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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- CN103422082A CN103422082A CN2012101519914A CN201210151991A CN103422082A CN 103422082 A CN103422082 A CN 103422082A CN 2012101519914 A CN2012101519914 A CN 2012101519914A CN 201210151991 A CN201210151991 A CN 201210151991A CN 103422082 A CN103422082 A CN 103422082A
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- phosphatization
- neodymium
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- iron
- zinc
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 37
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000000696 magnetic material Substances 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title claims description 14
- 239000007788 liquid Substances 0.000 title abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008139 complexing agent Substances 0.000 claims abstract description 10
- 239000011701 zinc Substances 0.000 claims description 28
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 15
- 229910052725 zinc Inorganic materials 0.000 claims description 15
- 229910021293 PO 4 Inorganic materials 0.000 claims description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 239000012530 fluid Substances 0.000 claims description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 6
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 claims description 6
- 229910000165 zinc phosphate Inorganic materials 0.000 claims description 6
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- PPSSQRUPSRPZON-UHFFFAOYSA-N nitrobenzene;sodium Chemical compound [Na].[O-][N+](=O)C1=CC=CC=C1 PPSSQRUPSRPZON-UHFFFAOYSA-N 0.000 claims description 4
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- -1 Sodium tetrafluoroborate Chemical compound 0.000 claims description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 3
- 239000011609 ammonium molybdate Substances 0.000 claims description 3
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 3
- 229940010552 ammonium molybdate Drugs 0.000 claims description 3
- 229940045641 monobasic sodium phosphate Drugs 0.000 claims description 3
- 150000002815 nickel Chemical class 0.000 claims description 3
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 3
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims description 2
- VGYYSIDKAKXZEE-UHFFFAOYSA-L hydroxylammonium sulfate Chemical compound O[NH3+].O[NH3+].[O-]S([O-])(=O)=O VGYYSIDKAKXZEE-UHFFFAOYSA-L 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 239000011775 sodium fluoride Substances 0.000 claims description 2
- 235000013024 sodium fluoride Nutrition 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 229940001516 sodium nitrate Drugs 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- 229910001495 sodium tetrafluoroborate Inorganic materials 0.000 claims description 2
- 229940095064 tartrate Drugs 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 abstract description 25
- 239000010452 phosphate Substances 0.000 abstract description 24
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 abstract description 24
- 238000012360 testing method Methods 0.000 abstract description 18
- 238000000576 coating method Methods 0.000 abstract description 16
- 239000011248 coating agent Substances 0.000 abstract description 14
- 238000005260 corrosion Methods 0.000 abstract description 14
- 230000007935 neutral effect Effects 0.000 abstract description 14
- 238000001962 electrophoresis Methods 0.000 abstract description 12
- 150000003839 salts Chemical class 0.000 abstract description 9
- 239000007921 spray Substances 0.000 abstract description 8
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000004381 surface treatment Methods 0.000 abstract description 2
- 230000037452 priming Effects 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 26
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 239000003973 paint Substances 0.000 description 13
- 230000007797 corrosion Effects 0.000 description 12
- 229910052742 iron Inorganic materials 0.000 description 7
- 239000012267 brine Substances 0.000 description 6
- 230000003628 erosive effect Effects 0.000 description 6
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 150000001875 compounds Chemical group 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 229910052779 Neodymium Inorganic materials 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000004070 electrodeposition Methods 0.000 description 3
- 238000010422 painting Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 206010023126 Jaundice Diseases 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000004581 coalescence Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910052722 tritium Inorganic materials 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- QUIGENFNPVOWNF-UHFFFAOYSA-N [B].[Fe].[Nd].[Zn] Chemical compound [B].[Fe].[Nd].[Zn] QUIGENFNPVOWNF-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- ZDVYABSQRRRIOJ-UHFFFAOYSA-N boron;iron Chemical compound [Fe]#B ZDVYABSQRRRIOJ-UHFFFAOYSA-N 0.000 description 1
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000006253 efflorescence Methods 0.000 description 1
- 238000001652 electrophoretic deposition Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000007590 electrostatic spraying Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 229910000150 monocalcium phosphate Inorganic materials 0.000 description 1
- 235000019691 monocalcium phosphate Nutrition 0.000 description 1
- 150000002828 nitro derivatives Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000002345 surface coating layer Substances 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Landscapes
- Chemical Treatment Of Metals (AREA)
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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