CN110863195B - Magnesium alloy surface treatment method used in high-concentration chloride ion environment - Google Patents
Magnesium alloy surface treatment method used in high-concentration chloride ion environment Download PDFInfo
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- CN110863195B CN110863195B CN201911193722.2A CN201911193722A CN110863195B CN 110863195 B CN110863195 B CN 110863195B CN 201911193722 A CN201911193722 A CN 201911193722A CN 110863195 B CN110863195 B CN 110863195B
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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
- C23C22/48—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 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/57—Treatment of magnesium or alloys based thereon
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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
- C23C22/60—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 alkaline aqueous solutions with pH greater than 8
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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
- C23C22/68—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 solutions with pH between 6 and 8
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- Chemical Kinetics & Catalysis (AREA)
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- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention provides a magnesium alloy surface treatment method used in a high-concentration chloride ion environment, which mainly comprises the steps of disodium hydrogen phosphate-ammonia water mixed solution treatment and dip-coating treatment. The magnesium alloy treated by the method can be stably applied to a high-concentration chloride ion environment for a long time, and the limitation of the high-concentration chloride ion environment to the application of the magnesium alloy for a long time is broken through. The method is suitable for surface treatment of magnesium alloy workpieces of various types, sizes and shapes, and has the characteristics of simple process, high degree of automation of operation, easiness in large-scale industrial treatment and the like. The surface treatment method can also be popularized and applied to other metal materials applied in high-concentration chloride ion environments.
Description
Technical Field
The invention belongs to the technical field of magnesium alloy, and particularly relates to a magnesium alloy surface treatment method used in a high-concentration chloride ion environment.
Background
The magnesium alloy has the excellent characteristics of low density, high specific strength, good vibration reduction and heat dissipation performance, strong electromagnetic radiation shielding capacity, excellent biocompatibility, environmental friendliness and the like, and has important application potential in multiple fields. But the corrosion resistance is poor, and the corrosion is very easy to occur, which seriously hinders the wide application of the alloy. The traditional surface treatment technologies such as chemical conversion, micro-arc oxidation and coating (plating) can provide a certain protection effect for the magnesium alloy and meet the conventional application requirements of the magnesium alloy. The super-hydrophobic protective film technology, the self-repairing protective film technology and the like developed in recent years can provide more effective protection for the magnesium alloy. However, in a high-concentration chloride ion environment such as seawater or a marine climate environment, since chloride ions are strong corrosive ions, have small ionic radius and strong penetrability, easily penetrate through a film layer, and replace other atoms to form chlorides, so that corrosion is accelerated, the magnesium alloy treated by the above technology hardly meets the application requirement of the magnesium alloy in the high-concentration chloride ion environment. Therefore, it is necessary and urgent to develop a surface treatment technique for magnesium alloys suitable for use in an environment with high concentration of chloride ions.
Disclosure of Invention
In view of the above problems in the prior art, an object of the present invention is to provide a method for treating a surface of a magnesium alloy in a high-concentration chloride ion environment, so that the treated magnesium alloy can be stably applied in the high-concentration chloride ion environment for a long time.
The purpose of the invention is realized as follows: a magnesium alloy surface treatment method used in a high-concentration chloride ion environment is characterized by comprising the following steps:
immersing a clean magnesium alloy workpiece into a 70-85 ℃ disodium hydrogen phosphate-ammonia water mixed solution for treatment for 20-40 minutes, taking out the workpiece, washing the workpiece with pure water, and drying the workpiece with compressed air;
the mixed solution of the disodium hydrogen phosphate and the ammonia water is formed by mixing 600-800 ml of 0.1mol/L disodium hydrogen phosphate aqueous solution and 200-400 ml of commercially available strong ammonia water;
placing the magnesium alloy workpiece processed in the step I in a dip coating machine for dip coating film forming: respectively and sequentially placing 10-40 g/L85-95 ℃ polyvinyl alcohol aqueous solution, 80-90 ℃ hot water, 30-60 g/L50-60 ℃ ammonium polymethacrylate aqueous solution, 50-60 ℃ warm water, 20-30 ℃ polyaziridine aqueous solution and room temperature pure water in 6 stations of a dipping and pulling coating machine, setting a program to enable the workpiece to be immersed in the 6 stations for 5-10 minutes, 10-20 seconds, 10-15 minutes, 20-30 seconds, 15-20 minutes and 30-40 seconds in sequence as a cycle, repeating the process for 4-8 cycles, taking out the workpiece, and drying the workpiece in a 100-120 ℃ drying oven for 1-2 hours to obtain the magnesium alloy workpiece which can be stably applied to a high-concentration chloride ion environment for a long time.
Further, the magnesium alloy is any type of magnesium alloy and is not limited by shape and size.
Compared with the prior art, the invention has the following advantages:
1. the magnesium alloy workpiece treated by the method can be stably applied to high-concentration chloride ion environments such as seawater or ocean atmosphere for a long time, and the limitation of the high-concentration chloride ion environment to the application of the magnesium alloy for a long time is broken through. The surface treatment method can also be popularized and applied to other metal materials applied in high-concentration chloride ion environments, and has wide prospects.
2. The principle of the method is that the magnesium alloy reacts with a mixed solution of disodium hydrogen phosphate and ammonia water by utilizing the high chemical activity of the magnesium alloy to generate a compact and firm fine microstructure in situ, so that the surface stability is enhanced, a large number of hydroxyl groups can be provided, and a compact three-dimensional network structure formed by directly bonding polyvinyl alcohol, ammonium polymethacrylate and polyazepine in the follow-up process is convenient, and the network structure is formed by high-sensitivity reversible non-covalent bonding and is very firm; particularly, even if damage and damage occur, the extremely high-activity chloride ions in the corrosion medium can drive the molecular chains to flow so that the molecules are bonded into a three-dimensional network structure again, and therefore the magnesium alloy workpiece can be ensured to be stably applied to a high-concentration chloride ion environment for a long time.
3. The method is suitable for surface treatment of magnesium alloy workpieces of various types, sizes and shapes. The method has the characteristics of simple process, high degree of automation of operation, easy large-scale industrial treatment and the like.
Detailed Description
The present invention will be described in further detail with reference to examples.
It should be noted that these examples are only for illustrating the present invention, and not for limiting the present invention, and the simple modification of the method based on the idea of the present invention is within the protection scope of the present invention.
Processing magnesium alloys of different types into magnesium alloy workpieces of different sizes and shapes according to requirements, sequentially polishing the magnesium alloy workpieces by 180#, 400# and 800# abrasive paper until the surfaces are smooth and flat, washing the magnesium alloy workpieces by pure water, ultrasonically cleaning the magnesium alloy workpieces in absolute ethyl alcohol for 5 minutes, taking the magnesium alloy workpieces out, and drying the magnesium alloy workpieces by cold air to obtain the workpieces with clean surfaces.
Example 1:
the AZ91 magnesium alloy workpiece is subjected to the following surface treatment:
immersing a clean magnesium alloy workpiece into a mixed solution of disodium hydrogen phosphate and ammonia water at 85 ℃ for treatment for 20 minutes, taking out the workpiece, washing the workpiece with pure water, and drying the workpiece with compressed air; wherein the mixed solution of the disodium hydrogen phosphate and the ammonia water is formed by mixing 800 ml of 0.1mol/L disodium hydrogen phosphate aqueous solution and 200 ml of commercial concentrated ammonia water;
placing the magnesium alloy workpiece processed in the step I in a dip coating machine for dip coating film forming: respectively and sequentially placing a 40 g/L85 ℃ polyvinyl alcohol aqueous solution, 80 ℃ hot water, a 60 g/L50 ℃ ammonium polymethacrylate aqueous solution, 50 ℃ warm water, a 50 g/L20 ℃ polyaziridine aqueous solution and room temperature pure water in 6 stations of a dip-coating machine, setting a program to enable the workpiece to be immersed in the 6 stations for 10 minutes, 20 seconds, 15 minutes, 30 seconds, 20 minutes and 40 seconds in sequence as a cycle, repeating for 4 cycles, taking out the workpiece, and drying the workpiece in a 120 ℃ drying oven for 1 hour to obtain the magnesium alloy workpiece which can be stably applied to a high-concentration chloride ion environment for a long time.
Example 2:
WE43 magnesium alloy workpiece was subjected to the following surface treatments:
immersing a clean magnesium alloy workpiece into a 70 ℃ disodium hydrogen phosphate-ammonia water mixed solution for treatment for 40 minutes, taking out the workpiece, washing the workpiece with pure water, and drying the workpiece with compressed air; wherein the mixed solution of the disodium hydrogen phosphate and the ammonia water is prepared by mixing 600 ml of 0.1mol/L disodium hydrogen phosphate aqueous solution and 400 ml of commercial strong ammonia water;
placing the magnesium alloy workpiece processed in the step I in a dip coating machine for dip coating film forming: respectively and sequentially placing a 95 ℃ polyvinyl alcohol aqueous solution with the concentration of 10 g/L, 90 ℃ hot water, a 60 ℃ ammonium polymethacrylate aqueous solution with the concentration of 30 g/L, 60 ℃ warm water, a 30 ℃ polyaziridine aqueous solution with the concentration of 20 g/L and room temperature pure water in 6 stations of a dip-coating machine, setting a program to enable the workpiece to be immersed in the 6 stations for 5 minutes, 10 seconds, 10 minutes, 20 seconds, 15 minutes and 30 seconds in sequence as a cycle, repeating for 8 cycles, taking out the workpiece, and drying the workpiece in an oven at 100 ℃ for 2 hours to obtain the magnesium alloy workpiece which can be stably applied to a high-concentration chloride ion environment for a long time.
Example 3:
the ZM60 magnesium alloy workpiece is subjected to the following surface treatment:
immersing a clean magnesium alloy workpiece into a mixed solution of disodium hydrogen phosphate and ammonia water at 80 ℃ for treatment for 30 minutes, taking out the workpiece, washing the workpiece with pure water, and drying the workpiece with compressed air; wherein the mixed solution of the disodium hydrogen phosphate and the ammonia water is formed by mixing 700 ml of 0.1mol/L disodium hydrogen phosphate aqueous solution and 300 ml of commercial strong ammonia water;
placing the magnesium alloy workpiece processed in the step I in a dip coating machine for dip coating film forming: respectively and sequentially placing 90 ℃ polyvinyl alcohol aqueous solution with the concentration of 30 g/L, 85 ℃ hot water, 55 ℃ ammonium polymethacrylate aqueous solution with the concentration of 50 g/L, 55 ℃ warm water, 25 ℃ polyaziridine aqueous solution with the concentration of 40 g/L and room temperature pure water in 6 stations of a dip-coating machine, setting a program to ensure that the workpiece is immersed in the 6 stations for 8 minutes, 15 seconds, 12 minutes, 25 seconds, 18 minutes and 35 seconds in sequence as a cycle, repeating the 6 cycles, taking out the workpiece, and drying the workpiece in a drying oven at 110 ℃ for 1.5 hours to obtain the magnesium alloy workpiece which can be stably applied to a high-concentration chloride ion environment for a long time.
Example 4:
the ZK40 magnesium alloy workpiece is subjected to the following surface treatment:
immersing a clean magnesium alloy workpiece into a 75 ℃ disodium hydrogen phosphate-ammonia water mixed solution for treatment for 35 minutes, taking out the workpiece, washing the workpiece with pure water, and drying the workpiece with compressed air; wherein the mixed solution of the disodium hydrogen phosphate and the ammonia water is formed by mixing 750 ml of 0.1mol/L disodium hydrogen phosphate aqueous solution and 250 ml of commercial strong ammonia water;
placing the magnesium alloy workpiece processed in the step I in a dip coating machine for dip coating film forming: respectively and sequentially placing a 95 ℃ polyvinyl alcohol aqueous solution with the concentration of 20 g/L, 90 ℃ hot water, a 55 ℃ ammonium polymethacrylate aqueous solution with the concentration of 40 g/L, 55 ℃ warm water, a 30 ℃ polyaziridine aqueous solution with the concentration of 30 g/L and room temperature pure water in 6 stations of a dip-coating machine, setting a program to ensure that the workpiece is immersed in the 6 stations for 10 minutes, 15 seconds, 15 minutes, 25 seconds, 20 minutes and 35 seconds in sequence as a cycle, repeating the cycle for 7 cycles, taking out the workpiece, and drying the workpiece in an oven at 105 ℃ for 2 hours to obtain the magnesium alloy workpiece which can be stably applied to a high-concentration chloride ion environment for a long time.
The performance test method comprises the following steps: according to the Salt spray experiment international standard 'ISO 9227:2017 corosion tests in artificial atmosphers-Salt spray tests', an improved neutral Salt spray test method (the chloride ion concentration is doubled compared with the standard ISO 9227: 2017) is adopted to test the stability of the workpiece in a high-concentration chloride ion environment. The experiment is carried out in an FDY/L-03 type salt spray corrosion test box, the temperature in the box is controlled to be 35 +/-2 ℃, and the components of mist liquid are as follows: 100 +/-5 g/L sodium chloride solution and continuous spraying mode. The control was a clean magnesium alloy workpiece that had not been treated by the above examples. And 3 parallel samples of various samples are checked regularly, and the generation time of corrosion on the surfaces of the samples is recorded.
And (4) performance test results: the clean AZ91, WE43, ZM60 and ZK40 magnesium alloy workpieces which are not treated by the above examples all have pitting points observed on the inner surface of the half day, and the AZ91, WE43, ZM60 and ZK40 magnesium alloy workpieces which are treated by the above 1-4 examples have no pitting points observed on the surfaces of the magnesium alloy workpieces after 60-day salt spray experiments, which shows that the magnesium alloy treated by the invention can be stably applied to high-concentration chlorine ion environments for a long time.
In the above embodiments, magnesium alloys of different types are used as the treatment objects, and it should be noted that the present invention can also be applied to surface treatment of other metal materials applied in a high-concentration chloride ion environment.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the technical solutions, and those skilled in the art should understand that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all that should be covered by the claims of the present invention.
Claims (2)
1. A magnesium alloy surface treatment method used in a high-concentration chloride ion environment is characterized by comprising the following steps:
immersing a clean magnesium alloy workpiece into a 70-85 ℃ disodium hydrogen phosphate-ammonia water mixed solution for treatment for 20-40 minutes, taking out the workpiece, washing the workpiece with pure water, and drying the workpiece with compressed air;
the mixed solution of the disodium hydrogen phosphate and the ammonia water is formed by mixing 600-800 ml of 0.1mol/L disodium hydrogen phosphate aqueous solution and 200-400 ml of commercially available strong ammonia water;
placing the magnesium alloy workpiece processed in the step I in a dip coating machine for dip coating film forming: respectively and sequentially placing 10-40 g/L85-95 ℃ polyvinyl alcohol aqueous solution, 80-90 ℃ hot water, 30-60 g/L50-60 ℃ ammonium polymethacrylate aqueous solution, 50-60 ℃ warm water, 20-30 ℃ polyaziridine aqueous solution and room temperature pure water in 6 stations of a dipping and pulling coating machine, setting a program to enable the workpiece to be immersed in the 6 stations for 5-10 minutes, 10-20 seconds, 10-15 minutes, 20-30 seconds, 15-20 minutes and 30-40 seconds in sequence as a cycle, repeating the process for 4-8 cycles, taking out the workpiece, and drying the workpiece in a 100-120 ℃ drying oven for 1-2 hours to obtain the magnesium alloy workpiece which can be stably applied to a high-concentration chloride ion environment for a long time.
2. The method for surface treatment of magnesium alloy in high-concentration chloride ion environment according to claim 1, wherein the magnesium alloy is any type of magnesium alloy and is not limited by shape and size.
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| CN1395605A (en) * | 2000-01-17 | 2003-02-05 | 日本巴卡萊近估股份有限公司 | Treating agent for imparting hydrophilicity and high corrosion resistance, hydrophilizing fluid, and method of hydrophilizing |
| CN1431454A (en) * | 2002-01-09 | 2003-07-23 | 株式会社神户制钢所 | Aluminium alloy material with coated film and heat exchanger radiating fin made by same material |
| CN1966766A (en) * | 2005-11-16 | 2007-05-23 | 比亚迪股份有限公司 | Method for processing Mg alloy surface |
| CN101054712A (en) * | 2007-02-07 | 2007-10-17 | 北京交通大学 | Method of preparing transparent film on magnesium alloy surface |
| WO2014044806A1 (en) * | 2012-09-20 | 2014-03-27 | Coventya Sas | Alkaline aqueous solution for improving corrosion resistance of a cr(iii) conversion coating and method for producing such coating and its use |
| CN107012454A (en) * | 2017-04-10 | 2017-08-04 | 武汉迪赛鸿印科技有限公司 | A kind of bolt surface antirust fastening agent |
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- 2019-11-28 CN CN201911193722.2A patent/CN110863195B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1395605A (en) * | 2000-01-17 | 2003-02-05 | 日本巴卡萊近估股份有限公司 | Treating agent for imparting hydrophilicity and high corrosion resistance, hydrophilizing fluid, and method of hydrophilizing |
| CN1431454A (en) * | 2002-01-09 | 2003-07-23 | 株式会社神户制钢所 | Aluminium alloy material with coated film and heat exchanger radiating fin made by same material |
| CN1966766A (en) * | 2005-11-16 | 2007-05-23 | 比亚迪股份有限公司 | Method for processing Mg alloy surface |
| CN101054712A (en) * | 2007-02-07 | 2007-10-17 | 北京交通大学 | Method of preparing transparent film on magnesium alloy surface |
| WO2014044806A1 (en) * | 2012-09-20 | 2014-03-27 | Coventya Sas | Alkaline aqueous solution for improving corrosion resistance of a cr(iii) conversion coating and method for producing such coating and its use |
| CN107012454A (en) * | 2017-04-10 | 2017-08-04 | 武汉迪赛鸿印科技有限公司 | A kind of bolt surface antirust fastening agent |
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