CN103996525A - Method for preparing anti-corrosion wear-resisting sintered Nd-Fe-B magnets - Google Patents
Method for preparing anti-corrosion wear-resisting sintered Nd-Fe-B magnets Download PDFInfo
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- CN103996525A CN103996525A CN201410227670.7A CN201410227670A CN103996525A CN 103996525 A CN103996525 A CN 103996525A CN 201410227670 A CN201410227670 A CN 201410227670A CN 103996525 A CN103996525 A CN 103996525A
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Abstract
The invention discloses a method for preparing anti-corrosion wear-resisting sintered Nd-Fe-B magnets. The method includes the following steps that first, sintered Nd-Fe-B magnet blanks are placed in an oil removing solution so that oil on the surfaces of the sintered Nd-Fe-B magnet blanks can be removed, and sand blasting and ultrasonic cleaning are performed on the sintered Nd-Fe-B magnet blanks; second, phosphating is performed on the sintered Nd-Fe-B magnet blanks; third, the products subjected to phosphating and bottoming are immersed into an electrophoresis solution to be subjected to cathode electrophoresis; fourth, primary water washing, spraying and secondary water washing are performed sequentially, and dehydration is performed; fifth, softening braking, curing baking and cooling are sequentially performed. Through the method for preparing the novel sintered Nd-Fe-B magnets, a surface cathode electrophoresis epoxy resin/nano-SiO2 composite coating subjected to phosphating and bottoming is prepared. The corrosion resistance and the wear resistance of the composite coating are greatly improved compared with a traditional epoxy resin coating, and the scratch resistance of the coating can also be correspondingly enhanced.
Description
Technical field
The present invention relates to the field of surface treatment of sintered Nd-Fe-B permanent magnetic material, be specifically related to a kind of preparation of antiseptic wearable coat of sintered NdFeB magnet.
Background technology
Sintered NdFeB (Nd-Fe-B) is that (Typical Representative of rare-earth Nd-Fe-B based permanent magnet) permanent magnet is the best permanent magnetic material of current magnetic property, has been widely used in the numerous areas such as motor, automobile, wind power generation.But this class magnet has an obvious shortcoming, i.e. magnet corrosion-resistant, has had a strong impact on the further application of Nd-Fe-Bo permanent magnet material.Current, neodymium iron boron magnetic body anti-corrosion treatment is mainly contained to two kinds of modes: the one, the alloying elements such as interpolation Al, Co, Cu, Ga improve the decay resistance of material matrix, and the 2nd, adopt metal coating, organic coating, composite coatings etc. are protective coating effectively.Wherein on neodymium-iron-boron magnetic material, ability cathode electrophoresis epoxy coating has very strong decay resistance.Epoxy resin (EP) is a kind of thermosetting resin, there is excellent cementability, resistance to wear, mechanical property, electrical insulation capability, chemical stability, resistant of high or low temperature, and low, the easy machine-shaping of shrinkage, preferably stress transmission and the advantage such as with low cost.But after EP solidifies, crosslink density is high, is tridimensional network, has that internal stress is large, matter is crisp, fatigue durability, thermal endurance, poor impact resistance deficiency, and the shortcoming such as peel strength, cracking adaptability to changes are low and humidity resistance is poor, surface can be high in addition.Therefore, enbrittle greatly at the neodymium-iron-boron magnetic material cathode of surface prepared epoxy coating of swimming, poor impact resistance, the easily shortcoming such as scuffing.
For these problems, domestic and international many researchers have carried out large quantity research to the modification of EP, produce four large effects because nano particle has great specific area and high surface activity, it is to make composite material obtain the effective way of new capability that the physics and chemistry activity of utilizing nano material is carried out modification to EP.
Summary of the invention
The invention provides a kind of preparation method of the Sintered NdFeB magnet with anticorrosion antiwear performance.
To achieve these goals, the technical solution adopted in the present invention is:
The preparation method of a kind of anticorrosion antiwear Sintered NdFeB magnet of the present invention, comprises the steps:
(1) Sintered NdFeB magnet blank is placed in to degreasing fluid and carries out surface degreasing, sandblast, ultrasonic cleaning;
(2) product after ultrasonic cleaning is carried out to phosphatization and process rear ultrasonic cleaning, dry up for subsequent use;
(3) the nanometer SiO of handle process drying and dewatering under stirring
2join in the solvent that is dissolved with silane coupler, then hyperthermic treatment in ultrasonic environment, is finally joined in the electrophoresis tank of being furnished with epoxy resin solution and stirs and form electrophoresis solution;
(4) product after phosphatization bottoming is immersed in the described electrophoresis tank of step (3), carries out ability cathode electrophoresis technique; Voltage control is at 45-70V, and electrophoresis time is 3-6min;
(5) by the above-mentioned product process one-level washing-spray-secondary washing process successively carrying out after electrophoresis, then product is immersed in dehydrating agent and is dewatered, then carry out air gun dewatering process;
(6) by softening baking through the neodymium iron boron product of air gun dehydration, be then cured baking, cooling.
Consisting of of described step (1) degreasing fluid: sodium metasilicate 5-8g/L, sodium carbonate 10-15 g/L, tertiary sodium phosphate .12H
2o 15-20 g/L, OP emulsifying agent 1-3 g/L, NaOH 5-10 g/L, solvent is water.
When described step (1) sandblast, select 140-200 object bead as sand-blast material, pressure is 0.2-0.5MPa, and the time is 20-30min.
Described step (2) phosphatization is processed consisting of of Phosphating Solution used: phosphate dihydrogen manganese molysite 15-25 g/L, and zinc dihydrogen phosphate 30-50 g/L, zinc nitrate 40-70 g/L, sodium chloride 2-5 g/L, zinc oxide 2-5 g/L, solvent is water.
In described step (3), ultrasonic treatment time is 2-3h, is warming up to 60-80 DEG C.
Nanometer SiO
2mass fraction in electrophoresis liquid is 2-4%.Wherein nanometer SiO
2and silane coupler is on market and buys, silane coupler can be KH550, KH560 etc.
In described step (4), epoxy resin solution is to carry out proportioning by mill base, white epoxy resin, water according to the ratio of 1:3-5:5.
Described step (5) dehydrating agent is to remove the dehydrating agent that water mark is conventional after electrophoresis, as the MTJ-100 of Mei Tejia Chemical Industry Science Co., Ltd of Shenzhen, MTJ-101, and the S-100 of Hangzhou You Li Chemical Co., Ltd. etc.
The softening baking time of described step (6) is 15-25min, and curing baking time is 15-30min.
The present invention's Sintered NdFeB magnet blank used is the blank obtaining through broken-mixed powder-die mould-sintering of slab-hydrogen, on market, can buy, and the trade mark of producing as Anhui Dai Xiongxin New Material Co., Ltd is the blank of 42M, 45M etc.
The invention provides a kind of antiseptic wearable coat of novel sintered ndfeb magnet, prepared the cathode of surface swimming Epoxy/nano SiO with phosphatization bottoming
2composite coating.The decay resistance of this composite coating and anti-wear performance all improve a lot than traditional epoxy coating, and the scratch resistant performance of coating also obtains corresponding enhancing.
Embodiment
Following embodiment is further illustrating using the explaination as to the technology of the present invention content for content of the present invention; but flesh and blood of the present invention is not limited in described in following embodiment, those of ordinary skill in the art can and should know any simple change or replacement based on connotation of the present invention all should belong to protection range of the presently claimed invention.
embodiment 1
(1) the Sintered NdFeB magnet blank that is 42M by the trade mark is placed in degreasing fluid and carries out surface degreasing, and the oil removing time is 15min; Consisting of of degreasing fluid: sodium metasilicate 6g/L, sodium carbonate 12 g/L, tertiary sodium phosphate 12H
2o 16 g/L, OP emulsifying agent 2 g/L, NaOH 6 g/L, solvent is water.
(2) product after oil removing is put into sand-blasting machine and carry out sandblast, select 150 object beades as sand-blast material, pressure is 0.3MPa, and the time is 20min;
(3) product after sandblast is inserted to ultrasonic cleaning 2min in pure water;
(4) product after ultrasonic cleaning is carried out in Phosphating Solution to phosphatization processing, phosphating time is 15min; Consisting of of Phosphating Solution: phosphate dihydrogen manganese molysite 20 g/L, zinc dihydrogen phosphate 40 g/L, zinc nitrate 50 g/L, sodium chloride 3 g/L, zinc oxide 3 g/L, solvent is water.
(5) product good above-mentioned phosphatization is dried up with hair-dryer after the ultrasonic cleaning of 5min, be then positioned on hanger.Under stirring, handle is through the nanometer SiO of drying and dewatering
2join in the solvent that is dissolved with silane coupler, then process 30min with ultrasonic wave, be warming up to 70 DEG C, again with being joined in electrophoresis tank after ultrasonic wave processing reaction 2h, in electrophoresis tank, is furnished with the epoxy resin solution being made according to 1:4:5 mass ratio by mill base, white epoxy resin, water, ultrasonic agitation 20min.Nanometer SiO
2mass fraction in electrophoresis liquid is 3%.
(6) product after phosphatization bottoming on above-mentioned hanger is immersed in electrophoresis tank, carries out ability cathode electrophoresis technique.Voltage control is between 50V, and according to being subject to, surfacing is long-pending to be regulated; Electrophoresis time is 3min.
(7) by the above-mentioned product process one-level washing-spray-secondary washing process carrying out after electrophoresis, then product is immersed in to about 5s in dehydrating agent, then carries out air gun dewatering process.
(8) the above-mentioned neodymium iron boron product through air gun dehydration is softened to baking process, the time is 20min, is then cured baking process.Time is 20min.From baking oven, take out the said goods cooling after, product is taken off from hanger.
comparative example 2
Adopt the technological process identical with embodiment 1, just omitted the dopen Nano SiO of step 5 in embodiment 1
2link, only on Sintered NdFeB magnet, ability cathode electrophoresis one deck epoxy coating is as a comparison case.
Product prepared by above-described embodiment 1 and comparative example 2 carries out respectively salt mist test and PCT experiment, and result is as shown in the table:
The above results explanation Epoxy/nano SiO
2the decay resistance of composite coating improves with respect to simple epoxy coating.
Product prepared by above-described embodiment 1 and comparative example 2 carries out friction test on MMW-1A type friction wear testing machine, and test temperature is room temperature, pressure 100N, 60 minutes time.After off-test, by the quality of two kinds of products of accurate weighing, calculate the wear rate of test.Apply Epoxy/nano SiO
2the coefficient of friction of composite coating product is 0.29, and quality wearing and tearing are 0.084 gram.Under equal conditions, the coefficient of friction of contrast coating pure epoxy resin coating sample is 0.51, and quality wearing and tearing are 0.28 gram.The Epoxy/nano SiO preparing by the method is described
2the anti-wear performance of composite coating is greatly improved.
Product prepared by above-described embodiment 1 and comparative example 2 carries out pencil hardness test experiment, and result is as follows:
These results suggest that Epoxy/nano SiO
2the adhesion strength of composite coating is compared epoxy coating and is also improved a lot.
Claims (8)
1. a preparation method for anticorrosion antiwear Sintered NdFeB magnet, comprises the steps:
(1) Sintered NdFeB magnet blank is placed in to degreasing fluid and carries out surface degreasing, sandblast, ultrasonic cleaning;
(2) product after ultrasonic cleaning is carried out to phosphatization and process rear ultrasonic cleaning, dry up for subsequent use;
(3) the nanometer SiO of handle process drying and dewatering under stirring
2join in the solvent that is dissolved with silane coupler, then hyperthermic treatment in ultrasonic environment, is finally joined in the electrophoresis tank of being furnished with epoxy resin solution and stirs and form electrophoresis solution;
(4) product after phosphatization bottoming is immersed in the described electrophoresis tank of step (3), carries out ability cathode electrophoresis technique; Voltage control is at 45-70V, and electrophoresis time is 3-6min;
(5) by the above-mentioned product process one-level washing-spray-secondary washing process successively carrying out after electrophoresis, then product is immersed in dehydrating agent and is dewatered, then carry out air gun dewatering process;
(6) by softening baking through the neodymium iron boron product of air gun dehydration, be then cured baking, cooling.
2. the preparation method of anticorrosion antiwear Sintered NdFeB magnet as claimed in claim 1, is characterized in that, the consisting of of step (1) degreasing fluid: sodium metasilicate 5-8g/L, sodium carbonate 10-15 g/L, tertiary sodium phosphate .12H
2o 15-20 g/L, OP emulsifying agent 1-3 g/L, NaOH 5-10 g/L, solvent is water.
3. the preparation method of anticorrosion antiwear Sintered NdFeB magnet as claimed in claim 1, is characterized in that, when step (1) sandblast, select 140-200 object bead as sand-blast material, pressure is 0.2-0.5MPa, and the time is 20-30min.
4. the preparation method of anticorrosion antiwear Sintered NdFeB magnet as claimed in claim 1, it is characterized in that, step (2) phosphatization is processed consisting of of Phosphating Solution used: phosphate dihydrogen manganese molysite 15-25 g/L, zinc dihydrogen phosphate 30-50 g/L, zinc nitrate 40-70 g/L, sodium chloride 2-5 g/L, zinc oxide 2-5 g/L, solvent is water.
5. the preparation method of anticorrosion antiwear Sintered NdFeB magnet as claimed in claim 1, is characterized in that, in step (3), ultrasonic treatment time is 2-3h, is warming up to 60-80 DEG C.
6. the preparation method of anticorrosion antiwear Sintered NdFeB magnet as claimed in claim 1, is characterized in that step (3) nanometer SiO
2mass fraction in electrophoresis liquid is 2-4%.
7. the preparation method of anticorrosion antiwear Sintered NdFeB magnet as claimed in claim 1, is characterized in that, step (4) epoxy resin solution is to carry out proportioning by mill base, white epoxy resin, water according to the mass ratio of 1:3-5:5.
8. the preparation method of anticorrosion antiwear Sintered NdFeB magnet as claimed in claim 1, is characterized in that, the softening baking time of step (6) is 15-25min, and curing baking time is 15-30min.
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| CN105149318A (en) * | 2015-08-06 | 2015-12-16 | 安徽大地熊新材料股份有限公司 | Method for removing nickel-plate layer of nickel-plate neodymium iron boron magnet |
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| WO2016161742A1 (en) * | 2015-04-09 | 2016-10-13 | 中国科学院宁波材料技术与工程研究所 | Method for improving performance of modification layer of material surface and application thereof |
| CN106544715A (en) * | 2016-11-24 | 2017-03-29 | 京磁材料科技股份有限公司 | The method for improving Nd-Fe-B permanent magnet epoxy resin coating performance |
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Application publication date: 20140820 |