CN104637664A - Method for manufacturing corrosion-resistant neodymium-iron-boron permanent magnet - Google Patents
Method for manufacturing corrosion-resistant neodymium-iron-boron permanent magnet Download PDFInfo
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Abstract
The invention provides a method for manufacturing a corrosion-resistant neodymium-iron-boron permanent magnet. The method includes the steps that a neodymium-iron-boron permanent magnet is manufactured into a quick hardening sheet through a vacuum induction quick hardening sheet casting furnace, hydrogen explosion smashing is carried out on the quick hardening sheet, dehydrogenation is carried out, powder generated after hydrogen explosion smashing is smashed in an air current mill by means of high-speed inert gas flow, fine powder with the average granularity being 1-5 microns is manufactured, a high-performance neodymium-iron-boron permanent magnet material is obtained through sintering after the fine powder is pressed, the product is machined, a required magnet in a small specification is manufactured, and finally a corrosion-resistant neodymium-iron-boron permanent magnet material is obtained through hole sealing of the permanent magnet. The method can effectively improve corrosion resistance of the neodymium-iron-boron permanent magnet and can prolong the service life of the neodymium-iron-boron permanent magnet.
Description
Technical field
The present invention relates to a kind of production method of Nd-Fe-B permanent magnet, specifically, relate to the preparation method of corrosion resistance Nd-Fe-Bo permanent magnet material.
Background technology
Neodymium iron boron (NdFeB) permanent magnetic material is the rare earth permanent-magnetic material that current magnetic property is the highest, is called as " magnetic king ".Be widely used in the numerous areas such as electroplating device, machinery, medical treatment, automobile, prospect is very wide.But NdFeB magnet also exists the shortcoming of poor corrosion resistance, have a strong impact on the useful life of Nd-Fe-B permanent magnet, reduce stability and the reliability of product.Therefore coating or application must be adopted to it, to solve its Anticorrosion.How to produce a kind of high anti-corrosion, process simple Nd-Fe-Bo permanent magnet material extremely urgent.The anti-corrosion method of current Nd-Fe-Bo permanent magnet material has a lot.Wherein there are electronickelling, electrogalvanizing (CN1421547A, CN1056133A), shooting of multi-layer nickel electroplating (CN102568732), copper facing (CN1514889A), the multiple methods such as phosphatization (CN101022051), electrophoretic paint.Relatively process simply has the method such as phosphatization, passivation.
Neodymium iron boron porous surface, very easily shelter evil people and countenance evil practices, namely sealing of hole carries out Seal treatment to the hole of piece surface, to make the treatment fluid of each procedure thereafter (as degreasing fluid, pickle, plating solution etc.) not infiltrate in hole, thus avoid the internal corrosion of plating rear coating as patent (CN200610172643).Sealing of hole adopts leaching zinc stearate method: zinc stearate is heated to 130 ~ 140 DEG C of fusings, part is flooded about 20min, take out dry 30min at 60 DEG C, or room temperature places more than 2h, makes it solidify.Then chamfering is carried out, the surface treatments such as plating.Another just heat after Nd-Fe-B permanent magnet contact low temperature hole sealing agent rear surface micro pore volume reduce, hole internal pressure reduces hole sealing agent is sucked the effect playing closed magnet hole, to contribute to reducing in electroplating process various acidity, alkaline solution to the erosion of magnet surface.As applied for by Shenyang Zhong Bei Tong Ci Science and Technology Co., Ltd., the surperficial hot dipping method for sealing of (CN201210040318.3) a kind of Nd-Fe-Bo permanent magnet material adopts in methyl oleate, ethyl oleate one or both, when adopting two kinds of mixtures, its ratio is 1: 1 or 1: 2.First, heated in 120 ~ 240 DEG C of temperature by Nd-Fe-B permanent magnet, heating time is 1 ~ 2.5 hour; Then, the Nd-Fe-B permanent magnet after heating be impregnated in the micropore closing surface of Nd-Fe-B permanent magnet in hole sealing agent, take out after permanent magnet surfaces temperature is lower than 40 DEG C.Or adopt and Nd-Fe-Bo permanent magnet material is vacuumized, then immersed in hole sealing agent, by pressure, pore-sealing liquid is sucked, reach the effect of sealing of hole.As by Wuhan material protection the patent (CN200610166528 that applied for; CN200610166529) be its vacuum equipment adopted and not easily realize producing in enormous quantities; and all above-mentioned sealing of holes have such problem once there be overlap, there will be the problem that sealing of hole is not gone up; and directly there is antiseptic property after sealing of hole cannot be realized, need the surface treatment carrying out being correlated with.The present invention adopts method Nd-Fe-B permanent magnet being adopted to normal temperature leaching, carries out rapid curing, achieves the sealing of hole of magnet, and effectively raise magnet antiseptic property.
Summary of the invention
The object of the invention is to the defect overcoming prior art, a kind of corrosion resistance Nd-Fe-Bo permanent magnet material is provided.
According to the manufacture method of corrosion resistance Sintered NdFeB permanent magnet of the present invention, described manufacture method comprises the steps: 1) utilize vacuum induction rapid hardening slab stove that Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice, by roller speed control built in 1 ~ 5m/s, sheet thickness is 0.1 ~ 0.3mm; 2) the rapid hardening thin slice in step 1) is carried out the broken and Dehydroepiandrosterone derivative of hydrogen explosion; 3) in airflow milling, utilize high velocity air inert gas by step 2) in hydrogen explosion broken and powder after Dehydroepiandrosterone derivative broken, make the micro mist that particle mean size is 1 ~ 5 μm; 4) micro mist obtained in step 3) is loaded mould in atmosphere of inert gases, mould is resistant to elevated temperatures carbon or carbide, and dress powder density scope is 2 ~ 4g/cm
3; 5) mould that micro mist is housed in step 4) is placed in 1 ~ 3T pulsed magnetic field orientation under inert gas shielding, orientation order is positive and negative, thus obtained green compact magnet; 6) under inert gas shielding, green compact magnet in step 4) is placed in vacuum sintering furnace, at 900 ~ 1150 DEG C of sintering 2 ~ 6h, then carries out 800 ~ 950 DEG C and 400 ~ 600 DEG C of second annealing process, thus obtained high performance sintered magnet product; And 7) described sintered magnet product is processed, manufacture the small dimension sintered magnet product of demand, sealing pores is carried out to described small dimension sintered magnet product.
Preferably, described inert gas is argon gas or nitrogen.
According to the manufacture method of corrosion resistance Sintered NdFeB permanent magnet of the present invention, described sealing pores comprises the steps: (1) degreasing degreasing: add sodium phosphate, sodium carbonate or NaOH and carry out conventional degreasing degreasing; (2) acid pickling and rust removing: add salpeter solution again and carry out conventional acid pickling and rust removing, washing; (3) pore-sealing liquid is adopted to carry out normal-temperature hole sealing process; And (4) are dry.
Preferably, described pore-sealing liquid is selected from least one in water-soluble fluorine carbon resin, water soluble acrylic resin, water soluble alkyd resin, water-soluble epoxy resin, water soluble phenol resin.Wherein, the ratio of two or more resin can be any ratio, because they can dissolve each other, preferably selects equal proportion.More preferably, adopt pore-sealing liquid carry out normal-temperature hole sealing process time, with sodium polyphosphate the pH of described pore-sealing liquid is adjusted to=8.0.
The manufacture method of corrosion resistance Sintered NdFeB permanent magnet provided by the invention, compared with prior art, the remarkable advantage of manufacture method of the present invention is: 1) sealing pores provided by the present invention can carry out at normal temperatures, and effectively can improve the corrosion resisting property of Nd-Fe-B permanent magnet; 2) pore-sealing liquid composition of the present invention is simple, can improve the useful life of Nd-Fe-B permanent magnet after product, especially in the environment of the high heat of high humidity.
Embodiment
Below with reference to embodiment, the present invention will be further described, and embodiments of the invention are only for illustration of technical scheme of the present invention, and non-limiting the present invention.
Embodiment 1
Utilize vacuum induction rapid hardening slab stove that Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice, by roller speed control built in 5m/s, sheet thickness is 0.3mm; Above-mentioned rapid hardening thin slice is carried out hydrogen explosion broken and carry out Dehydroepiandrosterone derivative; In airflow milling, utilize high velocity inert gas air-flow (argon gas) that the powder after broken for hydrogen explosion is broken, make the micro mist that particle mean size is 5 μm; Obtained micro mist is loaded mould in argon inert gas atmosphere, and mould is resistant to elevated temperatures carbon or carbide, and dress powder density scope is 2g/cm3.
The mould that micro mist is housed is placed in 3T pulsed magnetic field orientation under argon inert gas protection, and orientation order is positive and negative, thus obtained green compact magnet; Under argon inert gas protection, green compact magnet is placed in vacuum sintering furnace, at 900 DEG C of sintering 6h, then carries out 950 DEG C and 600 DEG C of second annealing process, thus obtained high performance sintered magnet product.
Sintered magnet product is processed, manufactures demand 9.2 × 5.2 × 1mm small dimension magnet.Add sodium phosphate, sodium carbonate or NaOH and carry out conventional degreasing degreasing; Add salpeter solution again and carry out conventional acid pickling and rust removing, washing; Pore-sealing liquid is adopted to be that water-soluble fluorine carbon resin carries out normal-temperature hole sealing process, dries up.Refer to table 1.
Embodiment 2
Utilize vacuum induction rapid hardening slab stove that Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice, by roller speed control built in 1/s, sheet thickness is 0.1mm; Above-mentioned rapid hardening thin slice is carried out hydrogen explosion broken and carry out Dehydroepiandrosterone derivative; In airflow milling, utilize high speed nitrogen gas air-flow that the powder after broken for hydrogen explosion is broken, make the micro mist that particle mean size is 1 μm; Obtained micro mist is loaded mould in inert gas (nitrogen) atmosphere, and mould is resistant to elevated temperatures carbon or carbide, and dress powder density scope is 4g/cm3.
The mould that micro mist is housed is placed in 1T pulsed magnetic field orientation under inert gas (nitrogen) protection, and orientation order is positive and negative, thus obtained green compact magnet; Under inert gas (nitrogen) protection, green compact magnet is placed in vacuum sintering furnace, at 1150 DEG C of sintering 2h, then carries out 800 DEG C and 400 DEG C of second annealing process, thus obtained high performance sintered magnet product.
Sintered magnet product is processed, manufactures demand 9.2 × 5.2 × 1mm small dimension magnet.Add sodium phosphate, sodium carbonate or NaOH and carry out conventional degreasing degreasing; Add salpeter solution again and carry out conventional acid pickling and rust removing, washing; Pore-sealing liquid is adopted to carry out normal-temperature hole sealing process, dry up for water soluble acrylic resin.Refer to table 1.
Embodiment 3
Utilize vacuum induction rapid hardening slab stove that Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice, by roller speed control built in 3m/s, sheet thickness is 0.2mm; Above-mentioned rapid hardening thin slice is carried out hydrogen explosion broken and carry out Dehydroepiandrosterone derivative; In airflow milling, utilize high velocity inert gas air-flow (argon gas) that the powder after broken for hydrogen explosion is broken, make the micro mist that particle mean size is 4 μm; Obtained micro mist is loaded mould in inert gas (argon gas) atmosphere, and mould is resistant to elevated temperatures carbon or carbide, and dress powder density scope is 3g/cm3.
The mould that micro mist is housed is placed in 2T pulse magnetic field orientation under inert gas (argon gas) protection, and orientation order is positive and negative, thus obtained green compact magnet; Under inert gas (argon gas) protection, green compact magnet is placed in vacuum sintering furnace, at 1110 DEG C of sintering 4h, then carries out 900 DEG C and 480 DEG C of second annealing process, thus obtained high performance sintered magnet product.
Sintered magnet product is processed, manufactures demand 9.2 × 5.2 × 1mm small dimension magnet.Add sodium phosphate, sodium carbonate or NaOH and carry out conventional degreasing degreasing; Add salpeter solution again and carry out conventional acid pickling and rust removing, washing; Pore-sealing liquid is adopted to be that water soluble alkyd resin carries out normal-temperature hole sealing process, dries up.Refer to table 1.
Embodiment 4
Utilize vacuum induction rapid hardening slab stove that Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice, by roller speed control built in 3m/s, sheet thickness is 0.2mm; Above-mentioned rapid hardening thin slice is carried out hydrogen explosion broken and carry out Dehydroepiandrosterone derivative; In airflow milling, utilize high velocity inert gas air-flow (nitrogen) that the powder after broken for hydrogen explosion is broken, make the micro mist that particle mean size is 3 μm; Obtained micro mist is loaded mould in inert gas (nitrogen) atmosphere, and mould is resistant to elevated temperatures carbon or carbide, and dress powder density scope is 4g/cm3.
The mould that micro mist is housed is placed in 3T pulsed magnetic field orientation under inert gas (nitrogen) protection, and orientation order is positive and negative, thus obtained green compact magnet; Under inert gas (nitrogen) protection, green compact magnet is placed in vacuum sintering furnace, at 1050 DEG C of sintering 4h, then carries out 850 DEG C and 500 DEG C of second annealing process, thus obtained high performance sintered magnet product.
Sintered magnet product is processed, manufactures demand 9.2 × 5.2 × 1mm small dimension magnet.Add sodium phosphate, sodium carbonate or NaOH and carry out conventional degreasing degreasing; Add salpeter solution again and carry out conventional acid pickling and rust removing, washing; Adopt pore-sealing liquid to be water-soluble fluorine carbon resin, phenolic resins and acrylic resin, and with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 5
Utilize vacuum induction rapid hardening slab stove that Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice, by roller speed control built in 5m/s, sheet thickness is 0.2mm; Above-mentioned rapid hardening thin slice is carried out hydrogen explosion broken and carry out Dehydroepiandrosterone derivative; In airflow milling, utilize high velocity inert gas air-flow (argon gas) that the powder after broken for hydrogen explosion is broken, make the micro mist that particle mean size is 4 μm; Obtained micro mist is loaded mould in argon inert gas atmosphere, and mould is resistant to elevated temperatures carbon or carbide, and dress powder density scope is 4g/cm3.
The mould that micro mist is housed is placed in 3T pulsed magnetic field orientation under inert gas (argon gas) protection, and orientation order is positive and negative, thus obtained green compact magnet; (under argon shield, green compact magnet is placed in vacuum sintering furnace at inert gas, at 950 DEG C of sintering 5h, then carries out 850 DEG C and 490 DEG C of second annealing process, thus obtain high performance sintered magnet product.
Sintered magnet product is processed, manufactures demand 9.2 × 5.2 × 1mm small dimension magnet.Add sodium phosphate, sodium carbonate or NaOH and carry out conventional degreasing degreasing; Add salpeter solution again and carry out conventional acid pickling and rust removing, washing; Pore-sealing liquid is adopted to be that water-soluble fluorine carbon resin and water-soluble epoxy resin carry out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 6
Utilize vacuum induction rapid hardening slab stove that Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice, by roller speed control built in 5m/s, sheet thickness is 0.2mm; Above-mentioned rapid hardening thin slice is carried out hydrogen explosion broken and carry out Dehydroepiandrosterone derivative; In airflow milling, utilize high velocity inert gas air-flow (nitrogen) that the powder after broken for hydrogen explosion is broken, make the micro mist that particle mean size is 4 μm; Obtained micro mist is loaded mould in argon inert gas atmosphere, and mould is resistant to elevated temperatures carbon or carbide, and dress powder density scope is 4g/cm3.
The mould that micro mist is housed is placed in 3T pulsed magnetic field orientation under inert gas (nitrogen) protection, and orientation order is positive and negative, thus obtained green compact magnet; Under inert gas (nitrogen) protection, green compact magnet is placed in vacuum sintering furnace, at 950 DEG C of sintering 5h, then carries out 850 DEG C and 490 DEG C of second annealing process, thus obtained high performance sintered magnet product.
Sintered magnet product is processed, manufactures demand 9.2 × 5.2 × 1mm small dimension magnet.Add sodium phosphate, sodium carbonate or NaOH and carry out conventional degreasing degreasing; Add salpeter solution again and carry out conventional acid pickling and rust removing, washing; Adopt pore-sealing liquid to be water-soluble fluorine carbon resin, phenolic resins and acrylic resin, and with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 7
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Employing pore-sealing liquid is water-soluble epoxy resin, and to be adjusted to by pH with sodium polyphosphate and 8.0 to carry out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 8
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Employing pore-sealing liquid is water soluble phenol resin, and to be adjusted to by pH with sodium polyphosphate and 8.0 to carry out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 9
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Adopt pore-sealing liquid to be water-soluble fluorine carbon resin+water soluble acrylic resin, and with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 10
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Adopt pore-sealing liquid to be water-soluble fluorine carbon resin+water soluble alkyd resin, and with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 11
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Pore-sealing liquid is adopted to be water-soluble fluorine carbon resin+water soluble phenol resin; And with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 12
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Adopt pore-sealing liquid to be water soluble acrylic resin+water soluble alkyd resin, and with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 13
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Adopt pore-sealing liquid to be water soluble acrylic resin+water-soluble epoxy resin, and with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 14
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Adopt pore-sealing liquid to be water soluble acrylic resin+water soluble phenol resin, and with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 15
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Adopt pore-sealing liquid to be water soluble alkyd resin+water-soluble epoxy resin, and with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 16
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Adopt pore-sealing liquid to be water soluble alkyd resin+water soluble phenol resin, and with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 17
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Adopt pore-sealing liquid to be water-soluble epoxy resin+water soluble phenol resin, and with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 18
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Adopt pore-sealing liquid to be water-soluble fluorine carbon resin+water soluble acrylic resin+water soluble alkyd resin, and with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 19
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Employing pore-sealing liquid is; Water-soluble fluorine carbon resin+water soluble alkyd resin+water-soluble epoxy resin, and with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 20
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Adopt pore-sealing liquid to be water-soluble fluorine carbon resin+water-soluble epoxy resin+water soluble phenol resin, and with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 21
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Adopt pore-sealing liquid to be water soluble acrylic resin+water soluble alkyd resin+water-soluble epoxy resin, and with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 22
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Pore-sealing liquid is adopted to be water soluble acrylic resin+water soluble alkyd resin+water soluble phenol resin; Water soluble alkyd resin+water soluble alkyd resin+water soluble phenol resin, and with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Embodiment 23
Adopt in the method for embodiment 1 and Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet, carry out oil removing, rust cleaning, washing.Adopt pore-sealing liquid to be water soluble alkyd resin+water soluble alkyd resin+water soluble phenol resin, and with sodium polyphosphate pH is adjusted to and 8.0 carries out normal-temperature hole sealing process, dry up.Refer to table 1.
Comparative example 1
Utilize vacuum induction rapid hardening slab stove that Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice, by roller speed control built in 5m/s, sheet thickness is 0.2mm; Above-mentioned rapid hardening thin slice is carried out hydrogen explosion broken and carry out Dehydroepiandrosterone derivative; In airflow milling, utilize high velocity inert gas air-flow (argon gas) that the powder after broken for hydrogen explosion is broken, make the micro mist that particle mean size is 4 μm; Obtained micro mist is loaded mould in argon inert gas atmosphere, and mould is resistant to elevated temperatures carbon or carbide, and dress powder density scope is 4g/cm3;
The mould that micro mist is housed is placed in 3T pulsed magnetic field orientation under inert gas (argon gas) protection, and orientation order is positive and negative, thus obtained green compact magnet; Under inert gas (argon gas) protection, green compact magnet is placed in vacuum sintering furnace, at 950 DEG C of sintering 5h, then carries out 850 DEG C and 490 DEG C of second annealing process, thus obtained high performance sintered magnet.Product is processed, manufactures demand 9.2 × 5.2 × 1mm small dimension magnet.(CN200610172643) method of employing carries out sealing of hole, dries up.Refer to table 1.
Comparative example 2
Product 9.2 × 5.2 × 1mm small dimension permanent magnet after comparative example 1 sealing of hole.Carry out phosphatization according to (CN200610172643), dry up.Refer to table 1.
Comparative example 3
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet by comparative example 1.Product method for sealing is as the oil removing of patent (CN03134079) high-temperature baking, and boiling water sealing hole dries up.Refer to table 1.
Comparative example 4
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet by comparative example 3.Product method for sealing is as the oil removing of patent (CN03134079) high-temperature baking, and boiling water sealing hole, carries out phosphatization according to (CN200610172643), passivation, dry up.Refer to table 1.
Comparative example 5
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet by comparative example 1.Product method for sealing such as Shenyang Zhong Bei Tong Ci Science and Technology Co., Ltd. applies for a patent the 200 DEG C of bakings of (CN 201210040318.3) high temperature, puts into hole sealing agent sealing of hole, dries up.Refer to table 1.
Comparative example 6
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet by comparative example 1.Product method for sealing such as Shenyang Zhong Bei Tong Ci Science and Technology Co., Ltd. applies for a patent the 200 DEG C of bakings of (CN 201210040318.3) high temperature, puts into hole sealing agent sealing of hole, chamfering, plating ambrose alloy nickel protection layer.Refer to table 1.
Comparative example 7
Nd-Fe-B permanent magnet is prepared into 9.2 × 5.2 × 1mm small dimension magnet by 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 full of a rust, surface corrosion |
Wherein, PCT high temperature and pressure test experimental condition temperature 120 DEG C, 2 atmospheric pressure, relative humidity 100%, high temperature demagnetizing factor=[(normal temperature magnetic flux)-(getting back to the magnetic flux of normal temperature after magnet high temperature a period of time))/(magnet normal temperature magnetic flux) * 100%)].
As can be seen from Table 1, adopt hole sealing technology of the present invention, ensure that the high temperature demagnetize performance of Nd-Fe-B permanent magnet and ensure that magnet was at 24 hours PCT(120 DEG C of 2 atmospheric pressure, relative humidity 100%) condition under, ensure that magnet is not perishable.And adopt other sealing of hole and process for treating surface not only to have great impact to magnet high temperature demagnetize, and after high voltage test PCT accelerated test, product high temperature demagnetizing factor extreme difference, and this method performance is splendid.
It should be noted that, summary of the invention disclosed in this specification and embodiment are intended to the practical application proving technical scheme provided by the present invention, this area skilled practitioner in spirit of the present invention and principle, when doing various amendment, replace on an equal basis.Protection scope of the present invention is as the criterion with appended claims.
Claims (5)
1. a manufacture method for corrosion resistance Sintered NdFeB permanent magnet, described manufacture method comprises the steps:
1) utilize vacuum induction rapid hardening slab stove that Nd-Fe-B permanent magnet is prepared into rapid hardening thin slice, by roller speed control built in 1 ~ 5m/s, sheet thickness is 0.1 ~ 0.3mm;
2) the rapid hardening thin slice in step 1) is carried out the broken and Dehydroepiandrosterone derivative of hydrogen explosion;
3) in airflow milling, utilize high velocity air inert gas by step 2) in hydrogen explosion broken and powder after Dehydroepiandrosterone derivative broken, make the micro mist that particle mean size is 1 ~ 5 μm;
4) micro mist obtained in step 3) is loaded mould in atmosphere of inert gases, mould is resistant to elevated temperatures carbon or carbide, and dress powder density scope is 2 ~ 4g/cm
3;
5) mould that micro mist is housed in step 4) is placed in 1 ~ 3T pulsed magnetic field orientation under inert gas shielding, orientation order is positive and negative, thus obtained green compact magnet;
6) under inert gas shielding, green compact magnet in step 4) is placed in vacuum sintering furnace, at 900 ~ 1150 DEG C of sintering 2 ~ 6h, then carries out 800 ~ 950 DEG C and 400 ~ 600 DEG C of second annealing process, thus obtained high performance sintered magnet product; And
7) described sintered magnet product is processed, manufacture the small dimension sintered magnet product of demand, sealing pores is carried out to described small dimension sintered magnet product.
2. manufacture method according to claim 1, wherein, described inert gas is argon gas or nitrogen.
3. manufacture method according to claim 1, wherein, described sealing pores comprises the steps:
(1) degreasing degreasing: add sodium phosphate, sodium carbonate or NaOH and carry out conventional degreasing degreasing;
(2) acid pickling and rust removing: add salpeter solution again and carry out conventional acid pickling and rust removing, washing;
(3) pore-sealing liquid is adopted to carry out normal-temperature hole sealing process; And
(4) dry.
4. manufacture method according to claim 3, wherein, described pore-sealing liquid is selected from least one in water-soluble fluorine carbon resin, water soluble acrylic resin, water soluble alkyd resin, water-soluble epoxy resin, water soluble phenol resin.
5. manufacture method according to claim 4, wherein, adopt pore-sealing liquid carry out normal-temperature hole sealing process time, with sodium polyphosphate the pH of described pore-sealing liquid is adjusted to=8.0.
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