacting green compact by mo(u)ldenpress, and the green compact then are carried out isostatic cool pressing, cold etc.
The pressure of static pressure is 115~300MPa, and the time is 45~200s, and isostatic cool pressing green compact are obtained after release, is conducive to eliminate magnet
Interior microscopic pores improve magnet consistency, and crystal grain are avoided to elongate.
3rd, the present invention carries out low pressure sintering using same sintering furnace, not only simplifies operation, the energy saving energy, and can avoid magnetic
The oxidation that body is easily led to when sintering furnace is converted.
4th, the present invention mixes coarse powder with the first antioxidant, can not only effectively prevent Nd-Fe-B powder in process of production
Oxidation, and lubricity is also improved, so as to improve the magnetic powder degree of orientation, magnetic property also enhances therewith.
5th, the present invention injects the second antioxidant in a manner of spraying in airflow mill in airflow milling crushing process,
It can effectively ensure that NdFeB magnetic powder in the continuous oxygen-proof property for producing each stage.
6th, in antioxidant substance component of the present invention the gold in being set to airflow milling is avoided without mordant ingredient
Metal elements and rubber element generate damage.
Specific embodiment
The present invention is described in further detail below, to enable those skilled in the art being capable of evidence with reference to specification word
To implement.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more
The presence or addition of a other element or combinations.
The present invention provides a kind of sintered NdFeB anti-oxidation processing method, step includes：
In airflow milling crushing process, pure oxygen is injected in airflow mill, the amount of filling into of pure oxygen is 1.0~15L/h, pure oxygen
Concentration not less than 99.9%, oxygen content is 5~15ppm in airflow milling crushing system.
In the sintered NdFeB anti-oxidation processing method, in airflow milling crushing process, gas pressure for 0.45~
0.65Mpa, gas flow are 10~25m3/ min, the disperse gas pressure of airflow mill bottom is 0.2~0.4Mpa, disperses gas
Body flow is 4~8m3/min。
In the sintered NdFeB anti-oxidation processing method, it will be mixed by the powder that airflow milling is made through overmulling powder machine
After uniformly, density is pressed into as 3.9~4.2g/cm in the mo(u)ldenpress orientation that magnetizes3Green compact, then the green compact are carried out cold etc.
Static pressure, the pressure of isostatic cool pressing is 115~300MPa, and the time is 45~200s, and isostatic cool pressing green compact are obtained after release.
In the sintered NdFeB anti-oxidation processing method, isostatic cool pressing green compact are packed into sintering furnace, the sintering furnace
Interior vacuum degree is not more than 0.3Pa, and the sintering furnace temperature-rise period is as follows：
After the sintering furnace is warming up to 250~420 DEG C, 1~3h is kept the temperature；
After the sintering furnace is warming up to 450~550 DEG C, 2~4h is kept the temperature；
After the sintering furnace is warming up to 750~850 DEG C, 1~3h is kept the temperature；
After the sintering furnace is warming up to 1020~1050 DEG C, 1~2h is kept the temperature.
In the sintered NdFeB anti-oxidation processing method, after sintering, it is filled in argon gas to the sintering furnace, institute
It is 85~100Kpa, and cool down the sintering furnace simultaneously to 60~80 DEG C to state air pressure in sintering furnace.
In the sintered NdFeB anti-oxidation processing method, before the airflow milling crushes, need neodymium iron boron raw material
Be broken into coarse powder, coarse powder mixed with the first antioxidant, the additive amount of first antioxidant account for coarse powder weight 0.03~
5wt%.
In the sintered NdFeB anti-oxidation processing method, first antioxidant includes benzo three in parts by weight
5~20 parts of 0.08~6 part of nitrogen azoles, 80~120 parts of petroleum ether, 5~20 parts of thymol and triphenylcarbinol.
In the sintered NdFeB anti-oxidation processing method, in airflow milling crushing process, by the second antioxidant with
The mode of spraying is injected in airflow mill, and second antioxidant includes in parts by weight：Polyethylene oxide alkyl ethers 0.1~
0.8 part, 0.05~0.15 part of electrometer, 10~30 parts of ethyl alcohol, 0.01~0.09 part of 1- hexadecanols.
Embodiment 1
It present embodiments provides a kind of sintered NdFeB and adds anti-oxidation processing method, step includes：
The present embodiment is by airflow milling crushing process, by oxygenating pipeline, being injected in mill entrance forepart micro
Pure oxygen, powder particle along with the micro oxygen uptake of particle surface, forms uniform passivation film while grinding machine internal comminution.It mends
The oxygen purity entered is 99.9%, and the amount of filling into is 1L/h, and the oxygen content in airflow milling crushing system is maintained at 5ppm, air-flow milling
Broken gas pressure is 0.45MPa, and crushing gas flow is 10m3/ min, the disperse gas pressure of bottom is 0.2Mpa, disperses gas
Body flow is 4m3/ min, the powder that airflow milling is made are uniformly mixed through overmulling powder machine, and density is pressed into the mo(u)ldenpress orientation that magnetizes
3.9g/cm3Green compact, cold isostatic press further compresses green compact, green compact is packed into vacuum sintering furnace, be evacuated to vacuum degree and arrive
0.3Pa keeps the temperature draining gas hereinafter, being warming up to 250 DEG C, is warming up to 450 DEG C of heat preservation row's organic matters, is warming up to 750 DEG C of heat preservation row H2,
I.e. 1020 DEG C of DEG C of temperature liquid-phase sinterings are warming up to below main phase fusing point, and crystal boundary richness neodymium is mutually in liquid phase state at this time, at a temperature of this
Continue to keep the temperature 60min, close heater, applying argon gas to 85Kpa, the machine that blows in is cooled to 60 DEG C DEG C and comes out of the stove, and obtains blank.
Embodiment 2
It present embodiments provides a kind of sintered NdFeB and adds anti-oxidation processing method, step includes：
The present embodiment is by airflow milling crushing process, by oxygenating pipeline, being injected in mill entrance forepart micro
Pure oxygen, powder particle along with the micro oxygen uptake of particle surface, forms uniform passivation film while grinding machine internal comminution.It mends
The oxygen purity entered is 99.9%, and the amount of filling into is 15L/h, and the oxygen content in airflow milling crushing system is maintained at 15ppm, airflow milling
Crushing gas pressure is 0.65MPa, and crushing gas flow is 25m3/ min, the disperse gas pressure of bottom is 0.4Mpa, is disperseed
Gas flow is 8m3/ min, the powder that airflow milling is made are uniformly mixed through overmulling powder machine, mo(u)ldenpress magnetize orientation be pressed into it is close
Spend 4.2g/cm3Green compact, cold isostatic press further compresses green compact, green compact is packed into vacuum sintering furnace, are evacuated to vacuum degree
To 0.3Pa hereinafter, being warming up to 420 DEG C of heat preservation draining gas, 550 DEG C of heat preservation row's organic matters are warming up to, are warming up to 850 DEG C of heat preservation rows
H2, i.e. 1050 DEG C of temperature liquid-phase sinterings are warming up to below main phase fusing point, and crystal boundary richness neodymium is mutually in liquid phase state at this time, at a temperature of this
Continue to keep the temperature 120min, close heater, applying argon gas to 100Kpa, the machine that blows in is cooled to 80 DEG C and comes out of the stove, and obtains blank.
Embodiment 3
It present embodiments provides a kind of sintered NdFeB and adds anti-oxidation processing method, step includes：
Before the airflow milling crushes, need neodymium iron boron raw material being broken into coarse powder, coarse powder and the first antioxidant are mixed
It closes, the additive amount of first antioxidant accounts for coarse powder weight 0.03wt%, and first antioxidant includes in parts by weight
5 parts of 0.08 part of benzotriazole, 80 parts of petroleum ether, 5 parts of thymol and triphenylcarbinol.By in airflow milling crushing process,
By oxygenating pipeline, inject micro pure oxygen in mill entrance forepart, powder particle while grinding machine internal comminution along with
The micro oxygen uptake of particle surface forms uniform passivation film.The oxygen purity filled into be 99.9%, the amount of filling into be 15L/h, airflow milling
Oxygen content in crushing system is maintained at 15ppm, and it is 0.65MPa that airflow milling, which crushes gas pressure, and crushing gas flow is 25m3/
Min, the disperse gas pressure of bottom is 0.4Mpa, and gas dispersion flow is 8m3/ min, the powder that airflow milling is made is through overmulling powder
Machine is uniformly mixed, and density 4.2g/cm is pressed into the mo(u)ldenpress orientation that magnetizes3Green compact, cold isostatic press further compresses green compact,
Green compact are packed into vacuum sintering furnace, vacuum degree is evacuated to 0.3Pa hereinafter, being warming up to 420 DEG C of heat preservation draining gas, is warming up to
550 DEG C of heat preservation row's organic matters are warming up to 850 DEG C of heat preservation row H2, i.e. 1050 DEG C of temperature liquid-phase sinterings are warming up to below main phase fusing point,
Crystal boundary richness neodymium is mutually in liquid phase state at this time, continues to keep the temperature 120min at a temperature of this, closes heater, applying argon gas to 100Kpa,
The machine that blows in is cooled to 80 DEG C and comes out of the stove, and obtains blank.
Embodiment 4
It present embodiments provides a kind of sintered NdFeB and adds anti-oxidation processing method, step includes：
Before the airflow milling crushes, need neodymium iron boron raw material being broken into coarse powder, coarse powder and the first antioxidant are mixed
It closes, the additive amount of first antioxidant accounts for coarse powder weight 05wt%, and first antioxidant includes benzene in parts by weight
And 20 parts of 6 parts of triazole, 120 parts of petroleum ether, 20 parts of thymol and triphenylcarbinol.By in airflow milling crushing process, leading to
Cross oxygenating pipeline, inject micro pure oxygen in mill entrance forepart, powder particle while grinding machine internal comminution along with
The grain micro oxygen uptake in surface, forms uniform passivation film.The oxygen purity filled into is 99.9%, and the amount of filling into is 15L/h, and air-flow is milled
Oxygen content in broken system is maintained at 15ppm, and it is 0.65MPa that airflow milling, which crushes gas pressure, and crushing gas flow is 25m3/
Min, the disperse gas pressure of bottom is 0.4Mpa, and gas dispersion flow is 8m3/ min, the powder that airflow milling is made is through overmulling powder
Machine is uniformly mixed, and density 4.2g/cm is pressed into the mo(u)ldenpress orientation that magnetizes3Green compact, cold isostatic press further compresses green compact,
Green compact are packed into vacuum sintering furnace, vacuum degree is evacuated to 0.3Pa hereinafter, being warming up to 420 DEG C of heat preservation draining gas, is warming up to
550 DEG C of heat preservation row's organic matters are warming up to 850 DEG C of heat preservation row H2, i.e. 1050 DEG C of temperature liquid-phase sinterings are warming up to below main phase fusing point,
Crystal boundary richness neodymium is mutually in liquid phase state at this time, continues to keep the temperature 120min at a temperature of this, closes heater, applying argon gas to 100Kpa,
The machine that blows in is cooled to 80 DEG C and comes out of the stove, and obtains blank.
Embodiment 5
It present embodiments provides a kind of sintered NdFeB and adds anti-oxidation processing method, step includes：
Before the airflow milling crushes, need neodymium iron boron raw material being broken into coarse powder, coarse powder and the first antioxidant are mixed
It closes, the additive amount of first antioxidant accounts for coarse powder weight 05wt%, and first antioxidant includes benzene in parts by weight
And 20 parts of 6 parts of triazole, 120 parts of petroleum ether, 20 parts of thymol and triphenylcarbinol.By in airflow milling crushing process, leading to
Oxygenating pipeline is crossed, micro pure oxygen is injected in mill entrance forepart, while the second antioxidant is injected into gas in a manner of spraying
It flows in grinding machine, second antioxidant includes in parts by weight：0.1 part of polyethylene oxide alkyl ethers, electrometer 0.05
Part, 10 parts of ethyl alcohol, 0.01 part of 1- hexadecanols.Powder particle is while grinding machine internal comminution along with the micro suction of particle surface
Oxygen forms uniform passivation film.The oxygen purity filled into is 99.9%, and the amount of filling into is 15L/h, the oxygen in airflow milling crushing system
Content is maintained at 15ppm, and it is 0.65MPa that airflow milling, which crushes gas pressure, and crushing gas flow is 25m3/ min, point of bottom
It is 0.4Mpa to dissipate gas pressure, and gas dispersion flow is 8m3/ min, the powder that airflow milling is made are uniformly mixed through overmulling powder machine,
Density 4.2g/cm is pressed into the mo(u)ldenpress orientation that magnetizes3Green compact, cold isostatic press further compresses green compact, green compact is packed into
Vacuum sintering furnace is evacuated to vacuum degree to 0.3Pa hereinafter, being warming up to 420 DEG C of heat preservation draining gas, is warming up to 550 DEG C of heat preservation rows
Organic matter is warming up to 850 DEG C of heat preservation row H2, i.e. 1050 DEG C of temperature liquid-phase sinterings are warming up to below main phase fusing point, and crystal boundary is rich at this time
Neodymium continues to keep the temperature 120min mutually in liquid phase state, at a temperature of this, closes heater, applying argon gas to 100Kpa, the machine that blows in cooling
It comes out of the stove to 80 DEG C, obtains blank.
Embodiment 6
It present embodiments provides a kind of sintered NdFeB and adds anti-oxidation processing method, step includes：
Before the airflow milling crushes, need neodymium iron boron raw material being broken into coarse powder, coarse powder and the first antioxidant are mixed
It closes, the additive amount of first antioxidant accounts for coarse powder weight 05wt%, and first antioxidant includes benzene in parts by weight
And 20 parts of 6 parts of triazole, 120 parts of petroleum ether, 20 parts of thymol and triphenylcarbinol mixing.By in airflow milling crushing process
In, by oxygenating pipeline, micro pure oxygen is injected in mill entrance forepart, while the second antioxidant is penetrated in a manner of spraying
Enter in airflow mill, second antioxidant includes in parts by weight：0.8 part of polyethylene oxide alkyl ethers, electrometer
0.15 part, 30 parts of ethyl alcohol, 0.09 part of 1- hexadecanols.Powder particle is micro- along with particle surface while grinding machine internal comminution
Oxygen uptake is measured, forms uniform passivation film.The oxygen purity filled into is 99.9%, and the amount of filling into is 15L/h, in airflow milling crushing system
Oxygen content be maintained at 15ppm, it is 0.65MPa that airflow milling, which crushes gas pressure, and crushings gas flow is 25m3/ min, bottom
Disperse gas pressure is 0.4Mpa, and gas dispersion flow is 8m3/ min, the powder that airflow milling is made mix equal through overmulling powder machine
It is even, it is pressed into density 4.2g/cm in the mo(u)ldenpress orientation that magnetizes3Green compact, cold isostatic press further compresses green compact, green compact filled
Enter vacuum sintering furnace, be evacuated to vacuum degree to 0.3Pa hereinafter, being warming up to 420 DEG C of heat preservation draining gas, be warming up to 550 DEG C of heat preservations
Organic matter is arranged, is warming up to 850 DEG C of heat preservation row H2, i.e. 1050 DEG C of temperature liquid-phase sinterings are warming up to below main phase fusing point, at this time crystal boundary
Rich neodymium continues to keep the temperature 120min mutually in liquid phase state, at a temperature of this, closes heater, applying argon gas to 100Kpa, and the machine that blows in is cold
But it comes out of the stove to 80 DEG C, obtains blank.
Comparative example
A kind of sintered NdFeB preparation method, step include：
1) NbFeB sintered raw material are broken into coarse powder；
2) rare earth metal is subjected to the quick-fried processing of hydrogen, powder, powder diameter and coarse powder grain size phase made from the step 1 is made
Together；
3) rare earth metal powder made from step 2 is added to according to 1~3 ‰ ratio in coarse powder made from step 1, into
Row uniformly mixes powder；
4) powder made from step 3 is carried out air-flow to grind, powder is made, the powder size is 2.0~4.0 μm；
5) powder made from step 4 is pressed into green compact；
6) green compact are put into sintering furnace under the action of protective gas and by the sintering stove evacuation, pressure is
0.4~0.6Pa.
Experiment effect data
Table 1 is gained sintered NdFeB product oxygen content and magnetism testing result in Examples 1 to 6 and comparative example
| Number | Oxygen content (ppm) | Br(kGs) | Hcj(kOe) | (BH)m |
| Embodiment 1 | 660 | 13.28 | 24.75 | 42.37 |
| Embodiment 2 | 650 | 13.26 | 24.62 | 42.48 |
| Embodiment 3 | 590 | 13.28 | 24.75 | 42.37 |
| Embodiment 4 | 610 | 13.26 | 24.62 | 42.48 |
| Embodiment 5 | 605 | 13.98 | 25.01 | 43.10 |
| Embodiment 6 | 595 | 13.14 | 24.98 | 42.05 |
| Comparative example | 1340 | 12.13 | 22.45 | 41.05 |
The oxygen content of Examples 1 to 6 and comparative example is not it is found that carry out the Nd-Fe-B permanent magnetic material of anti-oxidant treatment of the present invention
Oxygen content is apparently higher than the present invention and carries out the permanent-magnet material after anti-oxidant treatment in material.By Examples 1 to 6 and the magnetism of comparative example
It can be it is found that it be capable of the invention anti-oxidant that the magnetic property for carrying out the Nd-Fe-B permanent magnet material of anti-oxidant treatment of the present invention, which is apparently higher than,
Processed Nd-Fe-B permanent magnet material.
Although the embodiments of the present invention have been disclosed as above, but its be not restricted in specification and embodiment it is listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, it is of the invention and unlimited
In specific details.
Claims (8)
1. sintered NdFeB anti-oxidation processing method, which is characterized in that step includes：
In airflow milling crushing process, pure oxygen is injected in airflow mill, the amount of filling into of pure oxygen is 1.0~15L/h, pure oxygen it is dense
Degree is not less than 99.9%, and oxygen content is 5~15ppm in airflow milling crushing system.
2. sintered NdFeB anti-oxidation processing method according to claim 1, which is characterized in that in airflow milling crushing process
In, gas pressure is 0.45~0.65Mpa, and gas flow is 10~25m3/ min, the disperse gas pressure of airflow mill bottom
For 0.2~0.4Mpa, gas dispersion flow is 4~8m3/min。
3. sintered NdFeB anti-oxidation processing method according to claim 2, which is characterized in that will be made by airflow milling
Powder through overmulling powder machine after mixing, be pressed into density as 3.9~4.2g/cm in the mo(u)ldenpress orientation that magnetizes3Green compact, so
The green compact are subjected to isostatic cool pressing afterwards, the pressure of isostatic cool pressing is 115~300MPa, and the time is 45~200s, after release
To isostatic cool pressing green compact.
4. sintered NdFeB anti-oxidation processing method according to claim 3, which is characterized in that fill isostatic cool pressing green compact
Enter sintering furnace, vacuum degree is not more than 0.3Pa in the sintering furnace, and the sintering furnace temperature-rise period is as follows：
After the sintering furnace is warming up to 250~420 DEG C, 1~3h is kept the temperature；
After the sintering furnace is warming up to 450~550 DEG C, 2~4h is kept the temperature；
After the sintering furnace is warming up to 750~850 DEG C, 1~3h is kept the temperature；
After the sintering furnace is warming up to 1020~1050 DEG C, 1~2h is kept the temperature.
5. sintered NdFeB anti-oxidation processing method according to claim 4, which is characterized in that after sintering, be filled with
In argon gas to the sintering furnace, air pressure is 85~100Kpa in the sintering furnace, and cools down the sintering furnace simultaneously to 60~80
℃。
6. sintered NdFeB anti-oxidation processing method according to claim 1, which is characterized in that the airflow milling crushes
Before, it needs neodymium iron boron raw material being broken into coarse powder, coarse powder be mixed with the first antioxidant, first antioxidant adds
Dosage accounts for 0.03~5wt% of coarse powder weight.
7. sintered NdFeB anti-oxidation processing method according to claim 6, which is characterized in that first antioxidant
Include 0.08~6 part of benzotriazole, 80~120 parts of petroleum ether, 5~20 parts of thymol and triphenylcarbinol 5 in parts by weight
~20 parts.
8. sintered NdFeB anti-oxidation processing method according to claim 7, which is characterized in that in airflow milling crushing process
In, the second antioxidant is injected in a manner of spraying in airflow mill, second antioxidant includes in parts by weight：It is poly-
0.1~0.8 part of ethylene oxide alkyl ether, 0.05~0.15 part of electrometer, 10~30 parts of ethyl alcohol and 1- hexadecanols 0.01~
0.09 part.
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