CN104637664B - A kind of preparation method of corrosion resistance Nd-Fe-B permanent magnet - Google Patents
A kind of preparation method of corrosion resistance Nd-Fe-B permanent magnet Download PDFInfo
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- CN104637664B CN104637664B CN201310574777.4A CN201310574777A CN104637664B CN 104637664 B CN104637664 B CN 104637664B CN 201310574777 A CN201310574777 A CN 201310574777A CN 104637664 B CN104637664 B CN 104637664B
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Abstract
The present invention provides a kind of manufacturing methods of corrosion resistance Sintered NdFeB permanent magnet, Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice by the manufacturing method including the use of vacuum induction rapid hardening slab stove, it is broken and carry out Dehydroepiandrosterone derivative method and the quick-fried broken powder of hydrogen is crushed using high velocity inert gas air-flow using in airflow milling that rapid hardening thin slice is subjected to hydrogen explosion, the micro mist that average particle size is 15 μm is made, micro mist is orientated after die mould and obtains high-performance Ne-Fe-B permanent-magnet material through oversintering, then product will be processed, and will be manufactured into the small dimension magnet of demand.Sealing pores finally are carried out to permanent magnet, obtain a kind of corrosion proof Nd-Fe-B permanent magnet material.The manufacturing method of the present invention can effectively improve the corrosion resisting property of Nd-Fe-B permanent magnet, can improve the service life of Nd-Fe-B permanent magnet.
Description
Technical field
The present invention relates to a kind of production methods of Nd-Fe-B permanent magnet, specifically, being related to corrosion resistance Nd-Fe-B permanent magnetic material
The preparation method of material.
Background technology
Neodymium iron boron (NdFeB) permanent-magnet material is the highest rare earth permanent-magnetic material of current magnetic property, is referred to as " magnetic king ".
It is widely used in the numerous areas such as electroplating device, machinery, medical treatment, automobile, foreground is very wide.But NdFeB magnets there is
The shortcomings that poor corrosion resistance, has seriously affected the service life of Nd-Fe-B permanent magnet, reduces the stability of product and reliable
Property.Therefore coating or application must be used to it, to solve its Anticorrosion.How to produce a kind of high anti-corrosion, processing is simple
Nd-Fe-B permanent magnet material is extremely urgent.The anti-corrosion method of Nd-Fe-B permanent magnet material has much at present.Wherein there are electronickelling, electricity
It is zinc-plated（CN1421547A、CN1056133A）, shooting of multi-layer nickel electroplating（CN102568732）, copper facing（CN1514889A）, phosphatization
（CN101022051）, a variety of methods such as electrophoretic paint.Comparing processing simply has the methods of phosphatization, passivation.
Neodymium iron boron porous surface, easily shelters evil people and countenance evil practices, and sealing of hole is the hole progress Seal treatment to piece surface, so that its
The treatment fluid (such as degreasing fluid, pickle, plating solution) of various processes does not penetrate into hole afterwards, to avoid the inside of coating after plating rotten
Erosion such as patent（CN200610172643）.Sealing of hole is using leaching zinc stearate method：Zinc stearate is heated to 130~140 DEG C of fusings,
Part is impregnated into about 20min, the dry 30min at 60 DEG C is taken out, or be placed at room temperature for 2h or more, makes its solidification.Then it is fallen
Angle, the surface treatments such as plating.Another after heating Nd-Fe-B permanent magnet contact low temperature hole sealing agent rear surface micropore
Volume-diminished, in hole pressure reduction play the role of hole sealing agent sucking to close magnet hole, help to reduce in electroplating process
Various acid, erosions of the alkaline solution to magnet surface.Such as applied by Shenyang Zhong Bei Tong Ci Science and Technology Co., Ltd.
（CN201210040318.3）A kind of surface hot dipping method for sealing of Nd-Fe-B permanent magnet material is using in methyl oleate, ethyl oleate
One or two, when using two kinds of mixtures, its ratio be 1: 1 or 1: 2.First, by Nd-Fe-B permanent magnet 120~240
It is heated in DEG C temperature, heating time is 1~2.5 hour；Then, the Nd-Fe-B permanent magnet after heating is impregnated in hole sealing agent and is sealed
The micropore for closing surface of Nd-Fe-B permanent magnet takes out after permanent magnet surfaces temperature is less than 40 DEG C.Or it uses Nd-Fe-B permanent magnetic
Material vacuumizes, and is then immersed in hole sealing agent, sucks pore-sealing liquid by pressure, achievees the effect that sealing of hole.Such as by Wuhan
The apllied patent of material protection（CN200610166528, CN200610166529）It is its vacuum equipment for using and is not easy
Realize produce in enormous quantities, and all above-mentioned sealing of holes all have problems that once have be overlapped if will appear sealing of hole not on ask
Topic, and directly there is antiseptic property after cannot achieve sealing of hole, it needs to carry out relevant surface treatment.The present invention is used to neodymium iron
The method that boron permanent magnet uses room temperature leaching carries out rapid curing, realizes the sealing of hole of magnet, and it is anti-to effectively raise magnet
Rotten performance.
Invention content
It is an object of the invention to overcome the deficiencies of existing technologies, a kind of corrosion resistance Nd-Fe-B permanent magnet material is provided.
The manufacturing method of corrosion resistance Sintered NdFeB permanent magnet according to the present invention, the manufacturing method include following step
Suddenly：1）Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice using vacuum induction rapid hardening slab stove, roller speed is controlled in 1~5m/s,
Sheet thickness is 0.1~0.3mm；2）By step 1）In rapid hardening thin slice carry out that hydrogen explosion is broken and Dehydroepiandrosterone derivative；3）In airflow milling
It is middle to utilize high-speed flow inert gas by step 2）In the powder after hydrogen explosion is broken and Dehydroepiandrosterone derivative it is broken, average particle size is made
For 1~5 μm of micro mist；4）By step 3）In micro mist obtained be packed into mold in atmosphere of inert gases, mold is heat safe
Carbon or carbide, dress powder density ranging from 2~4g/cm3；5）By step 4）In equipped with micro mist mold under inert gas protection
It is placed in 1~3T pulsed magnetic fields and is orientated, orientation sequence is positive and negative, to which green compact magnet be made；6）In inert gas shielding
It is lower by step 4）Middle green compact magnet is placed in vacuum sintering furnace, 2~6h is sintered at 900~1150 DEG C, then carry out 800~950 DEG C
It is handled with 400~600 DEG C of second annealings, to which high performance sintered magnet product be made；And 7）The sintered magnet is produced
Product are processed, and are manufactured into the small dimension sintered magnet product of demand, are carried out at sealing of hole to the small dimension sintered magnet product
Reason.
Preferably, the inert gas is argon gas or nitrogen.
The manufacturing method of corrosion resistance Sintered NdFeB permanent magnet according to the present invention, the sealing pores include following step
Suddenly：（1）Degreasing degreasing：Sodium phosphate, sodium carbonate or sodium hydroxide is added and carries out conventional degreasing degreasing；（2）Acid pickling and rust removing：It adds
Salpeter solution carries out conventional acid pickling and rust removing, washing；（3）Normal-temperature hole sealing processing is carried out using pore-sealing liquid；And（4）It is dry.
Preferably, the pore-sealing liquid be selected from water-soluble fluorine carbon resin, water soluble acrylic resin, water soluble alkyd resin,
At least one of water-soluble epoxy resin, water soluble phenol resin.Wherein, the ratio of two or more resin can be
Any ratio preferably selects equal proportion because they can dissolve each other.It is highly preferred that carrying out normal-temperature hole sealing using pore-sealing liquid
When processing, the pH of the pore-sealing liquid is adjusted with sodium polyphosphate and arrives=8.0.
The manufacturing method of corrosion resistance Sintered NdFeB permanent magnet provided by the invention, it is compared with prior art, of the invention
The remarkable advantage of manufacturing method is：1）Sealing pores provided by the present invention can carry out at normal temperatures, and can be effective
Raising Nd-Fe-B permanent magnet corrosion resisting property；2）Pore-sealing liquid ingredient of the present invention is simple, and neodymium iron boron can be improved after product
The service life of permanent magnet, especially in the environment of high humidity high fever.
Specific implementation mode
Below with reference to embodiment, the present invention will be further described, and the embodiment of the present invention is merely to illustrate the present invention's
Technical solution, and the non-limiting present invention.
Embodiment 1
Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice using vacuum induction rapid hardening slab stove, roller speed is controlled in 5m/s,
Sheet thickness is 0.3mm；It is broken and carry out Dehydroepiandrosterone derivative that above-mentioned rapid hardening thin slice is subjected to hydrogen explosion；High speed is utilized in airflow milling
Inert gas flow（Argon gas）The quick-fried broken powder of hydrogen is crushed, the micro mist that average particle size is 5 μm is made；By micro mist obtained
Mold is packed into argon inert gas atmosphere, mold is heat safe carbon or carbide, dress powder density ranging from 2g/cm3.
Mold equipped with micro mist is placed under argon inert gas protection in 3T pulsed magnetic fields and is orientated, orientation sequence is just
Anyway anti-, to which green compact magnet be made；Green compact magnet is placed in vacuum sintering furnace under argon inert gas protection, 900
DEG C sintering 6h, then carry out 950 DEG C and 600 DEG C of second annealings are handled, to obtained high performance sintered magnet product.
Sintered magnet product is processed, demand 9.2 × 5.2 × 1mm small dimension magnets are manufactured into.Addition sodium phosphate,
Sodium carbonate or sodium hydroxide carry out conventional degreasing degreasing；It adds salpeter solution and carries out conventional acid pickling and rust removing, washing；Using sealing of hole
Liquid is that water-soluble fluorine carbon resin carries out normal-temperature hole sealing processing, drying.Refer to table 1.
Embodiment 2
Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice using vacuum induction rapid hardening slab stove, it is thin by the control of roller speed in 1/s
Piece thickness is 0.1mm；It is broken and carry out Dehydroepiandrosterone derivative that above-mentioned rapid hardening thin slice is subjected to hydrogen explosion；High speed nitrogen is utilized in airflow milling
The quick-fried broken powder of hydrogen is crushed by gas gas flow, and the micro mist that average particle size is 1 μm is made；By micro mist obtained in indifferent gas
Body（Nitrogen）Mold is packed into atmosphere, mold is heat safe carbon or carbide, dress powder density ranging from 4g/cm3.
By the mold equipped with micro mist in inert gas（Nitrogen）It is placed in 1T pulsed magnetic fields and is orientated under protection, orientation sequence is
It is positive and negative, to which green compact magnet be made；In inert gas（Nitrogen）Green compact magnet is placed in vacuum sintering furnace under protection,
1150 DEG C of sintering 2h, then 800 DEG C and 400 DEG C of second annealing processing are carried out, to which high performance sintered magnet product be made.
Sintered magnet product is processed, demand 9.2 × 5.2 × 1mm small dimension magnets are manufactured into.Addition sodium phosphate,
Sodium carbonate or sodium hydroxide carry out conventional degreasing degreasing；It adds salpeter solution and carries out conventional acid pickling and rust removing, washing；Using sealing of hole
Liquid is that water soluble acrylic resin carries out normal-temperature hole sealing processing, drying.Refer to table 1.
Embodiment 3
Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice using vacuum induction rapid hardening slab stove, roller speed is controlled in 3m/s,
Sheet thickness is 0.2mm；It is broken and carry out Dehydroepiandrosterone derivative that above-mentioned rapid hardening thin slice is subjected to hydrogen explosion；High speed is utilized in airflow milling
Inert gas flow（Argon gas）The quick-fried broken powder of hydrogen is crushed, the micro mist that average particle size is 4 μm is made；By micro mist obtained
In inert gas（Argon gas）Mold is packed into atmosphere, mold is heat safe carbon or carbide, dress powder density ranging from 3g/cm3.
By the mold equipped with micro mist in inert gas（Argon gas）It is placed in 2T pulse magnetic field and is orientated under protection, orientation sequence is
It is positive and negative, to which green compact magnet be made；In inert gas（Argon gas）Green compact magnet is placed in vacuum sintering furnace under protection,
1110 DEG C of sintering 4h, then 900 DEG C and 480 DEG C of second annealing processing are carried out, to which high performance sintered magnet product be made.
Sintered magnet product is processed, demand 9.2 × 5.2 × 1mm small dimension magnets are manufactured into.Addition sodium phosphate,
Sodium carbonate or sodium hydroxide carry out conventional degreasing degreasing；It adds salpeter solution and carries out conventional acid pickling and rust removing, washing；Using sealing of hole
Liquid is that water soluble alkyd resin carries out normal-temperature hole sealing processing, drying.Refer to table 1.
Embodiment 4
Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice using vacuum induction rapid hardening slab stove, roller speed is controlled in 3m/s,
Sheet thickness is 0.2mm；It is broken and carry out Dehydroepiandrosterone derivative that above-mentioned rapid hardening thin slice is subjected to hydrogen explosion；High speed is utilized in airflow milling
Inert gas flow（Nitrogen）The quick-fried broken powder of hydrogen is crushed, the micro mist that average particle size is 3 μm is made；By micro mist obtained
In inert gas（Nitrogen）Mold is packed into atmosphere, mold is heat safe carbon or carbide, dress powder density ranging from 4g/cm3.
By the mold equipped with micro mist in inert gas（Nitrogen）It is placed in 3T pulsed magnetic fields and is orientated under protection, orientation sequence is
It is positive and negative, to which green compact magnet be made；In inert gas（Nitrogen）Green compact magnet is placed in vacuum sintering furnace under protection,
1050 DEG C of sintering 4h, then 850 DEG C and 500 DEG C of second annealing processing are carried out, to which high performance sintered magnet product be made.
Sintered magnet product is processed, demand 9.2 × 5.2 × 1mm small dimension magnets are manufactured into.Addition sodium phosphate,
Sodium carbonate or sodium hydroxide carry out conventional degreasing degreasing；It adds salpeter solution and carries out conventional acid pickling and rust removing, washing；Using sealing of hole
Liquid is water-soluble fluorine carbon resin, phenolic resin and acrylic resin, is used in combination sodium polyphosphate that pH is adjusted to 8.0 carry out normal-temperature hole sealings
Processing, drying.Refer to table 1.
Embodiment 5
Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice using vacuum induction rapid hardening slab stove, roller speed is controlled in 5m/s,
Sheet thickness is 0.2mm；It is broken and carry out Dehydroepiandrosterone derivative that above-mentioned rapid hardening thin slice is subjected to hydrogen explosion；High speed is utilized in airflow milling
Inert gas flow（Argon gas）The quick-fried broken powder of hydrogen is crushed, the micro mist that average particle size is 4 μm is made；By micro mist obtained
Mold is packed into argon inert gas atmosphere, mold is heat safe carbon or carbide, dress powder density ranging from 4g/cm3.
By the mold equipped with micro mist in inert gas（Argon gas）It is placed in 3T pulsed magnetic fields and is orientated under protection, orientation sequence is
It is positive and negative, to which green compact magnet be made；In inert gas（Green compact magnet is placed in vacuum sintering furnace under argon gas protection,
950 DEG C of sintering 5h, then 850 DEG C and 490 DEG C of second annealing processing are carried out, to which high performance sintered magnet product be made.
Sintered magnet product is processed, demand 9.2 × 5.2 × 1mm small dimension magnets are manufactured into.Addition sodium phosphate,
Sodium carbonate or sodium hydroxide carry out conventional degreasing degreasing；It adds salpeter solution and carries out conventional acid pickling and rust removing, washing；Using sealing of hole
Liquid is that water-soluble fluorine carbon resin and water-soluble epoxy resin carry out normal-temperature hole sealing processing, drying.Refer to table 1.
Embodiment 6
Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice using vacuum induction rapid hardening slab stove, roller speed is controlled in 5m/s,
Sheet thickness is 0.2mm；It is broken and carry out Dehydroepiandrosterone derivative that above-mentioned rapid hardening thin slice is subjected to hydrogen explosion；High speed is utilized in airflow milling
Inert gas flow（Nitrogen）The quick-fried broken powder of hydrogen is crushed, the micro mist that average particle size is 4 μm is made；By micro mist obtained
Mold is packed into argon inert gas atmosphere, mold is heat safe carbon or carbide, dress powder density ranging from 4g/cm3.
By the mold equipped with micro mist in inert gas（Nitrogen）It is placed in 3T pulsed magnetic fields and is orientated under protection, orientation sequence is
It is positive and negative, to which green compact magnet be made；In inert gas（Nitrogen）Green compact magnet is placed in vacuum sintering furnace under protection,
950 DEG C of sintering 5h, then 850 DEG C and 490 DEG C of second annealing processing are carried out, to which high performance sintered magnet product be made.
Sintered magnet product is processed, demand 9.2 × 5.2 × 1mm small dimension magnets are manufactured into.Addition sodium phosphate,
Sodium carbonate or sodium hydroxide carry out conventional degreasing degreasing；It adds salpeter solution and carries out conventional acid pickling and rust removing, washing；Using sealing of hole
Liquid is water-soluble fluorine carbon resin, phenolic resin and acrylic resin, is used in combination sodium polyphosphate that pH is adjusted to 8.0 carry out normal-temperature hole sealings
Processing, drying.Refer to table 1.
Embodiment 7
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.It uses pore-sealing liquid for water-soluble epoxy resin, sodium polyphosphate is used in combination that pH is adjusted to 8.0 carry out normal-temperature hole sealings
Processing, drying.Refer to table 1.
Embodiment 8
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.It uses pore-sealing liquid for water soluble phenol resin, sodium polyphosphate is used in combination that pH is adjusted to 8.0 carry out normal-temperature hole sealings
Processing, drying.Refer to table 1.
Embodiment 9
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.It uses pore-sealing liquid for water-soluble fluorine carbon resin+water soluble acrylic resin, is used in combination sodium polyphosphate by pH tune
Normal-temperature hole sealing processing, drying are carried out to 8.0.Refer to table 1.
Embodiment 10
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.It uses pore-sealing liquid for water-soluble fluorine carbon resin+water soluble alkyd resin, sodium polyphosphate is used in combination to be adjusted to pH
8.0 carry out normal-temperature hole sealing processing, drying.Refer to table 1.
Embodiment 11
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.Use pore-sealing liquid for water-soluble fluorine carbon resin+water soluble phenol resin；It is used in combination sodium polyphosphate to be adjusted to pH
8.0 carry out normal-temperature hole sealing processing, drying.Refer to table 1.
Embodiment 12
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.It uses pore-sealing liquid for water soluble acrylic resin+water soluble alkyd resin, is used in combination sodium polyphosphate by pH tune
Normal-temperature hole sealing processing, drying are carried out to 8.0.Refer to table 1.
Embodiment 13
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.It uses pore-sealing liquid for water soluble acrylic resin+water-soluble epoxy resin, is used in combination sodium polyphosphate by pH tune
Normal-temperature hole sealing processing, drying are carried out to 8.0.Refer to table 1.
Embodiment 14
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.It uses pore-sealing liquid for water soluble acrylic resin+water soluble phenol resin, is used in combination sodium polyphosphate by pH tune
Normal-temperature hole sealing processing, drying are carried out to 8.0.Refer to table 1.
Embodiment 15
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.It uses pore-sealing liquid for water soluble alkyd resin+water-soluble epoxy resin, sodium polyphosphate is used in combination to be adjusted to pH
8.0 carry out normal-temperature hole sealing processing, drying.Refer to table 1.
Embodiment 16
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.It uses pore-sealing liquid for water soluble alkyd resin+water soluble phenol resin, sodium polyphosphate is used in combination to be adjusted to pH
8.0 carry out normal-temperature hole sealing processing, drying.Refer to table 1.
Embodiment 17
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.It uses pore-sealing liquid for water-soluble epoxy resin+water soluble phenol resin, sodium polyphosphate is used in combination to be adjusted to pH
8.0 carry out normal-temperature hole sealing processing, drying.Refer to table 1.
Embodiment 18
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.It uses pore-sealing liquid for water-soluble fluorine carbon resin+water soluble acrylic resin+water soluble alkyd resin, is used in combination
PH is adjusted to 8.0 carry out normal-temperature hole sealing processing, drying by sodium polyphosphate.Refer to table 1.
Embodiment 19
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.Use pore-sealing liquid for；Water-soluble fluorine carbon resin+water soluble alkyd resin+water-soluble epoxy resin, is used in combination more
PH is adjusted to 8.0 carry out normal-temperature hole sealing processing, drying by polyphosphate sodium.Refer to table 1.
Embodiment 20
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.It uses pore-sealing liquid for water-soluble fluorine carbon resin+water-soluble epoxy resin+water soluble phenol resin, is used in combination more
PH is adjusted to 8.0 carry out normal-temperature hole sealing processing, drying by polyphosphate sodium.Refer to table 1.
Embodiment 21
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.It uses pore-sealing liquid for water soluble acrylic resin+water soluble alkyd resin+water-soluble epoxy resin, is used in combination
PH is adjusted to 8.0 carry out normal-temperature hole sealing processing, drying by sodium polyphosphate.Refer to table 1.
Embodiment 22
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.Use pore-sealing liquid for water soluble acrylic resin+water soluble alkyd resin+water soluble phenol resin；It is water-soluble
Property alkyd resin+water soluble alkyd resin+water soluble phenol resin, is used in combination sodium polyphosphate that pH is adjusted to 8.0 carry out room temperature envelopes
Hole processing, drying.Refer to table 1.
Embodiment 23
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnets using in the method for embodiment 1, is removed
Oil, rust and washing.It uses pore-sealing liquid for water soluble alkyd resin+water soluble alkyd resin+water soluble phenol resin, is used in combination more
PH is adjusted to 8.0 carry out normal-temperature hole sealing processing, drying by polyphosphate sodium.Refer to table 1.
Comparative example 1
Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice using vacuum induction rapid hardening slab stove, roller speed is controlled in 5m/s,
Sheet thickness is 0.2mm；It is broken and carry out Dehydroepiandrosterone derivative that above-mentioned rapid hardening thin slice is subjected to hydrogen explosion；High speed is utilized in airflow milling
Inert gas flow（Argon gas）The quick-fried broken powder of hydrogen is crushed, the micro mist that average particle size is 4 μm is made；By micro mist obtained
Mold is packed into argon inert gas atmosphere, mold is heat safe carbon or carbide, dress powder density ranging from 4g/cm3；
By the mold equipped with micro mist in inert gas（Argon gas）It is placed in 3T pulsed magnetic fields and is orientated under protection, orientation sequence is
It is positive and negative, to which green compact magnet be made；In inert gas（Argon gas）Green compact magnet is placed in vacuum sintering furnace under protection, 950
DEG C sintering 5h, then carry out 850 DEG C and 490 DEG C of second annealings are handled, to obtained high performance sintered magnet.Product is added
Work is manufactured into demand 9.2 × 5.2 × 1mm small dimension magnets.Using（CN200610172643）Method carries out sealing of hole, drying.Please
Referring to table 1.
Comparative example 2
Product 9.2 × 5.2 × 1mm small dimension permanent magnets after 1 sealing of hole of comparative example.According to（CN200610172643）
Carry out phosphatization, drying.Refer to table 1.
Comparative example 3
Nd-Fe-B permanent magnet will be prepared into 9.2 × 5.2 × 1mm small dimension magnets in comparative example 1.Product sealing of hole side
Method such as patent（CN03134079）High-temperature baking oil removing, boiling water sealing hole drying.Refer to table 1.
Comparative example 4
Nd-Fe-B permanent magnet will be prepared into 9.2 × 5.2 × 1mm small dimension magnets in comparative example 3.Product sealing of hole side
Method such as patent（CN03134079）High-temperature baking oil removing, boiling water sealing hole, according to（CN200610172643）Phosphatization is carried out, is passivated,
Drying.Refer to table 1.
Comparative example 5
Nd-Fe-B permanent magnet will be prepared into 9.2 × 5.2 × 1mm small dimension magnets in comparative example 1.Product sealing of hole side
Method such as Shenyang Zhong Bei Tong Ci Science and Technology Co., Ltd. applies for a patent（CN 201210040318.3）200 DEG C of bakings of high temperature, are put into
Sealing of hole in hole sealing agent, drying.Refer to table 1.
Comparative example 6
Nd-Fe-B permanent magnet will be prepared into 9.2 × 5.2 × 1mm small dimension magnets in comparative example 1.Product sealing of hole side
Method such as Shenyang Zhong Bei Tong Ci Science and Technology Co., Ltd. applies for a patent（CN 201210040318.3）200 DEG C of bakings of high temperature, are put into
Sealing of hole in hole sealing agent, chamfering, electronickelling cupro-nickel protective layer.Refer to table 1.
Comparative example 7
Nd-Fe-B permanent magnet will be prepared into 9.2 × 5.2 × 1mm small dimension magnets in comparative example 1.
Table 1
| Embodiment | High temperature demagnetizing factor | 24 hours PCT demagnetizing factors |
| Embodiment 1 | 0.02 | 2.03 |
| Embodiment 2 | 0.03 | 2.02 |
| Embodiment 3 | 0.01 | 1.21 |
| Embodiment 4 | 0.02 | 2.12 |
| Embodiment 5 | 0.03 | 2.33 |
| Embodiment 6 | 0.02 | 1.02 |
| Embodiment 7 | 0.02 | 1.03 |
| Embodiment 8 | 0.01 | 2.02 |
| Embodiment 9 | 0.01 | 1.01 |
| Embodiment 10 | 0.02 | 2.22 |
| Embodiment 11 | 0.03 | 2.33 |
| Embodiment 12 | 0.02 | 1.72 |
| Embodiment 13 | 0.02 | 2.23 |
| Embodiment 14 | 0.03 | 2.02 |
| Embodiment 15 | 0.01 | 1.71 |
| Embodiment 16 | 0.02 | 2.42 |
| Embodiment 17 | 0.03 | 2.33 |
| Embodiment 18 | 0.02 | 1.12 |
| Embodiment 19 | 0.02 | 2.03 |
| Embodiment 20 | 0.03 | 2.02 |
| Embodiment 21 | 0.01 | 1.21 |
| Embodiment 22 | 0.02 | 2.42 |
| Embodiment 23 | 0.03 | 2.43 |
| Comparative example 1 | 0.02 | 15 |
| Comparative example 2 | 3.2 | 11.4 |
| Comparative example 3 | 0.5 | 16.5 |
| Comparative example 4 | 3.5 | 12.2 |
| Comparative example 5 | 0.2 | 14 |
| Comparative example 6 | 6.3 | 6.3 |
| Comparative example 7 | 0 | 24 surfaces are become rusty full of point, surface corrosion |
Wherein, 120 DEG C of PCT high temperature and pressure tests experimental condition temperature, 2 atmospheric pressure, relative humidity 100%, high temperature demagnetizing factor
=[（Room temperature magnetic flux）-（Magnet high temperature returns to the magnetic flux of room temperature afterwards for a period of time））/（Magnet room temperature magnetic flux）*100%）].
As can be seen from Table 1, hole sealing technology using the present invention ensure that the high temperature of Nd-Fe-B permanent magnet subtracts magnetic property simultaneously
And also assure magnet in 24 hours PCT（120 DEG C of 2 atmospheric pressure, relative humidity 100%）Under conditions of, it ensure that magnet is not easy
Corrosion.And other sealing of holes and process for treating surface is used not only to subtract magnetic to magnet high temperature and have significant effect, and high pressure is tried
After testing PCT accelerated tests, product high temperature demagnetizing factor is very poor, and this method performance is splendid.
It should be noted that invention content and specific implementation mode disclosed in this specification is intended to prove institute of the present invention
The practical application of technical solution is provided, this field skilled practitioner is in spirit and principles of the present invention, when can make various repair
Change, replace on an equal basis.Protection scope of the present invention is subject to the appended claims.
Claims (2)
1. a kind of manufacturing method of corrosion resistance Sintered NdFeB permanent magnet, the manufacturing method include the following steps：
1) Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice using vacuum induction rapid hardening slab stove, roller speed is controlled in 1~5m/s,
Sheet thickness is 0.1~0.3mm；
2) the rapid hardening thin slice in step 1) carries out to hydrogen explosion is broken and Dehydroepiandrosterone derivative；
3) using high-speed flow inert gas that the powder after the hydrogen explosion in step 2) is broken and Dehydroepiandrosterone derivative is broken in airflow milling
It is broken, the micro mist that average particle size is 1~5 μm is made；
4) micro mist obtained in step 3) being packed into mold in atmosphere of inert gases, mold is heat safe carbon or carbide,
Fill powder density ranging from 2~4g/cm3；
5) mold that micro mist is housed in step 4) is placed under inert gas protection in 1~3T pulsed magnetic fields and is orientated, is orientated suitable
Sequence is positive and negative, to which green compact magnet be made；
6) green compact magnet in step 4) is placed in vacuum sintering furnace under inert gas protection, at 900~1150 DEG C be sintered 2~
6h, then 800~950 DEG C and 400~600 DEG C of second annealing processing are carried out, to which high performance sintered magnet product be made；And
7) the sintered magnet product is processed, the small dimension sintered magnet product of demand is manufactured into, to the small dimension
Sintered magnet product carries out sealing pores；The sealing pores include the following steps：
(1) degreasing degreasing：Sodium phosphate, sodium carbonate or sodium hydroxide is added and carries out conventional degreasing degreasing；
(2) acid pickling and rust removing：It adds salpeter solution and carries out conventional acid pickling and rust removing, washing；
(3) pore-sealing liquid is used to carry out normal-temperature hole sealing processing；The pore-sealing liquid is selected from water-soluble fluorine carbon resin, water-soluble acrylic tree
At least one of fat, water soluble alkyd resin, water-soluble epoxy resin, water soluble phenol resin；And
(4) dry；
When carrying out normal-temperature hole sealing processing using pore-sealing liquid, the pH of the pore-sealing liquid is adjusted with sodium polyphosphate and arrives=8.0.
2. manufacturing method according to claim 1, wherein the inert gas is argon gas or nitrogen.
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| CN111020659A (en) * | 2019-12-07 | 2020-04-17 | 爱科科技有限公司 | Method for reducing porosity of coating on surface of neodymium iron boron permanent magnet material |
| CN115985612A (en) * | 2022-12-20 | 2023-04-18 | 东莞金坤新材料股份有限公司 | Formula and preparation method of water-erosion-resistant powerful magnet |
| CN116230347A (en) * | 2023-03-01 | 2023-06-06 | 东莞金坤新材料股份有限公司 | Formula of flexible neodymium-iron-boron magnetic material and manufacturing method thereof |
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| JP3075281U (en) * | 2000-07-31 | 2001-02-16 | 沖マイクロ技研株式会社 | High corrosion resistance Nd-Fe-B magnet |
| JP2004064895A (en) * | 2002-07-29 | 2004-02-26 | Seiko Epson Corp | Manufacturing method for permanent magnet, permanent magnet, motor component and motor |
| CN100498987C (en) * | 2006-10-28 | 2009-06-10 | 山西师鸣精细化工有限公司 | Method for bonderizing sintered neodymium ferroboron magnetic material |
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