CN103422082B - Neodymium-iron-boron magnetic material Zinc phosphating solution and its application method - Google Patents
Neodymium-iron-boron magnetic material Zinc phosphating solution and its application method Download PDFInfo
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- CN103422082B CN103422082B CN201210151991.4A CN201210151991A CN103422082B CN 103422082 B CN103422082 B CN 103422082B CN 201210151991 A CN201210151991 A CN 201210151991A CN 103422082 B CN103422082 B CN 103422082B
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Abstract
The present invention relates to field of metal surface treatment, more particularly, to the Zinc phosphating solution of neodymium iron boron, the protection of neodymium iron boron surface anticorrosive and ability cathode electrophoresis bottoming phosphatization are mainly used in, it is characterised in that Zn2+:PO4 3‑:NO3 ‑:F‑:Accelerator（Mass ratio）For（3.5~10.5）：（14~41.3）：（7.3~21.9）：（0.95~2.8）：1, Ni2+ 0.01 ~ 0.2g/L, 0.04 ~ 0.18g/L of organic complexing agent, accelerator 0.2 ~ 1.5g/L, Yu Weishui.Free acidity 3 ~ 8 point of phosphatization working solution, total acidity 22 ~ 32 point, 48 ~ 55 DEG C of phosphatization temperature, phosphating time 6 ~ 15 minutes.Neodymium iron boron is handled using the Phosphating Solution of the present invention, generation is light grey to grey phosphating coat, and 3% neutral brine soak time is more than 3 hours.0 grade of the cross cut test of electrodeposited paint film, neutral salt spray test 500 hours.
Description
Technical field
The present invention relates to field of metal surface treatment, more particularly, to the Zinc phosphating solution of neodymium-iron-boron magnetic material, mainly
Applied to the protection of neodymium-iron-boron magnetic material surface anticorrosive and ability cathode electrophoresis bottoming phosphatization.
Background technology
NdFeB material small volume, lightweight, magnetic are strong, are widely used in the energy, traffic, communication, national defence, machinery, doctor
The fields such as treatment, computer, household electrical appliances.
Usual neodymium iron boron is made up of the rich neodymium and boron-rich phase and base phase Nd2Fe14B phases of thin layer phase, excellent to obtain
Magnetic, this compound structure is necessary.However, exactly this multiphase structure is anti-oxidant to magnet to bring unfavorable.Mutually
The difference for different its electromotive force of phase factor being in contact and form countless micro- " batteries ", thin layer mutually be anode, base mutually be negative electrode.Neodymium and
Iron is easily oxidized again, and the minimum thin layer of volume is accelerated under relatively very big anode current effect to be corroded, this corrosion
Carried out along base phase intergranular.
Neodymium chemism in magnet is strong, is easily oxidized, corrosion resistance is poor, in a humidity environment, and magnet surface forms corruption
Micro cell is lost, corrosion rate is increased, particularly in the presence of tritium isotope, tritium is expanded by rich neodymium intergranular into magnet
It is scattered that magnet the Nomenclature Composition and Structure of Complexes will be made to change, cause magnetic property to decline, quick-fried broken phenomenon finally occur." battery " is acted on and " hydrogen
It is broken " effect be neodymium iron boron corrosion, efflorescence main cause.
In view of the market prospects and critical role of neodymium iron boron, domestic and international manufacturer all regard the surfacecti proteon of neodymium iron boron as magnetic
The important technical links of body production, i.e. its surface must have good overcoat to can be only achieved requirement.
At present, neodymium iron boron surface anticorrosive technology includes plating, organic coating and composite coating etc..
Because the equipment cost of electroplating technology is relatively low, the uniformity and stability of product quality are generally poor, once
Property product yield is low, simultaneously because improvement is ineffective, very big pollution is often caused to environment.The shortcoming of galvanization coating also phase
When obvious：Plate layer porosity big, film is not fine and close, has shape dependence, it is necessary to do chamfered to magnet corner, to deep hole sample
Product can not plating.For some harsher occasions, after coating long-time use, it may appear that cracking, stripping, easy to fall off etc. are asked
Topic, barrier propterty declines.
Higher quality of forming film can be obtained using electrostatic spraying or electrophoretic deposition coating process, be relatively adapted to factory batch
Amount processing.Coating material available for neodymium iron boron surfacecti proteon mainly includes machine and inorganic two major class.Wherein with organic coating
Film layer consistency it is higher, etch-proof ability is stronger, and construction equipment is simple, is with a wide range of applications.In safeguard function
On, coating protecting both can be used alone, and can also be applied in combination with other coated layers.The magnetic such as used for high humidity environment
Body, current industrial circle largely deposits the means such as one or more layers epoxy resin or other organic coatings using electrophoretic painting and is used as it
The additional protection of his coating.
In order to improve the adhesive force of coating and neodymium iron boron, extend the anticorrosion life-span of coating, it is necessary to carry out phosphorus to neodymium iron boron
Change is handled, including ferric solid-acid and Zinc phosphating.
Chinese patent ZL200610172643.X（2006）Disclose a kind of Iron Phosphating Solution Employed For Normal-temperature Phosphatizing：First neodymium iron boron is carried out
Adjusted before sealing pores, phosphatization without surface, be not added with accelerator, total acidity 12-16 points, pH=2.1-2.8, normal temperature 10-15
Minute, make workpiece surface formation phosphating coat；Phosphating liquor of iron series is by nickel salt, phosphoric acid, sodium dihydrogen phosphate, molybdate, fluoride, organic
Acid complex is constituted.But such ferric solid-acid film is not suitable for cathode electro-coating, reason is that ferric solid-acid film is not corrosion-resistant,
It cannot be directly used to the anti-corrosion protection on neodymium iron boron surface.Dissolution rate is high under the conditions of ability cathode electrophoresis, on the one hand causes electrophoretic paint
Electrical conductivity rise, on the one hand deteriorate and the matching of paint film.
Due to the special construction of neodymium-iron-boron magnetic material, the Phosphating Solution for being commonly used for steel is difficult to realize zinc on neodymium iron boron
It is phosphatization.
United States Patent (USP) US6013411, which is disclosed, contains silicate, this degreasing agent in iron boron paint-on technique, its degreasing agent
Viscosity is big, and easy cleaning, bonderite is not made using zinc dihydrogen phosphate, and the zinc phosphating film anti-corrosion property of formation is low, and surface coating layer is adopted
With powder coating methods, its adhesion is poor, coats uneven, and especially corner part is more prominent.
Chinese patent CN1085963A discloses neodymium iron boron surface cathode electrophoretic painting technique, uses ZnCaNi based phosphatization liquids
Carry out phosphatization, Phosphating Solution composition：Zinc dihydrogen phosphate 3-4%, zinc nitrate 3-4%, calcium dihydrogen phosphate 1-2%, nickel nitrate 0.1-
0.2%, water surplus, 60-70 DEG C of phosphatization temperature, time 3-4 minute.Cr is used afterwards6+-Cr3+Mixing passivation is in electrophoretic painting.
Although paint film adhesion and rotproofness are good, harm is all constituted to environment and human body using Cr VI.
Domestic many researchers have carried out the Zinc phosphating of neodymium iron boron and negative electrode electricity in laboratory by making great efforts for many years
Swimming coated test research.
Zhao Fuxing et al.（Zhao Fuxing etc., New Technologies, 1996,1：43-44）The Zinc phosphating of neodymium iron boron is have studied,
The composition of Phosphating Solution is：
Zn2+5.0-6.5g/L, PO4 3-6.7-10.5g/L, NO3 -3.5-5.2g/L, Ni2+0.2g/L, 2- carboxylic 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 points,
Acid compares 20-25:1,35-45 DEG C of temperature, time 3-5min, 2-3 μm of phosphatization thickness.Because Phosphating Solution acid is than too high, cause a large amount of
Sediment, long-term use has a strong impact on phosphorization film quality.
Lv Baolin et al.（Lv Baolin etc., material protection, 2007,40（3）：30-32）It has studied a kind of Zinc phosphating solution, group
Turn into：Oxidation
Zinc 9-11g/L, phosphoric acid (85%) 33-38 ml/L, compound accelerant (mainly containing glycan and organic acid A) 7.2g/L,
Compound additive (mainly containing isopropanol and organic matter B) 15ml/L.Free acidity 4-7 points, total acidity 65-90 points, pH value 2.0-
2.6,30 DEG C of temperature, time 15min.Pointing out to be adjusted using titanium system table can be obtained uniformly densely on Sintered NdFeB magnet surface
Phosphating coat, and with stronger corrosion resistance.The neodymium iron boron handled using the Phosphating Solution, phosphating coat is partially thick, is not suitable for ability cathode electrophoresis
Application, and because the Zn content in Phosphating Solution is high, cause the alkali resistance of phosphating coat poor.
The process and process conditions that this laboratory condition is provided can not meet large batch of manufacturing specification request, because
This realizes the problem of industrialization automated production is exactly very crucial.
The content of the invention
It is an object of the invention to provide a kind of Zinc phosphating solution of neodymium-iron-boron magnetic material and its application method.
According to the Zinc phosphating solution of the neodymium-iron-boron magnetic material of the present invention, it is characterised in that Zn2+:PO4 3-:NO3 -:F-:Promote
Agent（Mass ratio）For（3.5~10.5）：（14~41.3）：（7.3~21.9）：（0.95~2.8）：1, Ni2+ 0.01 ~ 0.2g/L, it is organic
0.04 ~ 0.18g/L of complexing agent, 0.2 ~ 1.5g/L of accelerator, remaining is water.Wherein：Zn2+Zinc oxide, di(2-ethylhexyl)phosphate can be derived from
The one or two of hydrogen zinc, zinc nitrate, PO4 3-Phosphoric acid, zinc dihydrogen phosphate, the one or two of sodium dihydrogen phosphate can be derived from
More than, NO3 -Nitric acid, zinc nitrate, the one or more of sodium nitrate, F can be derived from-Can be from sodium fluoride, fluorination
Potassium, sodium fluoborate, prodan, ammonium fluoride, the one or more of ammonium acid fluoride, Ni2+From nickel nitrate, nickel sulfate
One kind, organic complexing agent can derive from citric acid, tartaric acid, one kind of ethylenediamine tetra-acetic acid, and accelerator derives from sulfuric acid hydroxyl
Amine, m-nitrobenzene sodium sulfonate, sodium molybdate, the one or two of ammonium molybdate.According to the zinc system of the neodymium-iron-boron magnetic material of the present invention
The application method of Phosphating Solution, it is characterised in that free acidity 3 ~ 8 point of phosphatization working solution, total acidity 22 ~ 32 point, phosphatization temperature 48
~ 55 DEG C, phosphating time 6 ~ 15 minutes.Neodymium iron boron is handled using the Phosphating Solution of the present invention, generation is light grey to grey phosphating 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.
Zn2+It is one of main film forming substance.Zn2+Concentration is low, and film forming is very slow, and film is thin and discontinuous, hair is color, corrosion resistance
It is low, or even it is unable to film forming.Zn2+Concentration height can improve film forming speed, and phosphating coat is thickened.But Zn2+It is too high, phosphatization can be caused
Film is coarse, loose, easy dust, and corrosion resistance declines, and Phosphating Solution sediment increases, and wastes medicament.
PO4 3-It is one of main film forming substance.PO4 3-Concentration is low, and film forming is slow, and film is thin and hair is color, and corrosion resistance is low, not even
Can film forming.PO4 3-Concentration height can improve film forming speed, and phosphating coat is thickened.But PO4 3-It is too high, phosphating coat can be caused coarse, thin
Pine, corrosion resistance declines, and Phosphating Solution sediment increases, and wastes medicament.
NO3 -It is oxidant.NO3 -The low phosphating coat of concentration is loose, and phosphating time is long, or even is unable to film forming.NO3 -Concentration is raised,
Phosphating coat even compact.But NO3 -It is too high, phosphating coat can be caused to turn to be yellow, or even only generate passivating film, corrosion-resistant.
F-It is one of main coalescents.There is no F-Or F-Phosphatization can not be completed when low.F-It is too high, cause phosphatization crystallization thick
Greatly, phosphating coat is loose, and corrosion resistance declines.
Ni2+It is one of main coalescents, phosphatization crystallization can be refined, corrosion resistance is improved.
Complexing agent can reduce the generation of phosphating dregs, extend the service life of Phosphating Solution.
Accelerator species and ratio produce material impact to phosphatization.Use the too high accelerator of oxidisability such as chlorate, mistake
Hydrogen oxide etc., can only obtain passivating film, or even the conversion film turned to be yellow.Therefore for neodymium iron boron, it is preferred to use oxidisability compared with
Low accelerator, such as molybdate, m-nitrobenzene sodium sulfonate, when consumption is low, phosphating coat is very thin, when consumption is high, and phosphating coat hair is color
Or turn blue.
Above-mentioned film forming matter, oxidant, auxiliary agent, the preferably suitable ratio of accelerator.The neodymium provided according to the present invention
Iron boron Zinc phosphating solution, in free acidity 3 ~ 8 point, total acidity 22 ~ 32 point, 48 ~ 55 DEG C of phosphatization temperature, phosphating time 6 ~ 15 minutes
Under conditions of, generation is light grey to grey phosphating coat, and 3% neutral brine soak time is more than 3 hours.Paint film after ability cathode electrophoresis
0 grade of cross cut test, neutral salt spray test 500 hours.
Embodiment
It is non-limiting examples of the present invention, the embodiment and implementation result that the present invention is furture elucidated below.
Technological process：
1. the pre- degreasing-ultrasonic degreasing-washing-washing-pickling-ultrasonic wave water washing-ultrasonic wave water of ultrasonic wave
Wash-table tune-phosphatization-washing-pure water wash-dries-finished product
2. the pre- degreasing-ultrasonic degreasing-washing-washing-pickling-ultrasonic wave water washing-ultrasonic wave water of ultrasonic wave
Wash-table tune-phosphatization-washing-pure water washes-ability cathode electrophoresis-solidification-finished product
The salt water immersion test of phosphating coat is pressed《Phosphorization treatment technology condition before iron and steel parts application》（GB/T6807-2001）
Regulation determine.The cross cut test of paint film is pressed《The cross cut test of paint and varnish paint film》（GB/T9286-1998）Regulation
Determine.The corrosion resistant test of coating is pressed《The measure of paint and varnish-resistance to neutral salt spray performance》（GB/T1771-91）Regulation is surveyed
It is fixed.
Degreasing agent uses water base degreasing agent, and table is adjusted and adjusted using colloidal titanium table.
Embodiment 1
Phosphatization formula of liquid：Zn2+:PO4 3-:NO3 -:F-:Accelerator（Mass ratio）For 3.5：17：8：1.1：1, Ni2+ 0.1g/L,
Organic complexing agent 0.09g/L, accelerator 1.5g/L, remaining is water.7 points of the free acidity of phosphatization working solution, 25 points of total acidity, phosphorus
Change 51 DEG C of temperature, phosphating time 10 minutes.Neodymium iron boron is handled using the Phosphating Solution of the present invention, is generated in light grey phosphating coat, 3%
Property the saline sook time be 3 hours.0 grade of the cross cut test of paint film after ability cathode electrophoresis, neutral salt spray test 500 hours.
Embodiment 2
Phosphatization formula of liquid：Zn2+:PO4 3-:NO3 -:F-:Accelerator（Mass ratio）For 8：30：10：0.95：1, Ni2+ 0.2g/L,
Organic complexing agent 0.04g/L, accelerator 1.0g/L, remaining is water.5 points of the free acidity of phosphatization working solution, 26 points of total acidity, phosphorus
Change 48 DEG C of temperature, phosphating time 12 minutes.Neodymium iron boron is handled using the Phosphating Solution of the present invention, is generated in light grey phosphating coat, 3%
Property the saline sook time be 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
Phosphatization formula of liquid：Zn2+:PO4 3-:NO3 -:F-:Accelerator（Mass ratio）For 10：35：19：2.6：1, Ni2+ 0.03g/
L, organic complexing agent 0.16g/L, accelerator 2.0g/L, remaining is water.6 points of the free acidity of phosphatization working solution, 28 points of total acidity,
55 DEG C of phosphatization temperature, phosphating time 10 minutes.Neodymium iron boron is handled using the Phosphating Solution of the present invention, is generated in grey phosphating coat, 3%
Property the saline sook time be 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
Phosphatization formula of liquid：Zn2+:PO4 3-:NO3 -:F-:Accelerator（Mass ratio）For 6：14：9.1：2.2：1, Ni2+ 0.05g/
L, organic complexing agent 0.11g/L, accelerator 0.6g/L, remaining is water.5 points of the free acidity of phosphatization working solution, total acidity 258
Point, 50 DEG C of phosphatization temperature, phosphating time 10 minutes.Neodymium iron boron is handled using the Phosphating Solution of the present invention, grey phosphating coat, 3% is generated
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 (4)
1. neodymium-iron-boron magnetic material Zinc phosphating solution, it is characterised in that Zn2+：PO4 3-：NO3 -：F-：Accelerator mass ratio is (3.5
~10.5)：(14~41.3)：(7.3~21.9)：(0.95~2.8)：1, Ni2+0.01~0.2g/L, organic complexing agent 0.04~
0.18g/L, 0.2~1.5g/L of accelerator, remaining is water；Zn2+From zinc oxide, zinc dihydrogen phosphate, one kind of zinc nitrate or
Two kinds, PO4 3-From phosphoric acid, zinc dihydrogen phosphate, sodium dihydrogen phosphate one or more, NO3 -From nitric acid, nitric acid
The one or more of zinc, sodium nitrate, F-From sodium fluoride, potassium fluoride, sodium fluoborate, prodan, ammonium fluoride, fluorination
The one or more of hydrogen ammonium, Ni2+From one kind of nickel nitrate, nickel sulfate, organic complexing agent derives from citric acid, winestone
Acid, one kind of ethylenediamine tetra-acetic acid, accelerator derive from HAS, m-nitrobenzene sodium sulfonate, sodium molybdate, one kind of ammonium molybdate
Or two kinds.
2. Phosphating Solution according to claim 1, it is characterised in that accelerator from m-nitrobenzene sodium sulfonate, sodium molybdate,
The one or two of ammonium molybdate.
3. the application method of neodymium-iron-boron magnetic material Zinc phosphating solution according to claim 1, it is characterised in that phosphorous chemical industry
Make free acidity 3~8 point of liquid, total acidity 22~32 point, 48~55 DEG C of phosphatization temperature, phosphating time 6~15 minutes.
4. the application method of neodymium-iron-boron magnetic material Zinc phosphating solution according to claim 3, it is characterised in that phosphorous chemical industry
Make free acidity 4~7 point of liquid, total acidity 25~30 point, 49~55 DEG C of phosphatization temperature, phosphating time 8~12 minutes.
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| CN104357824A (en) * | 2014-10-29 | 2015-02-18 | 合肥市华阳工程机械有限公司 | Phosphating solution for aluminum product surface treatment |
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| CN108179409A (en) * | 2017-12-26 | 2018-06-19 | 廊坊京磁精密材料有限公司 | The phosphatization antirust method of neodymium iron boron magnetic body |
| CN107937892A (en) * | 2017-12-26 | 2018-04-20 | 廊坊京磁精密材料有限公司 | The phosphatization antirust method of high-efficiency environment friendly neodymium iron boron magnetic body |
| CN110423998A (en) * | 2019-07-31 | 2019-11-08 | 泰伦特生物工程股份有限公司 | A kind of rare earth permanent-magnetic material protective agent and preparation method thereof |
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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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Inventor after: Yang Bo Inventor after: Wang Ensheng Inventor before: Wang Ensheng |