CN106756952A - The tin molybdate conversion liquid and its application method of a kind of compound nano-zinc sulfide for Mg alloy surface treatment - Google Patents
The tin molybdate conversion liquid and its application method of a kind of compound nano-zinc sulfide for Mg alloy surface treatment Download PDFInfo
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- CN106756952A CN106756952A CN201611216124.9A CN201611216124A CN106756952A CN 106756952 A CN106756952 A CN 106756952A CN 201611216124 A CN201611216124 A CN 201611216124A CN 106756952 A CN106756952 A CN 106756952A
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- Prior art keywords
- zinc sulfide
- stannate
- nano
- alloy surface
- deionized water
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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
- C23C22/40—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
- C23C22/44—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 fluorides or complex fluorides
Abstract
The invention discloses a kind of tin molybdate conversion liquid of the compound nano-zinc sulfide for Mg alloy surface treatment, the conversion fluid is from stannate, sodium molybdate as main film-former, assistant is with auxiliary agents such as sodium pyrophosphate, sodium fluoride, tannic acid, and nano-zinc sulfide is added as anti-corrosive aids, finely dispersed nano-zinc sulfide sol system is obtained as medium using end carboxyl super branched polyether aqueous solution, it is effective to prevent nano material from reuniting in system sedimentation, reach efficient modified effect；Conversion fluid prepared by the present invention has the advantages that film forming speed is fast, the feature of environmental protection is high, it has the advantages that Corrosion Protection is good, surface compatability in the conversion film that Mg alloy surface is formed, also there are unique photoelectric properties simultaneously, the performance of magnesium alloy is further improved.
Description
Technical field
The present invention relates to technical field of magnesium alloy surface treatment, more particularly to a kind of compound for Mg alloy surface treatment
The tin molybdate conversion liquid and its application method of nano-zinc sulfide.
Background technology
Magnesium alloy is the metal material of a kind of lightweight, high intensity, and the product weight of equality strength even can compare plastic cement
Also light, the ability of its load that withstands shocks is bigger than aluminium alloy, at the same magnesium alloy also have good processability, rapid heat dissipation, antidetonation,
The advantages of anti electromagnetic wave, recoverable, is widely used in fields such as Aero-Space, 3C Product, sports equipments, especially closely
3C Product gradually develops to compact direction over year so that high performance magnesium alloy is more favored by manufacturer.
Although magnesium alloy possesses above-mentioned advantage, because magnesium and its alloy activity are high, its oxide-film is loose porous,
Cause that material surface corrosion resistance is poor, environmental suitability is poor, limits the use of magnesium alloy.In order to improve these shortcomings, work
Magnesium alloy is surface-treated frequently with surface protection technique in industry application, wherein chemical conversion treatment be it is most quick, effectively,
A kind of economic processing mode, can not only improve alloy corrosion ability, go back the further protective treatment of alloy surface and lay
Good basis.The conventional chemical pretreatment solution of current magnesium alloy mainly have chromate, permanganate, phosphate, permanganate-
The technique of the solution systems such as phosphate, wherein chromate conversion coating is the most ripe, but Cr VI is carcinogen high, at present
Prohibit the use of, although the treatment fluid of other classes is more environmentally friendly to a certain extent, the conversion film for being formed exists corrosion-resistant
The problems such as poor, film layer of property is also easy to produce crackle, it is difficult to meet engineering demand.In order to improve chemical composition coating presence these lack
Fall into, researchers can significantly improve the microstructure of conversion film by adding nano-particle in conversion fluid, such as《Nanometer is hard
The influence of matter relative chemical conversion film microstructure》The result of study of one text shows a nanometer Al2O3, Nano-meter SiO_22Addition can have
The raising conversion film crystal grain quantity of effect, improves the consistency of conversion film, obtains corrosion resistance higher, but improve nano-powder and exist
Dispersiveness in conversion fluid is still more formidable problem, very high to technological operation requirement, using limited.
The content of the invention
A kind of defect in order to make up prior art of the invention, there is provided compound nanometer vulcanization for Mg alloy surface treatment
The tin molybdate conversion liquid and its application method of zinc, to improve the performance of traditional Molybdate Conversion Film, obtain highly efficient
Magnesium alloy surface protective effect.
The present invention is achieved by the following technical solutions：
A kind of tin molybdate conversion liquid of compound nano-zinc sulfide for Mg alloy surface treatment, the conversion fluid is by following weight
The raw material of part is formulated：Sodium pyrophosphate 5-8, stannate 20-30, sodium molybdate 20-30, sodium fluoride 1-2, tannic acid 1-2, end carboxylic
Base hyperbranched polyether 3-5, nano-zinc sulfide 1-2, appropriate deionized water, appropriate glacial acetic acid.
Described stannate is the one kind in potassium stannate, lithium stannate, calcium stannate, zinc stannate, sodium stannate.
Described conversion fluid is prepared by following steps：
（1）Sodium pyrophosphate is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（2）Stannate is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（3）Sodium molybdate is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（4）Sodium fluoride is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（5）By in the appropriate deionized water of end carboxyl super branched polyethers input, stirring is completely dissolved it, controls solution middle-end carboxylic
The concentration of base hyperbranched polyether is 1-2g/L, is subsequently added nano-zinc sulfide, and sonic oscillation treatment 1-2h obtains nano-zinc sulfide point
Dispersion liquid is standby；
（6）By step（1）To step（5）Deionized water is added to adjust into system stannate after the solution of preparation is well mixed dense
It is 20-30g/L to spend, then is 3.5-4 with glacial acetic acid regulation system pH value, obtains final product described conversion fluid.
A kind of user of the tin molybdate conversion liquid of described compound nano-zinc sulfide for Mg alloy surface treatment
Method, comprises the following steps：
（1）Mg alloy surface is dried naturally after the steps such as oil removing, water rinsing, acid attack, water rinsing, alkali activation, water rinsing
It is standby；
（2）Pretreated magnesium alloy is soaked in the tin molybdate conversion liquid of the compound nano-zinc sulfide that temperature is 80-90 DEG C
Taken out after middle reaction 20-30min, then workpiece is rinsed with water, dried naturally.
From stannate, sodium molybdate as main film-former, assistant is helped the present invention with sodium pyrophosphate, sodium fluoride, tannic acid etc.
Agent, and nano-zinc sulfide is added as anti-corrosive aids, while nano-zinc sulfide first is put into end carboxyl super branched polyethers water
Decentralized processing is carried out in dissolubility, the water-wet side of end carboxyl super branched polyethers can stretch to form 3-D solid structure in aqueous,
Dispersion of the nano-zinc sulfide in system is driven, finely dispersed nano-zinc sulfide sol system is obtained, nanometer is effectively prevented
Material is reunited sedimentation in system, reaches efficient modified effect；Conversion fluid prepared by the present invention has film forming speed fast, environmentally friendly
Property it is high the advantages of, it has the advantages that Corrosion Protection is good, surface compatability in the conversion film that Mg alloy surface is formed, while also
With unique photoelectric properties, the performance of magnesium alloy is further improved.
Specific embodiment
A kind of tin molybdate conversion liquid of compound nano-zinc sulfide for Mg alloy surface treatment, the conversion fluid is by following
The raw material of weight portion is formulated：It is sodium pyrophosphate 5, potassium stannate 20, sodium molybdate 20, sodium fluoride 1, tannic acid 1, end carboxyl super branched
Polyethers 3, nano-zinc sulfide 1, appropriate deionized water, appropriate glacial acetic acid.
The conversion fluid is prepared by following steps：
（1）Sodium pyrophosphate is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（2）Potassium stannate is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（3）Sodium molybdate is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（4）Sodium fluoride is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（5）By in the appropriate deionized water of end carboxyl super branched polyethers input, stirring is completely dissolved it, controls solution middle-end carboxylic
The concentration of base hyperbranched polyether is 1g/L, is subsequently added nano-zinc sulfide, and sonic oscillation treatment 1h obtains nano-zinc sulfide dispersion liquid
It is standby；
（6）By step（1）To step（5）Deionized water is added to adjust into system stannate after the solution of preparation is well mixed dense
It is 20g/L to spend, then is 3.5 with glacial acetic acid regulation system pH value, obtains final product described conversion fluid.
The application method of the conversion fluid is comprised the following steps：
（1）Mg alloy surface is dried naturally after the steps such as oil removing, water rinsing, acid attack, water rinsing, alkali activation, water rinsing
It is standby；
（2）Pretreated magnesium alloy sample is soaked in the tin molybdate conversion liquid of the compound nano-zinc sulfide that temperature is 80 DEG C
Taken out after middle reaction 30min, then workpiece is rinsed with water, dried naturally.
Conversion film to magnesium alloy sample surface carries out performance test, and test result is：
Pattern:Macroscopic view is grey black, and film forming uniform ground, microcosmic result is solid netted result, there is slight crackle, the μ of thickness 5.6
m。
Corrosion resistance：Undressed magnesium alloy substrate and sample are distinguished into salt spray test and damp heat test, it is as a result as follows：
| Project | Salt spray test | Damp heat test |
| Matrix | General corrosion after 8h, produces a large amount of erosions | Surface discolouration, a large amount of bubbles of appearance after 24h |
| Sample | There is corrosion pit in surface after 60h | Surface light discolouration after 205h, a small amount of bubble |
Claims (4)
1. it is a kind of for Mg alloy surface treatment compound nano-zinc sulfide tin molybdate conversion liquid, it is characterised in that this turn
Change liquid to be formulated by the raw material of following weight portion：Sodium pyrophosphate 5-8, stannate 20-30, sodium molybdate 20-30, sodium fluoride 1-2,
Tannic acid 1-2, end carboxyl super branched polyethers 3-5, nano-zinc sulfide 1-2, appropriate deionized water, appropriate glacial acetic acid.
2. the tin molybdate conversion of a kind of compound nano-zinc sulfide for Mg alloy surface treatment as claimed in claim 1
Liquid, it is characterised in that described stannate is the one kind in potassium stannate, lithium stannate, calcium stannate, zinc stannate, sodium stannate.
3. a kind of tin molybdate of compound nano-zinc sulfide for Mg alloy surface treatment as claimed in claim 1 or 2 turns
Change liquid, it is characterised in that described conversion fluid is prepared by following steps：
（1）Sodium pyrophosphate is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（2）Stannate is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（3）Sodium molybdate is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（4）Sodium fluoride is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（5）By in the appropriate deionized water of end carboxyl super branched polyethers input, stirring is completely dissolved it, controls solution middle-end carboxylic
The concentration of base hyperbranched polyether is 1-2g/L, is subsequently added nano-zinc sulfide, and sonic oscillation treatment 1-2h obtains nano-zinc sulfide point
Dispersion liquid is standby；
（6）By step（1）To step（5）Deionized water is added to adjust into system stannate after the solution of preparation is well mixed dense
It is 20-30g/L to spend, then is 3.5-4 with glacial acetic acid regulation system pH value, obtains final product described conversion fluid.
4. a kind of tin molybdate of the compound nano-zinc sulfide for Mg alloy surface treatment as described in claims 1 to 3 turns
Change the application method of liquid, it is characterised in that comprise the following steps：
（1）Mg alloy surface is dried naturally after the steps such as oil removing, water rinsing, acid attack, water rinsing, alkali activation, water rinsing
It is standby；
（2）Pretreated magnesium alloy is soaked in the tin molybdate conversion liquid of the compound nano-zinc sulfide that temperature is 80-90 DEG C
Taken out after middle reaction 20-30min, then workpiece is rinsed with water, dried naturally.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611216124.9A CN106756952A (en) | 2016-12-26 | 2016-12-26 | The tin molybdate conversion liquid and its application method of a kind of compound nano-zinc sulfide for Mg alloy surface treatment |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611216124.9A CN106756952A (en) | 2016-12-26 | 2016-12-26 | The tin molybdate conversion liquid and its application method of a kind of compound nano-zinc sulfide for Mg alloy surface treatment |
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| CN106756952A true CN106756952A (en) | 2017-05-31 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111041538A (en) * | 2019-12-25 | 2020-04-21 | 八龙应用材料科技(海南)有限公司 | Preparation method of non-ferrous alloy anticorrosive coating |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101845628A (en) * | 2009-03-25 | 2010-09-29 | 中国科学院金属研究所 | Method for preparing environment-friendly black film on magnesium alloy surface and film-forming liquid |
| CN104561980A (en) * | 2015-01-06 | 2015-04-29 | 南昌大学 | Surface treatment method for magnesium alloy |
| CN104884671A (en) * | 2012-12-26 | 2015-09-02 | Posco公司 | Surface-processing composition for galvanized steel sheet, surface processing method for galvanized steel sheet, and galvanized steel sheet |
-
2016
- 2016-12-26 CN CN201611216124.9A patent/CN106756952A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101845628A (en) * | 2009-03-25 | 2010-09-29 | 中国科学院金属研究所 | Method for preparing environment-friendly black film on magnesium alloy surface and film-forming liquid |
| CN104884671A (en) * | 2012-12-26 | 2015-09-02 | Posco公司 | Surface-processing composition for galvanized steel sheet, surface processing method for galvanized steel sheet, and galvanized steel sheet |
| CN104561980A (en) * | 2015-01-06 | 2015-04-29 | 南昌大学 | Surface treatment method for magnesium alloy |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111041538A (en) * | 2019-12-25 | 2020-04-21 | 八龙应用材料科技(海南)有限公司 | Preparation method of non-ferrous alloy anticorrosive coating |
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