CN1077757A - black phosphating solution and preparation method thereof - Google Patents
black phosphating solution and preparation method thereof Download PDFInfo
- Publication number
- CN1077757A CN1077757A CN 92107510 CN92107510A CN1077757A CN 1077757 A CN1077757 A CN 1077757A CN 92107510 CN92107510 CN 92107510 CN 92107510 A CN92107510 A CN 92107510A CN 1077757 A CN1077757 A CN 1077757A
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- Prior art keywords
- ion
- liquid
- reactor
- aequum
- phosphatization
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
- C23C22/08—Orthophosphates
- C23C22/22—Orthophosphates containing alkaline earth metal cations
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/40—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates
- C23C22/42—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates containing also phosphates
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The present invention aims to provide a kind of melanism decorative effect and the good steel part phosphatization liquid of corrosion stability.It is made up of blackening liquid and phosphatization liquid two portions.Blackening liquid is made up of mn ion, antimony ion, iron ion, phosphate anion, salt acid ion, molybdenum acid ion, tartrate anion ion and water, and its preparation method is that salt and the water that will contain its each ion component add stirring and dissolving in the reactor; Phosphatization liquid belongs to zinc calcium nickel salt phosphatization liquid.With the black phosphating film that the present invention generates, the pitch-black purity of color and luster, resistance to corrosion is extremely strong.The present invention is widely used in fields such as machinery, electronics, weapons, aviation, car and boat, instrument, building materials, household electrical appliances.
Description
The present invention relates to steel part alramenting treatment technology.
Steel part surface method for bonderizing commonly used protects and decorates processing.Chinese patent application number is that 88105272.8 name is called the application for a patent for invention of " phosphatization liquid and preparation method thereof ", provides a kind of by pickle solution and phosphatization liquid phosphatization liquid dimerous.Phosphatization liquid wherein mainly comprises nitrocalcite, zinc phosphate and nickel nitrate solution, also has a small amount of other salt, acid and additive.When this invention technology is used for the steel part phosphatization, the phosphatize phosphate coat gray or the Dark grey that are generated, color and luster is attractive in appearance inadequately, and decorative effect is not so good; Also the someone uses the active sulphur in the sulfide (for example sodium sulphite), generates Iron sulfuret at steel surface, generates the black phosphating film behind bonderizing.For example use the sulfide solution preimpregnation again through bonderizing, generate the phosphatize phosphate coat that contains the black Iron sulfuret.Because the sulfide poor chemical stability makes this kind black phosphating film black even poor, melanism effect and solidity to corrosion are all relatively poor, often are difficult to be put to production application.And will overflow in the production process has irritating hydrogen sulfide, the severe contamination production environment.
The object of the present invention is to provide a kind of black phosphating solution and manufacture method thereof, after this black phosphating solution is handled the steel part workpiece, the black phosphating film melanism good decorating effect of generation, and satisfactory stability and corrosion stability are arranged.
Black phosphating solution among the present invention, be made up of blackening liquid and phosphatization liquid two portions: wherein phosphatization liquid is formed by its weight percent and is contained:
Zine ion 0.5-3.50
Calcium ion 0.25-2.50
Nickel ion 0.15-0.48
Phosphate anion 1.15-3.00
Nitrate ion 1.50-15.00
Citrate ion 0.50-1.00
Borate ion 0.38-0.80
Surplus is a water;
It is characterized in that wherein blackening liquid consists of by its weight percent:
Mn ion 0.05-0.24
Antimony ion 0.08-0.42
Iron ion 0.17-0.34
Phosphate anion 3.00-6.00
Salt acid ion 2.00-5.00
Molybdenum acid ion 0.04-0.15
Tartrate anion ion 0.18-0.58
Surplus is a water.
The preparation method of black phosphating solution among the present invention is to be undertaken by following step:
Blackening liquid:
1), the Manganous chloride tetrahydrate with aequum, antimony chloride, iron(ic) chloride, tartrate add in the reactor one by one, adds a certain amount of water, stir and make it dissolving;
2), the phosphoric acid and the hydrochloric acid of aequum is added in the said reactor, make reactive material accelerate dissolution in the still;
3) Sodium orthomolybdate with aequum places container, after water dissolution, slowly adds in the said reactor;
4), in said reactor, add entry to requirement.
5) it is standby, Generation Liquid in the reactor to be moved to storage tank.
Phosphatization liquid:
1) place reactor fully to react in the zinc oxide of aequum and the phosphoric acid of proportion 1.71, it is standby to move to a storage tank after zinc oxide is dissolved fully;
2) it is standby, place reactor fully to react in the zinc oxide of aequum and the nitric acid of proportion 1.50, to move to second storage tank after zinc oxide is dissolved fully;
3) it is standby, place reactor fully to react in the calcium oxide of aequum and the nitric acid of proportion 1.50, to move to the 3rd storage tank after calcium oxide is dissolved fully;
4) solution in above-mentioned first, second and third storage tank is injected the phosphatization groove;
5), the nickelous nitrate with aequum, boric acid and citric acid inject the phosphatization groove, stirs, and adds entry then to requirement.
6), with free acidity and total acidity that zinc oxide is regulated solution in the phosphatization groove respectively, make free acidity value FA at the 4-6 point, total acidity value TA is at the 45-70 point.
Iron and steel parts is after clean, and with blackening liquid of the present invention under 15-60 ℃ of temperature pre-preg 0.5-5 minute, the phosphatization liquid in the present invention was under 55-95 ℃ of temperature phosphatization 4-15 minute again, can form phosphatize phosphate coat even, careful, corvinus.This black phosphating film melanism good decorating effect has strong sticking power, satisfactory stability and corrosion stability.Can also carry out aftertreatment to this melanism film, for example apply dryness oil film protective agent, further strengthen corrosion stability.
To after the workpiece pre-preg, adopt other phosphatization liquid to carry out bonderizing with blackening liquid among the present invention,, also can reach the black phosphating effect as phosphatization liquid and suitable additive such as zinc system, manganese systems.The major ingredient of blackening liquid among the present invention and the phosphatization liquid among the present invention or other phosphatization liquid can also be closed and be made into one, form black phosphating solution, workpiece directly be inserted wherein carry out the black phosphorus processing, reach the effect of black phosphating.
After the blackening liquid pre-preg of workpiece in the present invention, form continuous, the uniform melanism film of one deck at workpiece surface.This layer melanism film can improve the physical condition of workpiece surface, makes that it has that crystallization nuclei is many, grain refining, active strong and characteristics such as certain catalysis characteristics are arranged.Can quicken phosphating reaction speed, reduce phosphorization treatment time, reduce the rete porosity, improve corrosion resistance.This melanism film be in the blackening liquid plurality of inorganic salt on the steel part surface, act on and form, even film layer, chemical stability be good.
Below provide embodiments of the invention, see Table 1; The performance test results of the black phosphating film that generates sees Table 2.
Claims (2)
1, steel part black phosphating solution, be made up of blackening liquid and phosphatization liquid two portions: wherein phosphatization liquid is formed by its weight percent and is contained:
Zine ion 0.50-3.50
Calcium ion 0.25-2.50
Nickel ion 0.15-0.48
Phosphate anion 1.15-3.00
Nitrate ion 1.50-15.00
Citrate ion 0.50-1.00
Borate ion 0.38-0.80
Surplus is a water;
It is characterized in that wherein blackening liquid consists of by its weight percent:
Mn ion 0.05-0.24
Antimony ion 0.08-0.42
Iron ion 0.17-0.34
Phosphate anion 3.00-6.00
Salt acid ion 2.00-5.00
Molybdenum acid ion 0.04-0.15
Tartrate anion ion 0.18-0.58
Surplus is a water.
2, the preparation method of steel part black phosphating solution is characterized in that being undertaken by following step:
Blackening liquid:
1), the Manganous chloride tetrahydrate with aequum, antimony chloride, iron(ic) chloride, tartrate add in the reactor one by one, adds a certain amount of water, stir and make it dissolving;
2), the phosphoric acid and the hydrochloric acid of aequum is added in the said reactor, make reactive material accelerate dissolution in the still;
3) Sodium orthomolybdate with aequum places container, after water dissolution, slowly adds in the said reactor;
4), in said reactor, add entry to requirement.
5) it is standby, Generation Liquid in the reactor to be moved to storage tank.
Phosphatization liquid:
1) place reactor fully to react in the zinc oxide of aequum and the phosphoric acid of proportion 1.71, it is standby to move to a storage tank after zinc oxide is dissolved fully;
2) it is standby, place reactor fully to react in the zinc oxide of aequum and the nitric acid of proportion 1.50, to move to second storage tank after zinc oxide is dissolved fully;
3) it is standby, place reactor fully to react in the calcium oxide of aequum and the nitric acid of proportion 1.50, to move to the 3rd storage tank after calcium oxide is dissolved fully;
4) solution in above-mentioned first, second and third storage tank is injected the phosphatization groove;
5), the nickelous nitrate with aequum, boric acid and citric acid inject the phosphatization groove, stirs, and adds entry then to requirement.
6), with free acidity and total acidity that zinc oxide is regulated solution in the phosphatization groove respectively, make free acidity value FA at the 4-6 point, total acidity value TA is at the 45-70 point.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92107510 CN1077757A (en) | 1992-04-13 | 1992-04-13 | black phosphating solution and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92107510 CN1077757A (en) | 1992-04-13 | 1992-04-13 | black phosphating solution and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1077757A true CN1077757A (en) | 1993-10-27 |
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ID=4942850
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92107510 Pending CN1077757A (en) | 1992-04-13 | 1992-04-13 | black phosphating solution and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1077757A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003091480A1 (en) * | 2002-04-26 | 2003-11-06 | Liuzhou Construction Machinery Factory General | Corrosion resistant prestressed steel bar and its preparing process |
| CN103469187A (en) * | 2013-08-14 | 2013-12-25 | 南京久道科技有限公司 | Treatment fluid for phosphatizing and blackening steel surface |
| CN104294349A (en) * | 2014-09-23 | 2015-01-21 | 沈阳大学 | Method for coating normal-temperature black phosphating film on steel surface |
| CN113046738A (en) * | 2021-03-11 | 2021-06-29 | 廊坊师范学院 | Preparation method of black phosphating solution for steel surface |
-
1992
- 1992-04-13 CN CN 92107510 patent/CN1077757A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003091480A1 (en) * | 2002-04-26 | 2003-11-06 | Liuzhou Construction Machinery Factory General | Corrosion resistant prestressed steel bar and its preparing process |
| CN103469187A (en) * | 2013-08-14 | 2013-12-25 | 南京久道科技有限公司 | Treatment fluid for phosphatizing and blackening steel surface |
| CN103469187B (en) * | 2013-08-14 | 2015-07-29 | 南京久道科技有限公司 | For the treatment solution of steel surface phosphatization melanism |
| CN104294349A (en) * | 2014-09-23 | 2015-01-21 | 沈阳大学 | Method for coating normal-temperature black phosphating film on steel surface |
| CN113046738A (en) * | 2021-03-11 | 2021-06-29 | 廊坊师范学院 | Preparation method of black phosphating solution for steel surface |
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| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |