CN107916421A - A kind of preparation method of corrosion resistance magnesium alloy super-hydrophobic surface - Google Patents
A kind of preparation method of corrosion resistance magnesium alloy super-hydrophobic surface Download PDFInfo
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- CN107916421A CN107916421A CN201711114477.2A CN201711114477A CN107916421A CN 107916421 A CN107916421 A CN 107916421A CN 201711114477 A CN201711114477 A CN 201711114477A CN 107916421 A CN107916421 A CN 107916421A
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/22—Acidic compositions for etching magnesium or alloys thereof
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
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Abstract
The invention belongs to technical field of material surface treatment, and in particular to a kind of preparation method of corrosion resistance magnesium alloy super-hydrophobic surface.The present invention carries out surface corrosion processing by organic acid to magnesium alloy first,Its surface is set to form rough surface,Then by being carried out in material is gone out,Magnesium alloy recess is deposited in using the nano-titanium dioxide gone out in material,Form central point,The material used when being powered in material forms film in Mg alloy surface,At the same time snowflake shape is formed in nano-titanium dioxide central spot,Increase hydrophobic performance,Magnesium alloy forms oxide with silver ion and is quickly attached to Mg alloy surface,The super hydrophobic surface to be formed is set to form micro- two-layer structure,Under the action of nano-titanium dioxide graft reaction is carried out with organic silicon monomer,Add hydrophobicity,Improve corrosion resistance,Aqueous polyurethane is synthesized again,Pass through the modification of lauric monoglyceride and fumaric acid,It is polymer-modified that there is photosensitive property,In the effect of titanium dioxide,Carry out self-curing.
Description
Technical field
The invention belongs to technical field of material surface treatment, and in particular to a kind of corrosion resistance magnesium alloy super-hydrophobic surface
Preparation method.
Background technology
Magnesium alloy is as a kind of light metal material, it is considered to be the green engineering material of 21 century.Because it is with specific strength
High, specific stiffness height, thermal fatigue property is good, biocompatibility is good, capability of electromagnetic shielding is excellent, thermal conductivity ability is strong, antidetonation
Property it is good and recyclable the advantages that, have a wide range of applications in fields such as communications and transportation, biomedicine, aerospace and national defense industry
Prospect.In recent years, magnesium alloy by its good biocompatibility, low-density, with skeleton similar in elasticity modulus etc. it is special
Point, becomes current most potential medical metal material, has very strong development prospect.But so far, magnesium alloy is made
Huge contrast is still remained between the application potential and reality of biomaterial, the poor corrosion resistance of magnesium alloy is to restrict magnesium alloy
The bottleneck to elicit latent faculties.Since magnesium has potential minimum in all structural metals, chemism is very high, and the oxide-film of magnesium is dredged
Pine, so causing the corrosion resisting property of magnesium alloy poor.And this also constrains the development of magnesium alloy.
Super hydrophobic surface refers to that base material is more than the static contact angle of water on 150 ° of surface, as deposited extensively in nature
Nelumbo section blade face, the leg of water skipper, dragonfly wing etc., they are respectively provided with super-hydrophobicity and automatical cleaning ability.By to material
Surface is modified, and makes it have superhydrophobic characteristic, can effectively reduce the surface free energy of base material, is improved and is controlled material
Wetting, stick together, lubricate and polishing machine, there is huge application potential in material modification and application aspect.In material substrate
Building super-hydrophobic coat has well anticorrosive, fluid drag-reduction and self-cleaning surface performance, in the side such as medical magnesium alloy component
Mask has wide practical use.
The research of super-hydrophobic lotus leaf shows：Surface is micro-/receive binary coarse structure and low-surface energy substance to be that lotus leaf has super
The main reason for hydrophobic automatically cleaning effect.Although the preparation method of super hydrophobic surface is existing very much, such as carved using plasma, chemistry
The method that the technologies such as erosion technology, plating are combined with coating low-surface energy substance, or the method using chemical conversion, can prepare
Go out super hydrophobic surface, but these methods or equipment are expensive, or have pollution to environment, or manufacturing cycle is long etc., still
There are room for improvement.
Super hydrophobic surface is prepared on almag surface needs two steps：First, its surface is roughened structure
Build micro-nano coarse structure；Second, reduce its surface energy, usually using low-surface energy substance silane, silicon fluoride or stearic acid etc. come
The obtained coarse structure of modification.But above method process is complicated, the time is longer, and not easy to control, in addition strong acid and strong base
Largely environment is polluted using meeting.Therefore, suitable magnesium alloy hydrophobic surface is prepared in invention, this will be promoted significantly
China's industrial expansion, is extremely to have promising thing.
The content of the invention
The technical problems to be solved by the invention：It is poor for current magnesium alloy hydrophobic surface corrosion resistance, and manufacture method
Excessive cycle, the problem of being polluted to environment, the present invention provides a kind of preparation of corrosion resistance magnesium alloy super-hydrophobic surface
Method.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of preparation method of corrosion resistance magnesium alloy super-hydrophobic surface, the preparation method include the following steps：
（1）Count in parts by weight, take 80~90 parts of acetone, 45~50 parts of polyoxypropyleneglycols, 25~30 parts of toluene diisocyanates
Acid esters, 13~15 parts of dihydromethyl propionic acids, 10~13 parts of lauric monoglycerides, 9~11 parts of fumaric acid, 8~10 parts of nanometers two
Titanium oxide, 3~5 parts of catalyst, 2~5 parts of crosslinking agents, 1~3 part of nano silver and 1~3 part of emulsifying agent；
（2）Acetone, polyoxypropyleneglycol, toluene di-isocyanate(TDI), dihydromethyl propionic acid are put into reaction kettle first, used
Nitrogen protect, preheated at 60~80 DEG C, add cinnamic acid monoglyceride, crosslinking agent, be warming up at 100~105 DEG C into
Row reaction；
（3）After the completion of reaction, 85~90 DEG C are cooled to, adds fumaric acid, nano-titanium dioxide, nano silver, catalyst and breast
Agent, is gone out the gas displacement in reaction kettle using hydrogen, and boosts to 1.3~1.6MPa, and stirring, is cooled to room temperature, and is discharged,
Material is collected out, it is spare；
（4）Magnesium alloy is put into citric acid solution and is soaked, takes out the magnesium alloy of immersion, using water washing Mg alloy surface to washing
Wash liquid to be in neutrality, air-dried using nitrogen, obtain pretreatment magnesium alloy；
（5）Pretreatment magnesium alloy is put into container, add it is spare go out material, dipping pretreatment 4~6cm of magnesium alloy, 8~
It is powered at 10 DEG C to container, after to be energised, takes out magnesium alloy, air-dry, obtain magnesium alloy substrate；
（6）Isopropanol, aminopropyl end-blocking dimethyl silicone polymer and magnesium alloy substrate are put into container, stood at 90 DEG C,
Magnesium alloy substrate is taken out, is air-dried, up to corrosion resistance magnesium alloy super-hydrophobic surface.
The catalyst is any one in palladium carbon catalyst, platinum catalyst.
The crosslinking agent is any one in cumyl peroxide, benzoyl peroxide.
The emulsifying agent is any one in butyl phenol polyethenoxy ether, phenethyl phenol polyethenoxy ether.
The step（6）Middle isopropanol, aminopropyl end-blocking dimethyl silicone polymer and magnesium alloy substrate quality ratio are 9：1~
3：6.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention carries out surface corrosion processing by organic acid to magnesium alloy first, its surface is formed rough table
Face, then by being carried out in material is gone out, is deposited in magnesium alloy recess using the nano-titanium dioxide gone out in material, forms center
Point, then the effect in energization, the material used in material form film in Mg alloy surface, while in nano-titanium dioxide central point
Place forms snowflake shape, increases hydrophobic performance, while nano silver partly forms silver ion in material is gone out, and under energization, magnesium closes
Gold forms oxide with silver ion and is quickly attached to Mg alloy surface, the super hydrophobic surface to be formed is formed micro- two-layer structure, carries
High corrosion resistance, then and organic silicon monomer, graft reaction is carried out under the action of nano-titanium dioxide, is added hydrophobic
Property, improve corrosion resistance；
（2）The present invention is formed water-based poly- using polyoxypropyleneglycol, toluene di-isocyanate(TDI), dihydromethyl propionic acid etc. as raw material
Urethane, by the modification of lauric monoglyceride and fumaric acid, increases the photosensitive property of aqueous polyurethane, while improves water-soluble
Property, avoids using organic solvent, reduces the pollution to environment, has a good photosensitive property simultaneously because polymer-modified, and
And under the action of titanium dioxide, self-curing can be carried out, good film is formed, reduces manufacturing cycle.
Embodiment
Catalyst is palladium carbon catalyst（Chemical Co., Ltd. is reached in Shaanxi）, platinum catalyst（The luxuriant and rich with fragrance chemistry science and technology hair of Tianjin match
Open up Co., Ltd）In any one.
Crosslinking agent is any one in cumyl peroxide, benzoyl peroxide.
Emulsifying agent is any one in butyl phenol polyethenoxy ether, phenethyl phenol polyethenoxy ether.
A kind of preparation method of corrosion resistance magnesium alloy super-hydrophobic surface, the preparation method include the following steps：
（1）Count in parts by weight, take 80~90 parts of acetone, 45~50 parts of polyoxypropyleneglycols, 25~30 parts of toluene diisocyanates
Acid esters, 13~15 parts of dihydromethyl propionic acids, 10~13 parts of lauric monoglycerides, 9~11 parts of fumaric acid, 8~10 parts of nanometers two
Titanium oxide, 3~5 parts of catalyst, 2~5 parts of crosslinking agents, 1~3 part of nano silver and 1~3 part of emulsifying agent；
（2）Acetone, polyoxypropyleneglycol, toluene di-isocyanate(TDI), dihydromethyl propionic acid are put into reaction kettle first, used
Nitrogen is protected, and 45~50min of preheating is carried out at 60~80 DEG C, adds cinnamic acid monoglyceride, crosslinking agent, it is warming up to 100~
3~6h of reaction is carried out at 105 DEG C；
（3）After the completion of reaction, 85~90 DEG C are cooled to, adds fumaric acid, nano-titanium dioxide, nano silver, catalyst and breast
Agent, is gone out the gas displacement in reaction kettle using hydrogen, and boosts to 1.3~1.6MPa, and 3h, cooling are stirred with 500r/min
To room temperature, discharging, collects out material, spare；
（4）Magnesium alloy is fully immersed in 1.3mol/L citric acid solutions and soaks 50min, takes out the magnesium alloy of immersion, is used
Water washing Mg alloy surface to cleaning solution is in neutrality, and is air-dried using nitrogen, obtains pretreatment magnesium alloy；
（5）Pretreatment magnesium alloy is put into container, add it is spare go out material, dipping pretreatment 4~6cm of magnesium alloy, 8~
2~4h of energization is carried out at 10 DEG C to container, holding electric current is 90~100A, after to be energised, takes out magnesium alloy, air-dries, obtain
Magnesium alloy substrate；
（6）It is 9 in mass ratio：1~3：6, isopropanol, aminopropyl end-blocking dimethyl silicone polymer and magnesium alloy substrate are put into appearance
In device, 4h is stood at 90 DEG C, takes out magnesium alloy substrate, is air-dried, up to corrosion resistance magnesium alloy super-hydrophobic surface.
Embodiment 1
Catalyst is platinum catalyst（Tianjin Surfychem T＆D Co., Ltd.）.
Crosslinking agent is cumyl peroxide.
Emulsifying agent is phenethyl phenol polyethenoxy ether.
A kind of preparation method of corrosion resistance magnesium alloy super-hydrophobic surface, the preparation method include the following steps：
（1）Count in parts by weight, take 85 parts of acetone, 48 parts of polyoxypropyleneglycols, 28 parts of toluene di-isocyanate(TDI)s, 14 parts of dihydroxies
Methylpropanoic acid, 12 parts of lauric monoglycerides, 10 parts of fumaric acid, 9 parts of nano-titanium dioxides, 4 parts of catalyst, 4 parts of crosslinking agents, 2
Part nano silver and 2 parts of emulsifying agents；
（2）Acetone, polyoxypropyleneglycol, toluene di-isocyanate(TDI), dihydromethyl propionic acid are put into reaction kettle first, used
Nitrogen is protected, and preheating 48min is carried out at 70 DEG C, adds cinnamic acid monoglyceride, crosslinking agent, is warming up at 103 DEG C and is carried out instead
Answer 5h；
（3）After the completion of reaction, 88 DEG C are cooled to, adds fumaric acid, nano-titanium dioxide, nano silver, catalyst and emulsifying agent,
The gas displacement in reaction kettle is gone out using hydrogen, and boosts to 1.5MPa, 3h is stirred with 500r/min, is cooled to room temperature, goes out
Material, collects out material, spare；
（4）Magnesium alloy is fully immersed in 1.3mol/L citric acid solutions and soaks 50min, takes out the magnesium alloy of immersion, is used
Water washing Mg alloy surface to cleaning solution is in neutrality, and is air-dried using nitrogen, obtains pretreatment magnesium alloy；
（5）Will pretreatment magnesium alloy be put into container, add it is spare go out material, dipping pretreatment magnesium alloy 5cm, at 9 DEG C
Energization 3h is carried out to container, holding electric current is 95mA, after to be energised, takes out magnesium alloy, air-dries, obtain magnesium alloy substrate；
（6）It is 9 in mass ratio：2：6, isopropanol, aminopropyl end-blocking dimethyl silicone polymer and magnesium alloy substrate are put into container
In, 4h is stood at 90 DEG C, takes out magnesium alloy substrate, is air-dried, up to corrosion resistance magnesium alloy super-hydrophobic surface.
Embodiment 2
Catalyst is platinum catalyst（Tianjin Surfychem T＆D Co., Ltd.）.
Crosslinking agent is benzoyl peroxide.
Emulsifying agent is phenethyl phenol polyethenoxy ether.
A kind of preparation method of corrosion resistance magnesium alloy super-hydrophobic surface, the preparation method include the following steps：
（1）Count in parts by weight, take 90 parts of acetone, 50 parts of polyoxypropyleneglycols, 30 parts of toluene di-isocyanate(TDI)s, 15 parts of dihydroxies
Methylpropanoic acid, 13 parts of lauric monoglycerides, 11 parts of fumaric acid, 10 parts of nano-titanium dioxides, 5 parts of catalyst, 5 parts of crosslinking agents, 3
Part nano silver and 3 parts of emulsifying agents；
（2）Acetone, polyoxypropyleneglycol, toluene di-isocyanate(TDI), dihydromethyl propionic acid are put into reaction kettle first, used
Nitrogen is protected, and preheating 50min is carried out at 80 DEG C, adds cinnamic acid monoglyceride, crosslinking agent, is warming up at 105 DEG C and is carried out instead
Answer 6h；
（3）After the completion of reaction, 90 DEG C are cooled to, adds fumaric acid, nano-titanium dioxide, nano silver, catalyst and emulsifying agent,
The gas displacement in reaction kettle is gone out using hydrogen, and boosts to 1.6MPa, 3h is stirred with 500r/min, is cooled to room temperature, goes out
Material, collects out material, spare；
（4）Magnesium alloy is fully immersed in 1.3mol/L citric acid solutions and soaks 50min, takes out the magnesium alloy of immersion, is used
Water washing Mg alloy surface to cleaning solution is in neutrality, and is air-dried using nitrogen, obtains pretreatment magnesium alloy；
（5）Will pretreatment magnesium alloy be put into container, add it is spare go out material, dipping pretreatment magnesium alloy 6cm, at 10 DEG C
Energization 4h is carried out to container, holding electric current is 100mA, after to be energised, takes out magnesium alloy, air-dries, obtain magnesium alloy substrate；
（6）It is 9 in mass ratio：3：6, isopropanol, aminopropyl end-blocking dimethyl silicone polymer and magnesium alloy substrate are put into container
In, 4h is stood at 90 DEG C, takes out magnesium alloy substrate, is air-dried, up to corrosion resistance magnesium alloy super-hydrophobic surface.
Embodiment 3
Catalyst is palladium carbon catalyst（Chemical Co., Ltd. is reached in Shaanxi）.
Crosslinking agent is cumyl peroxide.
Emulsifying agent is butyl phenol polyethenoxy ether.
A kind of preparation method of corrosion resistance magnesium alloy super-hydrophobic surface, the preparation method include the following steps：
（1）Count in parts by weight, take 80 parts of acetone, 45 parts of polyoxypropyleneglycols, 25 parts of toluene di-isocyanate(TDI)s, 13 parts of dihydroxies
Methylpropanoic acid, 10 parts of lauric monoglycerides, 9 parts of fumaric acid, 8 parts of nano-titanium dioxides, 3 parts of catalyst, 2 parts of crosslinking agents, 1 part
Nano silver and 1 part of emulsifying agent；
（2）Acetone, polyoxypropyleneglycol, toluene di-isocyanate(TDI), dihydromethyl propionic acid are put into reaction kettle first, used
Nitrogen is protected, and preheating 45min is carried out at 60 DEG C, adds cinnamic acid monoglyceride, crosslinking agent, is warming up at 100 DEG C and is carried out instead
Answer 3h；
（3）After the completion of reaction, 85 DEG C are cooled to, adds fumaric acid, nano-titanium dioxide, nano silver, catalyst and emulsifying agent,
The gas displacement in reaction kettle is gone out using hydrogen, and boosts to 1.3MPa, 3h is stirred with 500r/min, is cooled to room temperature, goes out
Material, collects out material, spare；
（4）Magnesium alloy is fully immersed in 1.3mol/L citric acid solutions and soaks 50min, takes out the magnesium alloy of immersion, is used
Water washing Mg alloy surface to cleaning solution is in neutrality, and is air-dried using nitrogen, obtains pretreatment magnesium alloy；
（5）Will pretreatment magnesium alloy be put into container, add it is spare go out material, dipping pretreatment magnesium alloy 4cm, at 8 DEG C
Energization 2h is carried out to container, holding electric current is 90mA, after to be energised, takes out magnesium alloy, air-dries, obtain magnesium alloy substrate；
（6）It is 9 in mass ratio：1：6, isopropanol, aminopropyl end-blocking dimethyl silicone polymer and magnesium alloy substrate are put into container
In, 4h is stood at 90 DEG C, takes out magnesium alloy substrate, is air-dried, up to corrosion resistance magnesium alloy super-hydrophobic surface.
Comparative example：The magnesium alloy super-hydrophobic surface of Jiangsu metal material Co., Ltd production.
Method：The magnesium alloy super-hydrophobic surface for the embodiment of size such as taking to be prepared with comparative example, is immersed in brine
8h, detects its rate of corrosion.
The specific detection case of magnesium alloy hydrophobic surface such as table 1
Table 1
| Detection project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
| Rate of corrosion（%） | 39 | 33 | 25 | 60 |
It is short that the present invention prepares magnesium alloy hydrophobic surface preparation time, and without using strong acid and strong base, therefore surrounding environment will not be made
Into pollution.
From the foregoing, it will be observed that the present invention is a kind of preparation method of safe and efficient magnesium alloy hydrophobic surface, it is worthy to be popularized and makes
With.
Claims (5)
1. a kind of preparation method of corrosion resistance magnesium alloy super-hydrophobic surface, it is characterised in that the preparation method includes following step
Suddenly：
（1）Count in parts by weight, take 80~90 parts of acetone, 45~50 parts of polyoxypropyleneglycols, 25~30 parts of toluene diisocyanates
Acid esters, 13~15 parts of dihydromethyl propionic acids, 10~13 parts of lauric monoglycerides, 9~11 parts of fumaric acid, 8~10 parts of nanometers two
Titanium oxide, 3~5 parts of catalyst, 2~5 parts of crosslinking agents, 1~3 part of nano silver and 1~3 part of emulsifying agent；
（2）Acetone, polyoxypropyleneglycol, toluene di-isocyanate(TDI), dihydromethyl propionic acid are put into reaction kettle first, used
Nitrogen protect, preheated at 60~80 DEG C, add cinnamic acid monoglyceride, crosslinking agent, be warming up at 100~105 DEG C into
Row reaction；
（3）After the completion of reaction, 85~90 DEG C are cooled to, adds fumaric acid, nano-titanium dioxide, nano silver, catalyst and breast
Agent, is gone out the gas displacement in reaction kettle using hydrogen, and boosts to 1.3~1.6MPa, and stirring, is cooled to room temperature, and is discharged,
Material is collected out, it is spare；
（4）Magnesium alloy is put into citric acid solution and is soaked, takes out the magnesium alloy of immersion, using water washing Mg alloy surface to washing
Wash liquid to be in neutrality, air-dried using nitrogen, obtain pretreatment magnesium alloy；
（5）Pretreatment magnesium alloy is put into container, add it is spare go out material, dipping pretreatment 4~6cm of magnesium alloy, 8~
It is powered at 10 DEG C to container, after to be energised, takes out magnesium alloy, air-dry, obtain magnesium alloy substrate；
（6）Isopropanol, aminopropyl end-blocking dimethyl silicone polymer and magnesium alloy substrate are put into container, stood at 90 DEG C,
Magnesium alloy substrate is taken out, is air-dried, up to corrosion resistance magnesium alloy super-hydrophobic surface.
2. the preparation method of corrosion resistance magnesium alloy super-hydrophobic surface according to claim 1, it is characterised in that described to urge
Agent is any one in palladium carbon catalyst, platinum catalyst.
3. the preparation method of corrosion resistance magnesium alloy super-hydrophobic surface according to claim 1, it is characterised in that the friendship
Connection agent is any one in cumyl peroxide, benzoyl peroxide.
4. the preparation method of corrosion resistance magnesium alloy super-hydrophobic surface according to claim 1, it is characterised in that the breast
Agent is any one in butyl phenol polyethenoxy ether, phenethyl phenol polyethenoxy ether.
5. the preparation method of corrosion resistance magnesium alloy super-hydrophobic surface according to claim 1, it is characterised in that the step
Suddenly（6）Middle isopropanol, aminopropyl end-blocking dimethyl silicone polymer and magnesium alloy substrate quality ratio are 9：1~3：6.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110055524A (en) * | 2019-04-25 | 2019-07-26 | 西南交通大学 | A kind of bio-medical mg-based material surface can bioid hydrophobically modified layer preparation method |
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| CN101469425A (en) * | 2007-12-25 | 2009-07-01 | 中国科学院兰州化学物理研究所 | Method for fabricating magnesium alloy super-hydrophobic surface |
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| CN102409379A (en) * | 2011-11-08 | 2012-04-11 | 大连理工大学 | Method for preparing super-hydrophobic surface of magnesium alloy matrix by using primary battery method |
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| CN110055524A (en) * | 2019-04-25 | 2019-07-26 | 西南交通大学 | A kind of bio-medical mg-based material surface can bioid hydrophobically modified layer preparation method |
| CN110055524B (en) * | 2019-04-25 | 2020-10-30 | 西南交通大学 | Preparation method of bio-medical hydrophobic modified layer on magnesium-based material surface |
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