CN103422082A - Neodymium-iron-boron magnetic material zinc-series phosphatization liquid and application method thereof - Google Patents
Neodymium-iron-boron magnetic material zinc-series phosphatization liquid and application method thereof Download PDFInfo
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Abstract
The invention relates to the field of metal surface treatment, and especially relates to a neodymium-iron-boron magnetic material zinc-series phosphatization liquid. The phosphatization liquid is mainly used in neodymium-iron-boron surface anti-corrosion protection and cathodic electrophoresis priming and phosphatization. The liquid is characterized in that a mass ratio of Zn<2+>:PO4<3->:NO<3->:F<->:an accelerator is (3.5-10.5):(14-41.3):(7.3-21.9):(0.95-2.8):1, Ni<2+> is 0.01-0.2g/L, an organic complexing agent is 0.04-0.18g/L, the promoter is 0.2-1.5g/L, and balance is water. Free acidity of a phosphatization working liquid is 3-8 points, a total acidity is 22-32 points, a phosphatization temperature is 48-55 DEG C, and a phosphatization time is 6-15min. When the phosphatization liquid is used for treating neodymium-iron-boron, a light grey to grey phosphate coating is produced, and 3% neutral salt water soaking time is above 3h. An electrophoresis coating cut test is 0 grade, and a neutral salt spray test is 500h.
Description
Technical field
The present invention relates to field of metal surface treatment, especially relate to the Zinc phosphating solution of neodymium-iron-boron magnetic material, be mainly used in the protection of neodymium-iron-boron magnetic material surface anticorrosive and ability cathode electrophoresis bottoming phosphatization.
Background technology
The NdFeB material volume is little, lightweight, magnetic is strong, is widely used in the fields such as the energy, traffic, communication, national defence, machinery, medical treatment, computer, household electrical appliances.
Usually neodymium iron boron by the rich neodymium of thin layer phase and boron-rich phase and base phase Nd2Fe14B mutually institute form, for obtaining good magnetic, this compound structure is necessary.Yet, just this multiphase structure to magnet anti-oxidant bring unfavorable.The difference of different its electromotive force of phase factor that contact with each other and form countless micro-" battery ", thin layer is anode mutually, base is negative electrode mutually.Neodymium and iron are very easily oxidized again, thin layer accelerated corrosion under relatively very large anodic current effect that volume is minimum, and this corrosion is carried out along base phase intergranular.
Neodymium chemically reactive in magnet is strong, easily oxidized, solidity to corrosion is poor, under moist environment, magnet surface forms the corrosion microbattery, has increased corrosion speed, particularly in the situation that the existence of tritium isotropic substance, tritium will make the magnet the Nomenclature Composition and Structure of Complexes change by rich neodymium intergranular to diffusion in magnet, cause magnetic property to descend, and quick-fried broken phenomenon finally occur." battery " effect and " hydrogen is broken " effect are the major causes of neodymium iron boron corrosion, efflorescence.
In view of market outlook and the critical role of neodymium iron boron, domestic and international manufacturer's important technical links using the surfacecti proteon of neodymium iron boron as magnet generation all, its surface must have good protective layer and just can reach requirement.
At present, neodymium iron boron surface anticorrosive technology comprises plating, organic coating and compound coating etc.
Because the equipment cost of electroplating technology is relatively low, the consistence of quality product and stability are generally poor, and the disposable products qualification rate is low, simultaneously ineffective owing to administering, and tend to environment is caused to very large pollution.The shortcoming of galvanization coating is also quite obvious: the coating porosity is large, and film is not fine and close, and the shape dependency is arranged, and need to do chamfered to the magnet corner, can't plating to the deep hole sample.Harsher occasions for some, coating is long-time use after, problem, the barrier propterty decline such as there will be cracking, peel off, easily come off.
Adopt electrostatic spraying or electrophoretic deposition coating process can obtain higher quality of forming film, relatively be applicable to factory's batch processing.The coated material that can be used for the neodymium iron boron surfacecti proteon mainly includes machine and inorganic two large classes.Wherein the rete density with organic coating is higher, and etch-proof ability is stronger, and preparation of construction is simple, is with a wide range of applications.On protection function, coating protecting both can be used separately, also can be used in combination with other coated layer.As the magnet used for high humidity environment, industrial community adopts electrophoretic painting to deposit the append protection of the means such as one or more layers epoxy resin or other organic coatings as other coating in a large number at present.
In order to improve the sticking power of coating and neodymium iron boron, extend the protection against corrosion life-span of coating, need to carry out bonderizing to neodymium iron boron, comprise that iron is phosphatization and Zinc phosphating.
Chinese patent ZL200610172643.X(2006) a kind of Iron Phosphating Solution Employed For Normal-temperature Phosphatizing being disclosed: first neodymium iron boron is carried out to the sealing of hole processing, do not carry out surface adjustment before phosphatization, do not add promotor, total acidity 12-16 point, pH=2.1-2.8, normal temperature 10-15 minute, make workpiece surface form phosphatize phosphate coat; Phosphating liquor of iron series is comprised of nickel salt, phosphoric acid, SODIUM PHOSPHATE, MONOBASIC, molybdate, fluorochemical, organic acid complex compound.But such iron is phosphatize phosphate coat is not suitable for cathode electro-coating, reason is that iron is that phosphatize phosphate coat is not corrosion-resistant, can not be directly used in the anti-corrosion protection on neodymium iron boron surface.Under the ability cathode electrophoresis condition, solubility rate is high, causes on the one hand the specific conductivity of electrocoating paint to raise, and worsens on the one hand the matching capacity with paint film.
Due to the special construction of neodymium-iron-boron magnetic material, the common Phosphating Solution for iron and steel is difficult to realize Zinc phosphating on neodymium iron boron.
U.S. Pat 6013411 discloses iron boron paint-on technique, contain silicate in its grease-removing agent, this grease-removing agent viscosity is large, easy cleaning, do not adopt primary zinc phosphate to make phosphorization agent, and the zinc phosphating film corrosion-resistant of formation is low, surface coating layer adopts the powder spraying method, its bonding force is poor, applies inhomogeneously, and especially the position, corner is more outstanding.
Chinese patent CN1085963A discloses neodymium iron boron cathode of surface electrophoresis painting dressing technique, use the ZnCaNi based phosphatization liquid to carry out phosphatization, Phosphating Solution forms: primary zinc phosphate 3-4%, zinc nitrate 3-4%, monocalcium phosphate 1-2%, nickelous nitrate 0.1-0.2%, water surplus, phosphatization temperature 60-70 ℃, time 3-4 minute.Use afterwards Cr
6+-Cr
3+Mix passivation at electrophoretic painting.Although paint film adhesion and rotproofness are good, use sexavalent chrome all to form harm to environment and human body.
Domestic a lot of researchist in laboratory through making great efforts for many years to have carried out Zinc phosphating and the cathodic electrophoretic coating experimental study of neodymium iron boron.
The people such as Zhao Fuxing (Zhao Fuxing etc., New Technologies, 1996,1:43-44) studied the Zinc phosphating of neodymium iron boron, the consisting of of Phosphating Solution:
Zn
2+5.0-6.5g/L, PO
4 3-6.7-10.5g/L, NO
3 -3.5-5.2g/L, Ni
2+0.2g/L, 2-alcohol acid 0.2g/L, nitro-compound 0.5g/L, BH-A compound accelerant 1.0-1.2g/L, free acidity 0.6-1.0 point, total acidity 20-22 point, sour than 20-25:1, temperature 35-45 ℃, time 3-5min, phosphatization thickness 2-3 μ m.Than too high, cause a large amount of sediments due to Phosphating Solution acid, life-time service has a strong impact on phosphorization film quality.
The people such as Lv Baolin (Lv Baolin etc., material protection, 2007,40(3): 30-32) studied a kind of Zinc phosphating solution, consisted of: oxidation
Zinc 9-11g/L, phosphoric acid (85%) 33-38 ml/L, compound accelerant (mainly containing glycan and organic acid A) 7.2g/L, composite additive (mainly containing Virahol and organism B) 15ml/L.Free acidity 4-7 point, total acidity 65-90 point,, pH value 2.0-2.6,30 ℃ of temperature, time 15min.Point out to adopt titanium system table to adjust and can obtain on the Sintered NdFeB magnet surface phosphatize phosphate coat uniformly densely, and there is stronger solidity to corrosion.The neodymium iron boron that uses this Phosphating Solution to process, phosphatize phosphate coat is partially thick, is not suitable for cathode electro-coating, and, because the zinc content in Phosphating Solution is high, causes the alkali resistance of phosphatize phosphate coat poor.
The processing method that this laboratory condition provides and processing condition can not meet large batch of manufacturing specification request, therefore realize that the industrialization automatic production is exactly very crucial problem.
Summary of the invention
The Zinc phosphating solution and the using method thereof that the purpose of this invention is to provide a kind of neodymium-iron-boron magnetic material.
Zinc phosphating solution according to neodymium-iron-boron magnetic material of the present invention, is characterized in that Zn
2+: PO
4 3-: NO
3 -: F
-: promotor (mass ratio) is (3.5 ~ 10.5): (14 ~ 41.3): (7.3 ~ 21.9): (0.95 ~ 2.8): 1, Ni
2+0.01 ~ 0.2g/L, organic complexing agent 0.04 ~ 0.18g/L, promotor 0.2 ~ 1.5g/L, all the other are water.Wherein: Zn
2+Can derive from one or both of zinc oxide, primary zinc phosphate, zinc nitrate, PO
4 3-Can derive from one or more of phosphoric acid, primary zinc phosphate, SODIUM PHOSPHATE, MONOBASIC, NO
3 -Can derive from one or more of nitric acid, zinc nitrate, SODIUMNITRATE, F
-Can derive from one or more of Sodium Fluoride, Potassium monofluoride, Sodium tetrafluoroborate, Sodium Silicofluoride, Neutral ammonium fluoride, ammonium bifluoride, Ni
2+Derive from a kind of of nickelous nitrate, single nickel salt, organic complexing agent can derive from a kind of of citric acid, tartrate, ethylenediamine tetraacetic acid (EDTA), and promotor derives from one or both of oxammonium sulfate, m-nitrobenzene sodium sulfonate, Sodium orthomolybdate, ammonium molybdate.According to the using method of the Zinc phosphating solution of neodymium-iron-boron magnetic material of the present invention, it is characterized in that the free acidity 3 of phosphatization working fluid ~ 8 points, total acidity 22 ~ 32 points, 48 ~ 55 ℃ of phosphatization temperatures, phosphating time 6 ~ 15 minutes.Use Phosphating Solution of the present invention to process neodymium iron boron, generate light gray to the grey phosphatize phosphate coat, 3% neutral brine soak time is more than 3 hours.0 grade of the cross cut test of paint film after ability cathode electrophoresis, neutral salt spray test 500 hours.
Zn
2+It is one of main film forming substance.Zn
2+Concentration is low, and film forming is very slow, and film is thin and discontinuous, a coloured silk, and erosion resistance is low, even can not film forming.Zn
2+Concentration is high can improve film forming speed, and phosphatize phosphate coat thickens.But Zn
2+Too high, can cause coarse, loose, the easy dust of phosphatize phosphate coat, erosion resistance descends, and the Phosphating Solution sediment increases, the waste medicament.
PO
4 3-It is one of main film forming substance.PO
4 3-Concentration is low, and film forming is slow, and film is thin and send out coloured silk, and erosion resistance is low, even can not film forming.PO
4 3-Concentration is high can improve film forming speed, and phosphatize phosphate coat thickens.But PO
4 3-Too high, can cause phosphatize phosphate coat coarse, loose, erosion resistance descends, and the Phosphating Solution sediment increases, the waste medicament.
NO
3 -It is oxygenant.NO
3 -The low phosphatize phosphate coat of concentration is loose, and phosphating time is long, even can not film forming.NO
3 -Concentration raises, the phosphatize phosphate coat even compact.But NO
3 -Too high, can cause the phosphatize phosphate coat jaundice, even only generate passive film, corrosion-resistant.
F
-It is one of main film coalescence aid.There is no F
-Or F
-Can not complete phosphatization when low.F
-Too high, cause the phosphatization crystallization thick, phosphatize phosphate coat is loose, and erosion resistance descends.
Ni
2+Be one of main film coalescence aid, the crystallization of energy refinement phosphatization, improve erosion resistance.
Complexing agent can reduce the generation of phosphating dregs, extends the work-ing life of Phosphating Solution.
Promotor kind and ratio produce material impact to phosphatization.Use the too high promotor of oxidisability as oxymuriate, hydrogen peroxide etc., can only obtain passive film, even the conversion film of jaundice.Therefore for neodymium iron boron, preferably use the promotor that oxidisability is lower, as molybdate, m-nitrobenzene sodium sulfonate etc., when consumption hangs down, phosphatize phosphate coat is very thin, and when consumption is high, phosphatize phosphate coat is sent out coloured silk or turned blue.
The preferably suitable ratio of above-mentioned filmogen, oxygenant, auxiliary agent, promotor.According to neodymium iron boron Zinc phosphating solution provided by the invention, at free acidity 3 ~ 8 points, total acidity 22 ~ 32 points, 48 ~ 55 ℃ of phosphatization temperatures, under the phosphating time condition of 6 ~ 15 minutes, generate light gray to the grey phosphatize phosphate coat, and 3% neutral brine soak time is more than 3 hours.0 grade of the cross cut test of paint film after ability cathode electrophoresis, neutral salt spray test 500 hours.
Embodiment
Be below non-limiting examples of the present invention, further illustrate embodiment of the present invention and implementation result.
Technical process:
1. the pre-degreasing-ultrasonic degreasing of ultrasonic wave-washing-washing-pickling-ultrasonic wave water washing-ultrasonic wave water washing-table tune-phosphatization-washing-pure water is washed-is dried-finished product
2. the pre-degreasing-ultrasonic degreasing of ultrasonic wave-washing-washing-pickling-ultrasonic wave water washing-ultrasonic wave water washing-wash-ability cathode electrophoresis of table tune-phosphatization-washing-pure water-solidifying-finished product
The saline soak test of phosphatize phosphate coat is pressed " phosphorization treatment technology condition before the iron and steel parts application " regulation (GB/T6807-2001) and is measured.The cross cut test of paint film is pressed " cross cut test of paint and varnish paint film " regulation (GB/T9286-1998) and is measured.The corrosion resistant test of coating (GB/T1771-91) is stipulated to measure by " mensuration of paint and varnish-anti-neutral salt spray performance ".
Grease-removing agent is used water base grease-removing agent, and table is adjusted and used the colloidal titanium table to adjust.
Embodiment 1
Phosphating Solution formula: Zn
2+: PO
4 3-: NO
3 -: F
-: promotor (mass ratio) is 3.5:17:8:1.1:1, Ni
2+0.1g/L, organic complexing agent 0.09g/L, promotor 1.5g/L, all the other are water.Free acidity 7 points of phosphatization working fluid, total acidity 25 points, 51 ℃ of phosphatization temperatures, phosphating time 10 minutes.Use Phosphating Solution of the present invention to process neodymium iron boron, generate light grey phosphatize phosphate coat, 3% neutral brine soak time is 3 hours.0 grade of the cross cut test of paint film after ability cathode electrophoresis, neutral salt spray test 500 hours.
Embodiment 2
Phosphating Solution formula: Zn
2+: PO
4 3-: NO
3 -: F
-: promotor (mass ratio) is 8:30:10:0.95:1, Ni
2+0.2g/L, organic complexing agent 0.04g/L, promotor 1.0g/L, all the other are water.Free acidity 5 points of phosphatization working fluid, total acidity 26 points, 48 ℃ of phosphatization temperatures, phosphating time 12 minutes.Use Phosphating Solution of the present invention to process neodymium iron boron, generate light grey phosphatize phosphate coat, 3% neutral brine soak time is 3.5 hours.0 grade of the cross cut test of paint film after ability cathode electrophoresis, neutral salt spray test 560 hours.
Embodiment 3
Phosphating Solution formula: Zn
2+: PO
4 3-: NO
3 -: F
-: promotor (mass ratio) is 10:35:19:2.6:1, Ni
2+0.03g/L, organic complexing agent 0.16g/L, promotor 2.0g/L, all the other are water.Free acidity 6 points of phosphatization working fluid, total acidity 28 points, 55 ℃ of phosphatization temperatures, phosphating time 10 minutes.Use Phosphating Solution of the present invention to process neodymium iron boron, generate the grey phosphatize phosphate coat, 3% neutral brine soak time is 3.5 hours.0 grade of the cross cut test of paint film after ability cathode electrophoresis, neutral salt spray test 560 hours.
Embodiment 4
Phosphating Solution formula: Zn
2+: PO
4 3-: NO
3 -: F
-: promotor (mass ratio) is 6:14:9.1:2.2:1, Ni
2+0.05g/L, organic complexing agent 0.11g/L, promotor 0.6g/L, all the other are water.Free acidity 5 points of phosphatization working fluid, total acidity 258 points, 50 ℃ of phosphatization temperatures, phosphating time 10 minutes.Use Phosphating Solution of the present invention to process neodymium iron boron, generate the grey phosphatize phosphate coat, 3% neutral brine soak time is 3.0 hours.0 grade of the cross cut test of paint film after ability cathode electrophoresis, neutral salt spray test 500 hours.
Claims (5)
1. the neodymium-iron-boron magnetic material Zinc phosphating solution, is characterized in that Zn
2+: PO
4 3-: NO
3 -: F
-: promotor (mass ratio) is (3.5 ~ 10.5): (14 ~ 41.3): (7.3 ~ 21.9): (0.95 ~ 2.8): 1, Ni
2+0.01 ~ 0.2g/L, organic complexing agent 0.04 ~ 0.18g/L, promotor 0.2 ~ 1.5g/L, all the other are water.
2. according to the Phosphating Solution of claim 1, it is characterized in that Zn
2+Can derive from one or both of zinc oxide, primary zinc phosphate, zinc nitrate, PO
4 3-Can derive from one or more of phosphoric acid, primary zinc phosphate, SODIUM PHOSPHATE, MONOBASIC, NO
3 -Can derive from one or more of nitric acid, zinc nitrate, SODIUMNITRATE, F
-Can derive from one or more of Sodium Fluoride, Potassium monofluoride, Sodium tetrafluoroborate, Sodium Silicofluoride, Neutral ammonium fluoride, ammonium bifluoride, Ni
2+Can derive from a kind of of nickelous nitrate, single nickel salt, organic complexing agent can derive from a kind of of citric acid, tartrate, ethylenediamine tetraacetic acid (EDTA), and promotor can derive from one or both of oxammonium sulfate, m-nitrobenzene sodium sulfonate, Sodium orthomolybdate, ammonium molybdate.
3. according to the Phosphating Solution of claim 1 or 2, it is characterized in that promotor derives from one or both of m-nitrobenzene sodium sulfonate, Sodium orthomolybdate, ammonium molybdate.
4. the using method of neodymium-iron-boron magnetic material Zinc phosphating solution, is characterized in that the free acidity 3 of phosphatization working fluid ~ 8 points, total acidity 22 ~ 32 points, 48 ~ 55 ℃ of phosphatization temperatures, phosphating time 6 ~ 15 minutes.
5. according to the Phosphating Solution of claim 1 or 4, it is characterized in that the free acidity 4 of phosphatization working fluid ~ 7 points, total acidity 25 ~ 30 points, 49 ~ 55 ℃ of phosphatization temperatures, phosphating time 8 ~ 12 minutes.
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Address after: 100083 No. 20, Haidian District, Beijing, Xueyuan Road Patentee after: Sinochemical science and Technology Research Institute Co., Ltd. Address before: 100083 No. 20, Haidian District, Beijing, Xueyuan Road Patentee before: Central Research Institute of China Chemical Science and Technology |
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