CN107142470A - Be conducive to improving the zinc cathode conversion film of corrosion stability of magnesium alloy and the preparation method of epoxy coating - Google Patents
Be conducive to improving the zinc cathode conversion film of corrosion stability of magnesium alloy and the preparation method of epoxy coating Download PDFInfo
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- CN107142470A CN107142470A CN201710190051.9A CN201710190051A CN107142470A CN 107142470 A CN107142470 A CN 107142470A CN 201710190051 A CN201710190051 A CN 201710190051A CN 107142470 A CN107142470 A CN 107142470A
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- Prior art keywords
- magnesium alloy
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- conducive
- zinc
- epoxy resin
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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
- C23C22/82—After-treatment
Abstract
The present invention is to provide it is a kind of be conducive to improve corrosion stability of magnesium alloy zinc cathode conversion film and epoxy coating preparation method.Magnesium alloy component by pretreatment is impregnated in magnesium alloy phosphating solution and carries out conversion processing, the operating temperature of the conversion processing is 40~70 DEG C, the time is 10~70 minutes, it is then immersed in epoxy resin mixed liquor, taken out after standing 2 minutes, hang 24 hours, then be heat-treated 2 hours by 60 DEG C at room temperature.The present invention is not only able in the good Zinc-calcium series phosphatating film of Mg alloy surface formation binding ability, and obtains the composite coating that corrosion resistance, binding ability and wearability are all significantly improved by coating epoxy resin.
Description
Technical field
The present invention relates to a kind of preparation method of magnesium alloy Zinc-calcium series phosphatating-epoxy coating.It is specifically a kind of
The advantage of epoxy resin and chemistry and electrochemistry is combined together to the preparation technology for the face coat for being applied to magnesium alloy.
Background technology
With other metal phase ratios, magnesium alloy has the advantage of uniqueness, is mainly manifested in several aspects：It is lightweight, excellent
Good machining property and good casting character, dimensional stability and fatigue resistance, high-termal conductivity, good electromagnetic screen
Cover ability, extremely low toxicity, regeneration and capability of environmental protection.But, magnesium is a kind of very active metal, its standard electrode potential
For -2.37V, about 2V lower than the standard electrode potential of iron, about 0.7V also lower than aluminium can occur with surrounding environment in use
Electrochemistry or chemical reaction, surface form MgO, Mg (OH)2Loose porous oxide layer, do not have to magnesium alloy substrate substantially
There is any protective capability so that corrosion stability of magnesium alloy and wearability extreme difference, this also constrains the development of magnesium alloy.Therefore, magnesium
Appropriate surface treatment is had to pass through when alloy is used, to improve its anti-corrosion and abrasive resistance.
The conversion film of electrochemistry and chemical preparation is usually present the defects such as substantial amounts of micropore and micro-crack and organic coating
In the absence of these defects, but it is due to the difference of magnesium alloy and organic resin paint chemistries, is directly applied in Mg alloy surface
Cover organic resin to be difficult to form the stronger coating of adhesion, be easy to come off in use.So needing new using some
Method with both comprehensive advantage.
One kind is disclosed in Publication No. CN101671824A patent document《Magnesium alloy surface zinc-calcium series phosphating solution and
Its conversion treatment process》, the phosphating solution disclosed in it contains 10~30 grams of disodium hydrogen phosphate, nitric acid in every liter of solution
4~6 grams of zinc, 2~4 grams of natrium nitrosum, 0.5~2 gram of sodium potassium tartrate tetrahydrate, 0.5~2 gram of calcium nitrate.Its phosphating process flow is：Alkali
Elute fat → washing → acidic activated → washing → surface active → washing → conversion processing → washing → drying；Its operating temperature
40~70 DEG C, the time is 5~60 minutes.One layer, which is obtained, in Mg alloy surface improves corrosion proof Zinc-calcium series phosphatating film.But its phosphorus
Change in solution and belong to strong carcinogenic chemical containing natrium nitrosum, there is very big harm, and NO to health-In parkerizing process
Though in have certain consumption, its surplus of etching waste liquor is still larger, and the part of consumption is also in the form of oxynitrides
Into air, also above-mentioned film layer wearability and bad, therefore phosphating coat surface is surface-treated very necessary.
One kind is disclosed in Publication No. CN102534599A patent document《Before cast magnesium alloy Workpiece painting application specially
With bonderite and production method》, raw material and mass percent disclosed in it are zinc oxide 1.5~2.5%, phosphatase 24~
12%th, hydrofluoric acid 0.2~0.4%, nickelous carbonate 0.2~0.4%, citric acid 0.2~0.8%, ammonium molybdate 0.5~1.6%, 12
Sodium alkyl sulfate 0.3~0.5%, reduced iron powder 1~3% and water surplus.Change and do not have calcium ion in formula, it is impossible to form corrosion resistant
Corrosion and the higher Zinc-calcium series phosphatating film of associativity, and to obtain the higher phosphatization surface of wearability, it is necessary to surface is changed
Enter.
The content of the invention
It is an object of the invention to provide a kind of corrosion resistance, wearability and excellent coating of adhesion of being formed
Be conducive to improving the zinc cathode conversion film of corrosion stability of magnesium alloy and the preparation method of epoxy coating.
The object of the present invention is achieved like this：
Magnesium alloy component by pretreatment is impregnated in magnesium alloy phosphating solution and carries out conversion processing, at the conversion
The operating temperature of reason is 40~70 DEG C, the time is 10~70 minutes, is then immersed in epoxy resin mixed liquor, stands 2 minutes
After take out, at room temperature hang 24 hours, then by 60 DEG C be heat-treated 2 hours.
The present invention can also include：
1st, the magnesium alloy phosphating solution contains using water as solvent in every liter of water：0.5~10 gram of calcium nitrate, phosphoric acid 20~
50 grams, 5 grams~20 grams of zinc oxide, 2~20 grams of citric acid, 1~10 gram of sodium nitrate, 1~10 gram of sodium potassium tartrate tetrahydrate, detergent alkylate
0.1~5 gram of sodium sulfonate.
2nd, the pH value of the magnesium alloy phosphating solution is 2~4.
3rd, epoxy resin mixed solution is made up of epoxy resin, curing agent and Nano filling.
Present invention is generally directed to be usually present substantial amounts of micropore and micro-crack in the conversion film of electrochemistry and chemical preparation
Etc. defect, these defects are not present in organic coating, and modified Nano filling is added in epoxy resin can strengthen compound
The wearability toughness of coating, but be due to the difference of magnesium alloy and organic resin paint chemistries, it is direct in Mg alloy surface
Coating organic resin is difficult to form the stronger coating of adhesion, is easy to come off in use.So excellent to integrate both
Point, makes the epoxy resin of addition Nano filling can be good at combining to form zinc cathode-epoxy with the Mg alloy surface after phosphatization
Coating.
The technological process for carrying out magnesium alloy surface zinc-calcium series phosphating conversion processing with phosphating solution of the present invention includes：Sand paper
Polishing → washing → ultrasound → alkali cleaning → washing → acidic activated → washing → surface active → washing → conversion processing → washing
→ drying phosphatization → surface modification treatment → immersion epoxy resin mixed solution；Will be by pretreated magnesium alloy component dipping
Conversion processing is carried out in above-mentioned magnesium alloy phosphating solution, is then invaded in epoxy resin mixed liquor, it is slow to pull out, it will obtain
Sample hang at room temperature hour, then through Overheating Treatment, so that coating fully solidifies.
Its Main Ingredients and Appearance of the epoxy resin mixed liquor of the present invention is epoxy resin and curing agent, and adds modified nanometer
Filler, by Nano filling plus such as enters into epoxy resin to improve anti-corrosion, the wearability of composite coating.
Compared with prior art, the element that not only pollution such as not fluorine-containing, chromium is harmful in phosphating solution of the present invention, also combines electricity
The advantage of chemistry and chemical preparation conversion film and organic resin coating, had both overcome electrochemistry and had existed with the conversion film that chemistry is formed
The defect of a large amount of micropores and micro-crack, enhances the adhesion of organic resin coating and magnesium alloy again.Either corrosion resistance, is tied
With joint efforts, especially wearability has very big improvement.
Brief description of the drawings
Fig. 1 is the Tafel curve comparison figures that different phosphating coats and phosphating coat apply epoxy coating.
Fig. 2 is the comparison diagram of the coefficient of friction of Zinc-calcium series phosphatating film and phosphating coat painting epoxy coating.
Embodiment
Illustrate below and the present invention is described in more detail.
Example one：By following recipe configuration zinc-calcium series phosphating solution, contain in every liter of water：
37.5 grams of phosphoric acid,
9 grams of zinc oxide,
5 grams of citric acid,
2 grams of sodium nitrate,
2 grams of sodium potassium tartrate tetrahydrate,
0.2 gram of neopelex.
The pH value for adjusting solution is 3.23.
Technological process prepared by Zinc-calcium series phosphatating-epoxy coating：Sand paper polishing → washing → ultrasound → washing → alkali cleaning →
Washing → pickling → washing → cold wind drying → phosphatization.The technological process is concretely comprised the following steps：First magnesium alloy is polished, then by magnesium
Alloy is put into the beaker of absolute ethyl alcohol, ultrasonically treated in instrument is cleaned by ultrasonic, and is obtained by alkali cleaning decontamination, pickling except oxide
The magnesium alloy of surface uniform and delicate, is then impregnated in above-mentioned magnesium alloy phosphating solution by above-mentioned pretreated magnesium alloy component
Middle carry out conversion processing, 40~70 DEG C of its operating temperature, the time is 5~60 minutes.Obtain being formed the magnesium alloy of zinc phosphating film.
Example two：By following recipe configuration zinc-calcium series phosphating solution, contain in every liter of water：
1.5 grams of calcium nitrate,
37.5 grams of phosphoric acid,
9 grams of zinc oxide,
5 grams of citric acid,
2 grams of sodium nitrate,
2 grams of sodium potassium tartrate tetrahydrate,
0.2 gram of neopelex.
The pH value for adjusting solution is 3.23.
The technological process of Zinc-calcium series phosphatating film：Sand paper polishing → washing → ultrasound → washing → alkali cleaning → washing → pickling →
Washing → cold wind drying → phosphatization.The technological process is concretely comprised the following steps：First magnesium alloy is polished, then magnesium alloy is put into anhydrous
It is ultrasonically treated in instrument is cleaned by ultrasonic in the beaker of ethanol, surface uniform and delicate is obtained except oxide by alkali cleaning decontamination, pickling
Magnesium alloy, then by above-mentioned pretreated magnesium alloy component be impregnated in above-mentioned magnesium alloy phosphating solution carry out conversion at
Reason, 40~70 DEG C of its operating temperature, the time is 5~60 minutes.Obtain being formed the magnesium alloy of Zinc-calcium series phosphatating film.
Example three：By following recipe configuration zinc-calcium series phosphating solution, contain in every liter of water：
1.5 grams of calcium nitrate,
37.5 grams of phosphoric acid,
9 grams of zinc oxide,
5 grams of citric acid,
2 grams of sodium nitrate,
2 grams of sodium potassium tartrate tetrahydrate,
0.2 gram of neopelex.
The pH value for adjusting solution is 3.23.
Technological process prepared by Zinc-calcium series phosphatating-epoxy coating：Sand paper polishing → washing → ultrasound → washing → alkali cleaning →
Washing → pickling → washing → cold wind drying → phosphatization → immersion epoxy resin mixed solution.The specific steps of the technological process
For：First magnesium alloy is polished, then magnesium alloy is put into the beaker of absolute ethyl alcohol, it is ultrasonically treated in instrument is cleaned by ultrasonic, pass through
Alkali cleaning decontamination, pickling remove the magnesium alloy that oxide obtains surface uniform and delicate, then will pass through pretreated magnesium alloy component
It is impregnated in above-mentioned magnesium alloy phosphating solution and carries out conversion processing, 40~70 DEG C of its operating temperature, the time is 10~70 minutes, so
After invade in epoxy resin mixed liquor, stand 2 minutes after slowly pull out, obtained sample is hung 24 hours at room temperature,
It is heat-treated 2 hours by 60 DEG C again, so that coating fully solidifies.
By the Tafel polarization curves coefficient of friction and example two, three coefficient of frictions of the sample for measuring above-mentioned example one, two, three
(result is as shown in Figure 1, 2) is known that：
1. the corrosion resistance of Zinc-calcium series phosphatating film is better than zinc phosphating film, and after Zinc-calcium series phosphatating film coating epoxy resin,
Corrosion current density decreases again, and corrosion potential also continues to rise, and this is probably due to Zinc-calcium series phosphatating film and asphalt mixtures modified by epoxy resin
Associativity between fat is more firm, Cl-It is more difficult to penetrate the reason of the protection film layer arrival matrix of outer layer Deng Korrosionsmedium.It is comprehensive
It is best that the upper Zinc-calcium series phosphatating film applies its corrosion resistance after epoxy resin.
2. be can be seen that by the experiment of coefficient of friction by coating epoxy coating, magnesium is tested under the same conditions
The alloy surface coating destroyed time substantially increases so its abrasion-resistance is improved significantly.
Claims (4)
1. it is a kind of be conducive to improve corrosion stability of magnesium alloy zinc cathode conversion film and epoxy coating preparation method, it is characterized in that：
Magnesium alloy component by pretreatment is impregnated in magnesium alloy phosphating solution and carries out conversion processing, the work of the conversion processing
Temperature is 40~70 DEG C, the time is 10~70 minutes, is then immersed in epoxy resin mixed liquor, is taken out after standing 2 minutes,
Hang 24 hours, then be heat-treated 2 hours by 60 DEG C at room temperature.
2. the preparation according to claim 1 for being conducive to improving the zinc cathode conversion film and epoxy coating of corrosion stability of magnesium alloy
Method, it is characterized in that：The magnesium alloy phosphating solution contains using water as solvent in every liter of water：0.5~10 gram of calcium nitrate, phosphoric acid
20~50 grams, 5 grams~20 grams of zinc oxide, 2~20 grams of citric acid, 1~10 gram of sodium nitrate, 1~10 gram of sodium potassium tartrate tetrahydrate, dodecane
0.1~5 gram of base benzene sulfonic acid sodium salt.
3. the preparation according to claim 2 for being conducive to improving the zinc cathode conversion film and epoxy coating of corrosion stability of magnesium alloy
Method, it is characterized in that：The pH value of the magnesium alloy phosphating solution is 2~4.
4. being conducive to according to claim 1,2 or 3 improves the zinc cathode conversion film and epoxy coating of corrosion stability of magnesium alloy
Preparation method, it is characterized in that：Epoxy resin mixed solution is made up of epoxy resin, curing agent and Nano filling.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710190051.9A CN107142470A (en) | 2017-03-28 | 2017-03-28 | Be conducive to improving the zinc cathode conversion film of corrosion stability of magnesium alloy and the preparation method of epoxy coating |
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|---|---|---|---|
| CN201710190051.9A CN107142470A (en) | 2017-03-28 | 2017-03-28 | Be conducive to improving the zinc cathode conversion film of corrosion stability of magnesium alloy and the preparation method of epoxy coating |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108187994A (en) * | 2018-01-17 | 2018-06-22 | 太原工业学院 | A kind of preparation method for improving magnesium alloy anticorrosion stress-resistant performance epoxy coating |
| CN109680271A (en) * | 2018-12-29 | 2019-04-26 | 三一重机有限公司 | The method and hydraulic steel pipe of hydraulic steel pipe anti-corrosion treatment |
| CN110172700A (en) * | 2019-06-26 | 2019-08-27 | 匡云叶 | A kind of Mg alloy surface treatment fluid and surface treatment method |
| CN116082916A (en) * | 2022-12-20 | 2023-05-09 | 广州三孚新材料科技股份有限公司 | Efficient anti-corrosion hole sealing liquid for magnesium alloy surface and application thereof |
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| CN101029386A (en) * | 2007-04-09 | 2007-09-05 | 湖南大学 | Triple cationic phosphorizing fluid containing calcium, zinc and manganese for steel plate and zinc-coated plate treatment |
| US20110200754A1 (en) * | 2008-10-17 | 2011-08-18 | Battelle Memorial Institute | Corrosion resistant primer coating |
| CN102732871A (en) * | 2011-04-15 | 2012-10-17 | 中国科学院金属研究所 | Neodymium iron boron magnet material phosphating treatment and organic coating double layers protection method |
| CN103374714A (en) * | 2012-04-13 | 2013-10-30 | 上海顶旭化学品有限公司 | Zinc-calcium series phosphating solution for metal cold-drawing |
| CN103924232A (en) * | 2014-04-30 | 2014-07-16 | 中南大学 | Technical method for imitating copper and gold on surface of magnesium alloy |
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2017
- 2017-03-28 CN CN201710190051.9A patent/CN107142470A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101029386A (en) * | 2007-04-09 | 2007-09-05 | 湖南大学 | Triple cationic phosphorizing fluid containing calcium, zinc and manganese for steel plate and zinc-coated plate treatment |
| US20110200754A1 (en) * | 2008-10-17 | 2011-08-18 | Battelle Memorial Institute | Corrosion resistant primer coating |
| CN102732871A (en) * | 2011-04-15 | 2012-10-17 | 中国科学院金属研究所 | Neodymium iron boron magnet material phosphating treatment and organic coating double layers protection method |
| CN103374714A (en) * | 2012-04-13 | 2013-10-30 | 上海顶旭化学品有限公司 | Zinc-calcium series phosphating solution for metal cold-drawing |
| CN103924232A (en) * | 2014-04-30 | 2014-07-16 | 中南大学 | Technical method for imitating copper and gold on surface of magnesium alloy |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108187994A (en) * | 2018-01-17 | 2018-06-22 | 太原工业学院 | A kind of preparation method for improving magnesium alloy anticorrosion stress-resistant performance epoxy coating |
| CN108187994B (en) * | 2018-01-17 | 2020-12-22 | 太原工业学院 | Preparation method of epoxy coating for improving stress corrosion resistance of magnesium alloy |
| CN109680271A (en) * | 2018-12-29 | 2019-04-26 | 三一重机有限公司 | The method and hydraulic steel pipe of hydraulic steel pipe anti-corrosion treatment |
| CN110172700A (en) * | 2019-06-26 | 2019-08-27 | 匡云叶 | A kind of Mg alloy surface treatment fluid and surface treatment method |
| CN116082916A (en) * | 2022-12-20 | 2023-05-09 | 广州三孚新材料科技股份有限公司 | Efficient anti-corrosion hole sealing liquid for magnesium alloy surface and application thereof |
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Application publication date: 20170908 |