CN103993302B - A kind of preparation method of the sintered Nd-Fe-B permanent magnetic material of highly corrosion resistant - Google Patents
A kind of preparation method of the sintered Nd-Fe-B permanent magnetic material of highly corrosion resistant Download PDFInfo
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- CN103993302B CN103993302B CN201410228750.4A CN201410228750A CN103993302B CN 103993302 B CN103993302 B CN 103993302B CN 201410228750 A CN201410228750 A CN 201410228750A CN 103993302 B CN103993302 B CN 103993302B
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Abstract
The preparation method that the invention discloses the sintered Nd-Fe-B permanent magnetic material of a kind of high-corrosion resistance.It adopts and is placed in degreasing fluid and carries out surface degreasing by the sintered NdFeB blank after machining；Again the product after oil removing is put into and sandblasting machine carries out blasting craft, then the product after above-mentioned sandblasting is inserted ultrasonic cleaning in pure water, again the product after ultrasonic cleaning is carried out phosphating process, then product good for above-mentioned phosphatization is solidified through ultrasonic cleaning post-drying, it is positioned on hanger by magnet to carry out the coating of Teflon coating, finally will be coated with the product baking and curing of Teflon coating.The sintered Nd-Fe-B magnetic material decay resistance through surface prepared by the processing method of the present invention with phosphatization/Teflon composite coating is higher, salt spray resistance ability is especially prominent, and relative to other organic coating, its heat resistance and anti-wear performance also have part to improve.
Description
Technical field
The present invention relates to field of magnetic material, the preparation method being specifically related to the sintered Nd-Fe-B permanent magnetic material of a kind of corrosion resistance.
Background technology
Nd-Fe-B permanent magnet, since coming out, has just quickly entered industrialized society with excellent performance and price when rich in natural resources deposit, has been applied to the high-tech areas such as electronics, communication, medical treatment, aviation, environmental protection especially widely.China's Nd-Fe-B yield accounts for more than the 65% of the whole world, and its range of application following and the market demand will continuous enlargement.Under the support energetically of country, through vicennial development, China's Nd-Fe-B product tentatively completes from low and middle-end to middle and high end transition.As a kind of porous permanent magnet material being prepared from by powder metallurgical technique, rich neodymium phase, neodymium iron boron principal phase in Nd-Fe-B permanent magnet material are readily formed intercrystalline corrosion mutually with border.Owing to the character of the rear earth element nd in neodymium iron boron powder metallurgy is active, thus make the corrosion resisting property of whole Nd Fe B alloys become very poor, particularly very easily corrosion in damp and hot environment, and because corrosion failure causes decline or the damage of magnetic property, have a strong impact on the service life of Nd-Fe-B permanent magnet material, reduce stability and the reliability of product.The magnetic property of Nd-Fe-B permanent magnet material and its organizational structure have very big relation.The principal phase of Nd-Fe-B permanent magnet material is the main source of its magnetic property, and coercivity contribution is maximum be rich neodymium phase.After Nd-Fe-B permanent magnet material corrodes, will there is huge change in its magnetic property.Therefore, the research of Nd-Fe-B permanent magnetic material surface protective treatment is the one of the main reasons always restricting industry development with new technology spread work.
The industrial means of defence to Nd-Fe-B permanent magnet material mainly has two kinds: one to be add the alloying elements such as Al, Co, Cu, Ga to improve the decay resistance of material matrix at present, and two is adopt the effective protective coatings such as metal coating, organic coating, composite coating.The decay resistance improving sintered nd-fe-b magnet by adding alloying element has been achieved with very big effect, but this method is usually with the magnetic property sacrificing magnet for cost；And, in salt mist environment, magnet surface can produce red rust, improves the decay resistance of magnet in this case only by protective coating.
The organic coating that current sintered Nd-Fe-B industry surface treatment is commonly used is mainly ability cathode electrophoresis epoxy coating.But owing to the wearability of epoxy coating is very poor with heat resistance, in the applied environment that some are special, the corrosion resistance of epoxy coating is extremely difficult to the requirement under this special environment to magnet decay resistance.Therefore, the Main way that a kind of new organic coating being suitable for special environment is current sintered NdFeB industry surface treatment is developed.Teflon material is that a kind of fluorine that employs replaces the synthetic macromolecular material of all hydrogen atoms in polyethylene.This material has the feature of antiacid alkali resistant, anti-various organic solvents, is practically insoluble in all of solvent.Meanwhile, politef has resistant to elevated temperatures feature, and its coefficient of friction is extremely low, and therefore, its anti-wear performance is also significantly high.
Summary of the invention
The preparation method that it is an object of the invention to provide the sintered Nd-Fe-B permanent magnetic material of a kind of high-corrosion resistance.
In order to realize foregoing invention purpose, the technical solution adopted in the present invention is as follows:
The preparation method of a kind of high-corrosion resistance sintered Nd-Fe-B permanent magnetic material, comprises the steps:
(1) sintered NdFeB blank is dipped in degreasing fluid and carries out 3-10min surface degreasing；
(2) being put into by the product after oil removing and carry out sandblasting in sandblasting machine, select the bead of 120-200 order as sand-blast material, pressure is 0.2-0.8MPa, and the time is 10-40min；
(3) product after above-mentioned sandblasting is inserted ultrasonic cleaning 1-5min in pure water；
(4) being placed in Phosphating Solution by the product after ultrasonic cleaning and carry out bonderizing, phosphating time is 10-30min；
(5) product good for above-mentioned phosphatization is solidified through the ultrasonic cleaning post-drying of 3-5min, be positioned on hanger by magnet to carry out the coating of Teflon coating, finally will be coated with the product baking and curing of Teflon coating.
Consisting of of step (1) described degreasing fluid: sodium hydroxide (NaOH) 5-10g/L, sodium carbonate (NaCO3) 15-30g/L, tertiary sodium phosphate (Na3PO3) 20-40g/L, OP emulsifying agent 1-3g/L, solvent is water.
Sintered NdFeB blank of the present invention is the blank obtained through broken-mixed powder-die mould-sintering of common process such as slab-hydrogen, and it is also commercially available, such as trades mark such as N33-N45.
Consisting of of step (4) described Phosphating Solution: phosphoric acid the second light industry bureau ferromanganese salt ([xFe (H2P04)2·yMn(H2P04)2]) 30-40g/L, zinc dihydrogen phosphate (Zn (H2P02)2·2H20) 25-60g/L, zinc nitrate (Zn (NO3)2) 50-80g/L, sodium chloride (NaCl) 3-5g/L, zinc oxide (ZnO) 3-5g/L, solvent is water.
Step (5) adopts the processing method of dispersion coating to carry out the coating of Teflon coating, expulsion pressure 2.5-5Mpa during spraying, spray base 25-40cm, continuous spray.
The sintered Nd-Fe-B magnetic material decay resistance through surface prepared by the processing method of the present invention with phosphatization/Teflon composite coating is higher, salt spray resistance ability is especially prominent, and relative to other organic coating, its heat resistance and anti-wear performance also have part to improve.
Detailed description of the invention
Following embodiment is to further illustrate using as the explaination to the technology of the present invention content for present invention; but the flesh and blood of the present invention is not limited in described in following embodiment, those of ordinary skill in the art and can should know any simple change based on true spirit or replacement all should belong to protection domain of the presently claimed invention.
Embodiment 1
(1) sintered NdFeB blank is placed in degreasing fluid and carries out 10min surface degreasing.Consisting of of degreasing fluid: sodium hydroxide (NaOH) 5g/L, sodium carbonate (NaCO3) 15g/L, tertiary sodium phosphate (Na3PO3) 30g/L, OP emulsifying agent 3g/L, solvent is water.
(2) being put into by the product after oil removing and carry out blasting craft in sandblasting machine, select the bead of 150 orders as sand-blast material, pressure is 0.3MPa, and the time is 40min.
(3) product after above-mentioned sandblasting is inserted ultrasonic cleaning 3min in pure water.
(4) product after ultrasonic cleaning being carried out bonderizing, phosphating time is 15min.Consisting of of described Phosphating Solution: phosphate dihydrogen manganese iron salt ([xFe (H2P04)2·yMn(H2P04)2]) 30g/L, zinc dihydrogen phosphate (Zn (H2P02)2·2H20) 30g/L, zinc nitrate (Zn (NO3)2) 60g/L, sodium chloride (NaCl) 3g/L, zinc oxide (ZnO) 3g/L, solvent is water.
(5) product good for above-mentioned phosphatization is solidified through the ultrasonic cleaning post-drying of 3min, be positioned on hanger by magnet to carry out the coating of Teflon coating.Expulsion pressure 3.5Mpa, spray base 30cm, continuous spray, finally will be coated with the product baking and curing of Teflon coating, drying temperature is 220 DEG C, and the time is 15h.
Product after above-mentioned baking and curing is carried out salt spray test respectively, and PCT tests, and brine soaking experiment and hydrophilic are tested, and it are compared with the sintered NdFeB product through ability cathode electrophoresis epoxy coating, and result is as shown in table 1 below:
After the technological process of embodiment 1, the salt spray resistance experimental ability of the sintered Nd-Fe-B magnetic material that surface has phosphatization/Teflon composite coating has reached more than 400h, PCT experiment reaches 150h, illustrates that the corrosion resistance of the Sintered NdFeB magnet that surface has phosphatization/Teflon composite coating is very strong.
Embodiment 2
Technological process and test parameters that product is passed are identical with embodiment 1, and the technological parameter of change is following 2 points:
(1) in blasting craft, selecting the bead of 180 orders as sand-blast material, pressure is 0.5MPa, and the time is 30min；
(2) in Teflon coating coating processes.Coating constant speed stirrer is stirred 15min, then after standing 45min, is used for spraying.Expulsion pressure 4Mpa, spray base 30cm, continuous spray, finally will be coated with the product baking and curing (drying temperature is 240 DEG C) of Teflon coating, the time is 20h.
Product after having carried out oil removing-sandblasting-phosphatization equally is carried out ability cathode electrophoresis epoxy resin technology flow process, and with the product after phosphatization, with there is the product of phosphatization/epoxy composite coating as a comparison case, using pencil hardness test experiment as the index checking coating wear resistance.Test result is table 2 below such as:
Above-mentioned the results show, the anti-wear performance of the Sintered NdFeB magnet that surface has phosphatization/Teflon composite coating is higher than the anti-wear performance of other coating.
Embodiment 3
Technological process and technological parameter that product is passed are identical with embodiment 1, and the technological parameter of change is following 2 points:
(1) in blasting craft, selecting the bead of 180 orders as sand-blast material, pressure is 0.4MPa, and the time is 40min.
(2) in Teflon coating coating processes, coating constant speed stirrer is stirred 15min, then after standing 40min, be used for spraying.Expulsion pressure 4Mpa, spray base 30cm, continuous spray, finally will be coated with the product baking and curing (drying temperature is 190 DEG C) of Teflon coating, the time is 15h.
Product after above-mentioned baking and curing is carried out salt spray test respectively, and PCT tests, and brine soaking experiment and hydrophilic are tested, and result is as shown in table 3 below:
The above results is compared with embodiment 1, and its corrosion resistance further enhances, and illustrates that, in above-mentioned process implementing process, the optimization of parameter can promote the corrosion resistance of composite coating further.
Embodiment 4
(1) after machining, Sintered NdFeB magnet is placed in degreasing fluid and carries out 5min surface degreasing.Consisting of of described degreasing fluid: sodium hydroxide (NaOH) 5g/L, sodium carbonate (NaCO3) 20g/L, tertiary sodium phosphate (NaPO3) 30g/L, OP emulsifying agent 2g/L, solvent is water.
(2) being put into by the product after oil removing and carry out blasting craft in sandblasting machine, select the bead of 200 orders as sand-blast material, pressure is 0.8MPa, and the time is 20min.
(3) product after above-mentioned sandblasting is inserted ultrasonic cleaning 5min in pure water.
(4) product after ultrasonic cleaning being carried out phosphating process, phosphating time is 20min.Consisting of of described Phosphating Solution: phosphoric acid the second light industry bureau ferromanganese salt ([xFe (H2P04)2·yMn(H2P04)2]) 40g/L, zinc dihydrogen phosphate (Zn (H2P02)2·2H20) 35g/L, zinc nitrate (Zn (NO3)2) 60g/L, sodium chloride (NaCl) 5g/L, zinc oxide (ZnO) 5g/L.
(5) product good for above-mentioned phosphatization is solidified through the ultrasonic cleaning post-drying of 5min, be positioned on hanger by magnet to carry out the coating of Teflon coating.Coating constant speed stirrer is stirred 15min, then after standing 30min, is used for spraying.Expulsion pressure 5Mpa, spray base 40cm, continuous spray, finally will be coated with the product baking and curing (drying temperature is 200 DEG C) of Teflon coating, the time is 25h.
Product after above-mentioned baking and curing is carried out salt spray test respectively, and PCT tests, and brine soaking experiment and hydrophilic are tested, and result is as shown in table 4 below:
Above example shows, after neodymium iron boron magnetic body surface-coated phosphatization/Teflon composite coating, product has a significantly high corrosion resistance, and the anti-wear performance of phosphatization/Teflon composite coating is also significantly high relative to other organic coating.
It should be noted that foregoing invention content and detailed description of the invention are intended to prove the practical application of technical scheme provided by the present invention to should not be construed as limiting the scope of the present invention.Those skilled in the art are in the spirit and principle of the present invention, when doing various amendment, equivalent replacement or improve.Without departing from design or the scope defined not past present claims book of invention, protection scope of the present invention all should be belonged to.Protection scope of the present invention is as the criterion with appended claims.
Claims (2)
1. a preparation method for the sintered Nd-Fe-B permanent magnetic material of highly corrosion resistant, comprises the steps:
(1) sintered NdFeB blank is dipped in degreasing fluid and carries out 3-10min surface degreasing；
(2) being put into by the product after oil removing and carry out sandblasting in sandblasting machine, select the bead of 120-200 order as sand-blast material, pressure is 0.2-0.8MPa, and the time is 10-40min；
(3) product after above-mentioned sandblasting is inserted ultrasonic cleaning 1-5min in pure water；
(4) being placed in Phosphating Solution by the product after ultrasonic cleaning and carry out bonderizing, phosphating time is 10-30min；Consisting of of described Phosphating Solution: phosphate dihydrogen manganese iron salt 30-40g/L, zinc dihydrogen phosphate 25-60g/L, zinc nitrate 50-80g/L, sodium chloride 3-5g/L, zinc oxide 3-5g/L, solvent are water；
(5) product good for above-mentioned phosphatization is solidified through the ultrasonic cleaning post-drying of 3-5min, be positioned on hanger by magnet to carry out the coating of Teflon coating, finally will be coated with the product baking and curing of Teflon coating.
2. the preparation method of the sintered Nd-Fe-B permanent magnetic material of highly corrosion resistant as claimed in claim 1, it is characterized in that, consisting of of step (1) described degreasing fluid: sodium hydroxide 5-10g/L, sodium carbonate 15-30g/L, tertiary sodium phosphate 20-40g/L, OP emulsifying agent 1-3g/L, solvent are water.
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| CN106826115A (en) * | 2017-01-18 | 2017-06-13 | 安徽大地熊新材料股份有限公司 | A kind of welding processing of sintered Nd-Fe-B permanent magnet |
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| CN108505056A (en) * | 2017-07-18 | 2018-09-07 | 万向钱潮股份有限公司 | A kind of highly corrosion resistant surface treatment method |
| CN112768169B (en) * | 2020-12-30 | 2023-01-10 | 包头天和磁材科技股份有限公司 | Preform, method for producing the same, method for producing corrosion-resistant magnet, and use of the same |
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| JPH11307328A (en) * | 1998-04-16 | 1999-11-05 | Sumitomo Special Metals Co Ltd | Corrosion resistant permanent magnet and its manufacture |
| CN102732871A (en) * | 2011-04-15 | 2012-10-17 | 中国科学院金属研究所 | Neodymium iron boron magnet material phosphating treatment and organic coating double layers protection method |
| CN102389871B (en) * | 2011-10-18 | 2013-12-25 | 安泰科技股份有限公司 | Method for forming aluminum coating on surface of neodymium iron boron magnet |
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| CN106826115A (en) * | 2017-01-18 | 2017-06-13 | 安徽大地熊新材料股份有限公司 | A kind of welding processing of sintered Nd-Fe-B permanent magnet |
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