CN107240470A - A kind of low weightless Sintered NdFeB magnet and preparation method - Google Patents
A kind of low weightless Sintered NdFeB magnet and preparation method Download PDFInfo
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- CN107240470A CN107240470A CN201710564733.1A CN201710564733A CN107240470A CN 107240470 A CN107240470 A CN 107240470A CN 201710564733 A CN201710564733 A CN 201710564733A CN 107240470 A CN107240470 A CN 107240470A
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- H—ELECTRICITY
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- 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
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
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- H01F1/053—Alloys characterised by their composition containing rare earth metals
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- 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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- 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
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Abstract
Pass through optimization of C/C composites, improve alloy casting piece columanar structure structure, control powder particles size and distribution, addition appropriate lubricant and antioxidant, control magnet oxygen content, regulate and control the measures such as crystal boundary there is provided a kind of preparation method of Sintered NdFeB magnet, reach the corrosion proof purpose for improving sintered NdFeB product.Praseodymium neodymium 26.0% 33.0%, boron 0.85% 1.05%, dysprosium 0 9%, terbium 0 3.0%, aluminium 0.01% 1.0%, copper 0 0.3%, cobalt 0.3% 4%, zirconium 0 0.2%, niobium 0 0.5%, gallium 0 0.3% and iron 61.5% 68.6% are weighed by element weight percent, fusing casting is carried out and obtains slab；Slab is put into processing in rotary hydrogen crushing furnace and obtains coarse powder；Lubricant is added into coarse powder be milled obtaining fine powder；Lubricant and antioxidant are added into fine powder, powder machine is mixed with bipyramid and mixes powder acquisition powder；Model is made, green product is obtained, sinters and cool down acquisition product.
Description
Technical field
In particular it is a kind of preparation side of low weightless neodymium iron boron magnetic body the present invention relates to neodymium iron boron magnetic body production field
Method.
Background technology
Neodymium iron boron magnetic body has excellent magnetic performance, and its application field is quite extensive, is related to electronic computer, electronic
In terms of machine and generator, NMR imaging device, stereo set, communication, ore dressing, automation, Aero-Space.Using high property
Energy Sintered NdFeB magnet, can not only improve the service behaviour of magnetic device, can also realize the miniaturization or miniaturization of device, drop
Low energy consumption.
Although sintering neodymium body boron magnet permanent magnetism excellent performance, corrosion resistance is poor, mainly there is following 3 reasons:
(1) structure of material itself.Sintered NdFeB alloy has heterogeneous structure, and the oxidability of each phase is different,
The rich-Nd phase for being distributed in grain boundaries is easy to preferentially aoxidize with richness B phases, forms intercrystalline corrosion.The consistency of other magnet is not
Height, it is more loose to add oxide, and porosity is big, and the surface of magnet is hardly formed oxide film, once the oxidation company of resulting in
Lock reactor, accelerated oxidation.And because the volume fraction of magnet principal phase Nd2Fe14B phases is general all more than 90%, it is electric when being formed
During chemical part corrosion cell, the characteristics of negative electrode big with primary anode, the corrosion electric current density of grain boundaries rich-Nd phase and richness B phases compared with
Greatly, intercrystalline corrosion and destruction are accelerated.
(2) impurity present in alloy.Pollution impurity that may be present mainly has O, H, N in sintered NdFeB alloy,
C, Si, Cl and chloride etc., wherein endanger most serious to corrosive nature is oxygen, chlorine and chloride.The main table of corrosion of magnet
It is now oxidizing process, and the pollution of chlorine and chloride particularly sodium chloride will accelerate the oxidizing process of magnet.
(3) environment of work.Temperature environment, ambient condition and humidity and pressure etc. have larger to the corrosion behavior of magnet
Influence.
Now with appointed condition, technology, the progress in terms of managerial skills sinters the production water of neodymium body boron magnet
Flat to be all greatly improved, overall industry magnet performance is significantly lifted, and corresponding production cost has and significantly declined.But
It is the corrosion resistance difference never effective solution of magnet.Sintered NdFeB has an excellent magnetic property, but its corrosion resistance
Can be poor, its application is strongly limit, therefore, how to improve its corrosion resistance and is given birth to as sintered neodymium iron boron material
The major issue produced and used.The present invention mainly introduces a kind of low weightless sintering neodymium body boron preparation method, passes through party's legal system
Standby magnet have it is relatively low it is weightless (<2mg/cm2), corrosion resistance is significantly better than the magnet prepared using conventional method.
Sinter neodymium body boron magnetic material, its usual Making programme be dispensing, melting, broken hydrogen, powder processed, orientation suppress, etc. it is quiet
Pressure, sintering, tempering, post-processing, surface treatment etc..
The content of the invention
Present invention is generally directed to the existing anti-corrosion sex differernce of sintered NdFeB magnet steel and corresponding production technology it is not enough there is provided
A kind of low weightless Sintered NdFeB magnet and preparation method thereof, so as to improve the corrosion resistance of magnet.By optimization of C/C composites and getting rid of band
Piece alloy structure, the distribution of control powder particles and powder content, crystal grain thinning, regulate and control crystal boundary distributed mutually, etc. raising product
Hcj, prepares low weightless magnet steel, solves the problem of the batch production of low weightless sintered NdFeB product.
In order to solve the above technical problems, being in particular a kind of neodymium iron the present invention relates to neodymium iron boron magnetic body production field
The preparation method of boron magnet, comprises the following steps：
(1) praseodymium neodymium 26.0%-33.0%, boron 0.85%-1.05%, dysprosium 0-9%, terbium 0- are weighed by element weight percent
3.0%th, aluminium 0.01%-1.0%, copper 0-0.3%, cobalt 0.3%-4%, zirconium 0-0.2%, niobium 0-0.5%, gallium 0-0.3% and iron
61.5%-68.6%.
(2) material for weighing step (1) is fitted into crucible, and crucible is evacuated into below 15Pa, is dried with 50kw power
Stove, when vacuum is less than 15Pa, then applying argon gas to 26-29kPa increase power to 500-600kw meltings, after iron fusing again
Refining 6-12 minute to temperature be 1400-1530 DEG C when start casting, during casting copper rod rotate linear speed control in 1.1-1.5m/
S, obtains slab and cools down；
(3) slab for obtaining step (2) is put into rotary hydrogen crushing furnace, is evacuated to below 1Pa, is passed through 0.066-
0.098MPa hydrogen, saturation is inhaled after hydrogen, is heated to 540-600 DEG C, dehydrogenase 34-10 hours is cooled to discharging after normal temperature and obtains thick
Powder；
(4) added in the coarse powder obtained to step (3) coarse powder weight 0-0.1% lubricant and 0-0.2% it is anti-oxidant
Three-dimensional mixed powder machine is added after agent is well mixed and mixes powder 0.5-4 hours, then powder is added and is milled in airflow milling, was milled
System Control for Oxygen Content exists in journey<1000ppm, it is SMD2.4-4.0 microns, D90/D10 to obtain powder particles<5.5 fine powder；
(5) fine powder weight 0%-0.1% lubricant and 0-0.2% antioxygen are added in the fine powder obtained to step (4)
Agent, mixes powder machine with V-type and mixes 0.5-4 hours acquisition fine powder materials of powder；
(6) powder for obtaining step (5) is according to the big little makings model of product size, and in press system oxygen content<
1.0%, mold center's magnetic field intensity>Orientation compacting is carried out under conditions of 1.5T, green density is reached 3.6-4.3g/cm3, so
Green density is set to bring up to 4.4-4.7g/cm using isostatic pressed compacting afterwards3, obtain green product；
(7) green product for obtaining step (6) removes vacuum packaging bag under airbreak environment, and nitrogen charging is then put into rapidly
In the glove box of protection, green product is removed film pendulum by the Control for Oxygen Content in glove box within 1.0% in glove box
Enter in graphite, be then sent through sintering furnace, sintering furnace is evacuated to below 1Pa, after slow heating exhaust, highest sintering
Furnace temperature is kept for 1020-1100 DEG C, is incubated 3-12 hours, terminates rear applying argon gas and be cooled to less than 100 DEG C to be warming up to again
870-930 DEG C or directly it is furnace-cooled to 870-930 DEG C, is incubated 2-5 hours, then applying argon gas are cooled to less than 90 DEG C, then heat up
2-7 hours are incubated to 460-600 DEG C, insulation is cooled to less than 80 DEG C after terminating and come out of the stove.
As the further optimization of the technical program, the lubricant described in a kind of preparation method of neodymium iron boron magnetic body of the invention
The YSH-06 neodymium iron boron lubricant agent specials produced for Tianjin Yue Sheng magnetoelectricities Technology Co., Ltd..
As the further optimization of the technical program, a kind of preparation method of neodymium iron boron magnetic body of the invention, it is characterised in that：
Described antioxidant is the YSH-01 neodymium iron boron special antioxidants of Tianjin Yue Sheng magnetoelectricities Technology Co., Ltd..
A kind of of the invention preparation method of the low weightless magnet of neodymium iron boron has the beneficial effect that：
By optimization of C/C composites, improve alloy casting piece columanar structure structure, control powder particles size and distribution, addition is suitable
The lubricant and antioxidant of amount, control magnet oxygen content, and regulating and controlling the measures such as crystal boundary, there is provided a kind of system of Sintered NdFeB magnet
Preparation Method, reaches the corrosion proof purpose for improving sintered NdFeB product.
Embodiment
Embodiment one：
In particular it is a kind of preparation method of neodymium iron boron magnetic body the present invention relates to neodymium iron boron magnetic body production field, bag
Include following steps：
(1) praseodymium neodymium 26.0%-33.0%, boron 0.85%-1.05%, dysprosium 0-9%, terbium 0- are weighed by element weight percent
3.0%th, aluminium 0.01%-1.0%, copper 0-0.3%, cobalt 0.3%-4%, zirconium 0-0.2%, niobium 0-0.5%, gallium 0-0.3% and iron
61.5%-68.6%.Wherein plus cobalt to improve magnet corrosion resistance it is very crucial.The Co for entering rich neodymium phase in magnet is formed
Nd3Co phases, although its electrode potential is still negative than principal phase Nd2Fe14B, mutually improve a lot than the rich neodymium without Co；
Nd2Fe14B、Nd3Co and rich neodymium phase chemical-electrical potential.Therefore containing Nd3Mutually its corrosion resistance is significantly improved the rich neodymium of Co phases, particularly
Effect is especially apparent in the hygrothermal environment of HTHP, so that weightless reduction.And Nd3Co fusing point is total to rich neodymium phase
Brilliant fusion temperature is approached, (being 664 DEG C and 655 DEG C respectively), therefore will not reduce immersional wetting of the rich neodymium with respect to main phase grain, right
The distribution of magnet richness neodymium phase has no side effect.Therefore, magnet Co contents are properly increased, and Co is made in sintered magnet by modified technique
Distribution in each phase is more reasonable, is to improve the corrosion proof important means of magnet.For there is the product compared with high corrosion-resistant requirement, match somebody with somebody
Co contents should not be low by 1.0% in side.
(2) material for weighing step (1) is fitted into crucible, and crucible is evacuated into below 15Pa, is dried with 50kw power
Stove, when vacuum is less than 15Pa, then applying argon gas to 26-29kPa increase power to 500-600kw meltings, after iron fusing again
Refining 6-12 minute to temperature be 1400-1530 DEG C when start casting, during casting copper rod rotate linear speed control in 1.1-1.5m/
S, obtains slab and cools down；Slab structure plays material impact, optimization casting to final magnet grain size, distribution of richness RE phases etc.
Chip architecture turns into the key technology for obtaining high performance magnet.
(3) slab for obtaining step (2) is put into rotary hydrogen crushing furnace, is evacuated to below 1Pa, is passed through 0.066-
0.098MPa hydrogen, saturation is inhaled after hydrogen, is heated to 540-600 DEG C, dehydrogenase 34-10 hours is cooled to discharging after normal temperature and obtains thick
Powder；
(4) added in the coarse powder obtained to step (3) coarse powder weight 0-0.1% lubricant and 0-0.2% it is anti-oxidant
Three-dimensional mixed powder machine is added after agent is well mixed and mixes powder 0.5-4 hours, then powder is added and is milled in airflow milling, was milled
System Control for Oxygen Content exists in journey<1000ppm, it is SMD2.4-4.0 microns, D90/D10 to obtain powder particles<5.5 fine powder；
Powder particles are thin, and distribution is concentrated, and are conducive to being uniformly distributed for rich neodymium phase in sintering process, so as to be conducive to improving magnet anti-corrosion
Property.Oxygen content is appropriate in other magnet, is conducive to improving the corrosion resistance of magnet.Therefore, the not oxidized situation of magnet is being ensured
Under, appropriate oxygenating is needed in pulverizing process.
(5) fine powder weight 0%-0.1% lubricant and 0-0.2% antioxygen are added in the fine powder obtained to step (4)
Agent, mixes powder machine with V-type and mixes 0.5-4 hours acquisition powders of powder；Lubricant is properly added, is conducive to powder oriented moulding, is improved
The degree of orientation, so that increase remanent magnetism, but lubricant and antioxidant addition may excessively reduce coercivity, may result in magnetic
Body carbon content is exceeded, reduces the corrosion resistance of magnet.Therefore, in the case where ensuring that properties of product are qualified, antioxygen is added less as far as possible
Agent and lubricant.
(6) powder for obtaining step (5) is according to the big little makings model of product size, and in press system oxygen content<
1.0%, mold center's magnetic field intensity>Orientation compacting is carried out under conditions of 1.5T, green density is reached 3.6-4.3g/cm3, so
Green density is set to bring up to 4.4-4.7g/cm using isostatic pressed compacting afterwards3, obtain green product；Press system too high oxygen level,
Product oxidation deformation, and hydraulic performance decline can be caused.
(7) green product for obtaining step (6) removes vacuum packaging bag under airbreak environment, and nitrogen charging is then put into rapidly
In the glove box of protection, green product is removed film pendulum by the Control for Oxygen Content in glove box within 1.0% in glove box
Enter in graphite, be then sent through sintering furnace, sintering furnace is evacuated to below 1Pa, after slow heating exhaust, highest sintering
Furnace temperature is kept for 1020-1100 DEG C, is incubated 3-12 hours, terminates rear applying argon gas and be cooled to less than 100 DEG C to be warming up to again
870-930 DEG C or directly it is furnace-cooled to 870-930 DEG C, is incubated 2-5 hours, then applying argon gas are cooled to less than 90 DEG C, then heat up
2-7 hours are incubated to 460-600 DEG C, insulation is cooled to less than 80 DEG C after terminating and come out of the stove.In order to confirm magnet optimal sintering and
Temperature, sets different temperatures to be tested by gradient respectively in the highest holding temperature of three phases, optimal to confirm
Sintering and temperature.Sintering temperature is too high, and soaking time is long all to may result in product burning, crystal grain occurs extremely long
Greatly, coercivity declines；And sintering temperature is relatively low, soaking time is partially short, can cause product underburnt, and product density is too low, remanent magnetism,
The performance parameters such as maximum magnetic energy product decline.And suitable aging temp and corresponding soaking time, it can be ensured that rich neodymium distributed mutually
Evenly, agglomeration is reduced, so as to improve the corrosion resistance of magnet, the weightlessness of magnet is reduced.Therefore, suitable sintering temperature is selected
Degree and correspondence soaking time, suitable aging temp and corresponding soaking time are very crucial, it is necessary to for different product testings
Different temperature and times, finds out optimal technique.
Described lubricant is the YSH-06 neodymium iron boron lubricant agent specials that Tianjin Yue Sheng magnetoelectricities Technology Co., Ltd. produces, and is one
Macromolecule esters polymer is planted, there is preferable lubricity, dispersiveness, oxygen-proof property to sintered NdFeB product and product is improved
The effect of performance.
Described antioxidant is the YSH-01 neodymium iron boron special antioxidants of Tianjin Yue Sheng magnetoelectricities Technology Co., Ltd., is
A kind of low molecule alkane polymer, has preferable oxygen-proof property, lubricity to sintered NdFeB product and enhances product performance
Effect.
Concrete case one：A kind of low weightless N38SH magnets.
1. dispensing.Formula is as follows：Praseodymium neodymium 28.2%, dysprosium 1.3%, gadolinium 2.1%, boron are weighed by element weight percent
0.97%th, aluminium 0.75%, copper 0.15%, cobalt 1.2%, zirconium 0.04%, niobium 0.27%, gallium 0.18%, remaining is iron.
2. melting.Above-mentioned dispensing is fitted into crucible, the vacuum of stove is evacuated to below 10Pa, with 50kw power bakers,
When vacuum is less than 5Pa, then applying argon gas to 26.8kPa increase power to 550kw meltings, are refined 7 minutes after iron fusing,
Measurement molten steel temperature starts casting when being 1450-1470 DEG C, and the linear speed that copper rod rotates during casting is controlled in 1.32m/s, is cast
Piece is simultaneously cooled down, and is discharged after blow-on after slab cooling.
3. hydrogen is broken.Above-mentioned slab is put into rotary hydrogen crushing furnace, below 1Pa is evacuated to, 0.066MPa hydrogen is passed through
Gas, saturation is inhaled after hydrogen, is heated to 540 DEG C of dehydrogenase 34s hour, is cooled to discharging after normal temperature and is obtained coarse powder.
4. powder processed.The antioxidant for adding coarse powder weight 0.1% to coarse powder adds three-dimensional mixed powder machine and mixes powder after being well mixed
1.5 hours, then powder is added and is milled in airflow milling, oxygen content 90-110ppm in milling process obtains powder particles
For SMD 2.8-3.0um, D90/D10<5.2 fine powder.Added into obtained fine powder fine powder weight 0.03% lubricant and
0.08% antioxidant, mixes powder machine with V-type and mixes 3 hours acquisition powders of powder.Oxygen content is appropriate in magnet, is conducive to improving magnet
Corrosion resistance.Therefore, appropriate oxygenating is needed in the case where ensuring that magnet is not oxidized, in pulverizing process.
(5) fine powder weight 0%-0.1% lubricant and 0-0.2% antioxygen are added in the fine powder obtained to step (4)
Agent, mixes powder machine with V-type and mixes 0.5-4 hours acquisition powders of powder；Lubricant is properly added, is conducive to powder oriented moulding, is improved
The degree of orientation, so that increase remanent magnetism, but lubricant and antioxidant addition may excessively reduce coercivity, may result in magnetic
Body carbon content is exceeded, reduces the corrosion resistance of magnet.Therefore, it is as few anti-oxidant as possible in the case where ensuring that properties of product are qualified
Agent and the addition of lubricant.
(6) suppress.During orientation compacting, press system oxygen content<0.1%, to substantially ensure that powder is not oxidized, in mould
Core field intensity>1.8T is to improve the degree of orientation of magnet, and green density is 3.8-3.9g/cm3.The pressure of isostatic pressed is used
Green density brings up to 4.6-4.7g/cm after 160MPa, isostatic pressed3.Press system too high oxygen level, can cause product oxidation change
Shape, and hydraulic performance decline, green density is too high in addition, and orientation resistance is increased, and is unfavorable for the lifting of remanent magnetism.
(7) sinter.The green product that step (6) is obtained removes vacuum packaging bag under airbreak environment, is then placed in and fills
In the glove box of nitrogen protection, green product is removed film by the Control for Oxygen Content in glove box within 0.2% in glove box
Swing in graphite, be then sent through sintering furnace, sintering furnace is evacuated to below 1Pa, sintering furnace temperature keeps 1020-1100
DEG C, 7 hours are incubated, terminates rear applying argon gas and be cooled to less than 90 DEG C to be warming up to 870-930 DEG C again or being directly furnace-cooled to
870-930 DEG C, 3 hours are incubated, then applying argon gas are cooled to less than 90 DEG C, then are warming up to 460-600 DEG C and be incubated 5 hours, insulation
Less than 80 DEG C are cooled to after end to come out of the stove.The above-mentioned temperature model for being warming up to 870-930 DEG C or being directly furnace-cooled to 870-930 DEG C can
To choose 900 DEG C, 905 DEG C, 910 DEG C, 915 DEG C, 925 DEG C of equitemperatures, 470 can be chosen by being warming up to 460-600 DEG C of temperature model
DEG C, 485 DEG C, 500 DEG C, 520 DEG C, 550 DEG C, 580 DEG C of equitemperatures.Sintering temperature is too high, and overlong time all may result in product
, there is abnormal grain growth in burning, and coercivity declines；And sintering temperature is relatively low, time length partially can then cause product underburnt, product
Density is too low, and remanent magnetism etc. declines.
The neodymium iron boron magnetic body magnet oxygen content 700-1000ppm of acquisition, magnetic property and weightlessness (130 DEG C of test condition,
2.6bar, 95%RH, 168h) test as shown in the table.
Certainly, described above not limitation of the present invention, the present invention is also not limited to the example above, the art
The variations, modifications, additions or substitutions that those of ordinary skill is made in the essential scope of the present invention, fall within the guarantor of the present invention
Protect scope.
Claims (3)
1. a kind of low weightless sintered NdFeB preparation method, it is characterised in that：
(1) praseodymium neodymium 26.0%-33.0%, boron 0.85%-1.05%, dysprosium 0-9%, terbium 0- are weighed by element weight percent
3.0%th, aluminium 0.01%-1.0%, copper 0-0.3%, cobalt 0.3%-4%, zirconium 0-0.2%, niobium 0-0.5%, gallium 0-0.3% and iron
61.5%-68.6%；
(2) material for weighing step (1) is fitted into crucible, and crucible is evacuated into below 15Pa, with 50kw power bakers, directly
When being less than 15Pa to vacuum, then applying argon gas to 26-29kPa increase power to 500-600kw meltings, are refined again after iron fusing
Start casting when being 1400-1530 DEG C to temperature within 6-12 minutes, the linear speed that copper rod rotates during casting is controlled in 1.1-1.5m/s, is obtained
Obtain slab and cool down；
(3) slab for obtaining step (2) is put into rotary hydrogen crushing furnace, is evacuated to below 1Pa, is passed through 0.066-
0.098MPa hydrogen, saturation is inhaled after hydrogen, is heated to 540-600 DEG C, dehydrogenase 34-10 hours is cooled to discharging after normal temperature and obtains thick
Powder；
(4) antioxidant for the lubricant and 0-0.2% for adding coarse powder weight 0-0.1% in the coarse powder obtained to step (3) is mixed
Close the uniform rear mixed powder machine of three-dimensional that adds and mix powder 0.5-4 hours, then will be milled in powder addition airflow milling, in milling process
System Control for Oxygen Content exists<1000ppm, acquisition powder particles are 2.4-4.0 microns of SMD, D90/D10<5.5 fine powder；
(5) fine powder weight 0%-0.1% lubricant and 0-0.2% antioxidant are added in the fine powder obtained to step (4),
Powder machine, which is mixed, with V-type mixes 0.5-4 hours acquisition fine powder materials of powder；
(6) powder for obtaining step (5) is according to the big little makings model of product size, and in press system oxygen content<1.0%,
Mold center's magnetic field intensity>Orientation compacting is carried out under conditions of 1.5T, green density is reached 3.6-4.3g/cm3, then use
Isostatic pressed compacting makes green density bring up to 4.4-4.7g/cm3, obtain green product；
(7) green product for obtaining step (6) removes vacuum packaging bag under airbreak environment, and nitrogen filled protection is then put into rapidly
Glove box in, the Control for Oxygen Content in glove box within 1.0%, in glove box by green product removal film swing in stone
In print cartridge, sintering furnace is then sent through, sintering furnace is evacuated to below 1Pa, after slow heating exhaust, highest sintering furnace temperature
Degree is kept for 1020-1100 DEG C, is incubated 3-12 hours, terminates rear applying argon gas and be cooled to less than 100 DEG C to be warming up to 870-930 again
DEG C or be directly furnace-cooled to 870-930 DEG C, be incubated 2-5 hours, then applying argon gas are cooled to less than 90 DEG C, then are warming up to 460-
600 DEG C are incubated 2-7 hours, and insulation is cooled to less than 80 DEG C after terminating and come out of the stove.
2. the low weightless sintered NdFeB preparation method of one kind according to claim 1, it is characterised in that：Described lubricant
The YSH-06 neodymium iron boron lubricant agent specials produced for Tianjin Yue Sheng magnetoelectricities Technology Co., Ltd..
3. the low weightless sintered NdFeB preparation method of one kind according to claim 1, it is characterised in that：Described is anti-oxidant
Agent is the YSH-01 neodymium iron boron special antioxidants of Tianjin Yue Sheng magnetoelectricities Technology Co., Ltd..
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| CN112614685B (en) * | 2020-11-26 | 2022-06-24 | 宁波源盛磁业有限公司 | Sintered neodymium-iron-boron permanent magnet oxygen control preparation method and prepared neodymium-iron-boron permanent magnet |
| CN112863844A (en) * | 2021-03-24 | 2021-05-28 | 陈凯华 | Preparation process of corrosion-resistant neodymium iron boron magnet |
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