CN101824620A - Preparation method of superhydrophobic coating on magnesium alloy surface - Google Patents
Preparation method of superhydrophobic coating on magnesium alloy surface Download PDFInfo
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- CN101824620A CN101824620A CN 201010165310 CN201010165310A CN101824620A CN 101824620 A CN101824620 A CN 101824620A CN 201010165310 CN201010165310 CN 201010165310 CN 201010165310 A CN201010165310 A CN 201010165310A CN 101824620 A CN101824620 A CN 101824620A
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Abstract
The invention relates to a preparation method of a superhydrophobic coating on a magnesium alloy surface, which belongs to the magnesium alloy surface treatment technology, and comprises the following steps that: a magnesium alloy sample is sequentially cleaned by deionized water and acetone under an ultrasonic condition, showered by pure water, soaked into chemical etching solution to be treated for 2 to 5min at room temperature, cleaned under the ultrasonic condition and dried for standby use; then low-surface energy substance is coated on the surface of the sample; and finally the finished sample is dried, and the superhydrophobic coating on the magnesium alloy surface is obtained. The magnesium alloy surface treated through the method has excellent hydrophobic nature, so that the contact angle of the water and the surface can reach about 157 degrees, and the anti-corrosive performance of the prepared magnesium alloy superhydrophobic coating is improved. The method has the advantages of simple process, low cost and environmental protection.
Description
Technical field
The present invention relates on metallic substrate surface, construct the method for new texture, be specifically related to a kind of method for preparing super-hydrophobic coat at Mg alloy surface.
Background technology
Super-hydrophobic coat has unique surface property, as self-cleaning, didirtresistance, hydrophobicity etc.Super-hydrophobic coat is used for geographic satellite antenna of high snowfall or outdoor label plate, can prevent that the signal interruption or the outward appearance that cause because of accumulated snow are fuzzy; Super-hydrophobic coat is used for metallic substance, the effect that can play automatically cleaning, inhibition surface corrosion and surface oxidation and reduce rubbing factor (is lubricant with water); Super-hydrophobic coat is used for the shell of boats and ships, naval vessels or the inwall of pipeline, can reduce the friction resistance between they and the current; Super-hydrophobic coat is used for miniature marine communication means, can make it have superpower carrying capacity.
The density of magnesium alloy is about 1.3～1.9g/cm
3, lighter by 30%～50% than aluminium alloy, lighter more than 70% than iron and steel, and have high specific tenacity and specific rigidity, be easy to advantages such as forming process and mechanical workout and have broad application prospects.Yet the electropotential of magnesium is low, chemically reactive is high, and oxide film is loose, cause the corrosion resisting property of magnesium alloy relatively poor, particularly in the atmosphere and marine atmosphere of malaria, sulfur-bearing, the magnesium alloy component etching problem is more apparent serious, has greatly limited the widespread use of magnesium alloy in the engineering field.How to enlarge the application of magnesium alloy in industry, enjoy people to pay close attention to.Prevent that the corrosion of magnesium alloy component in humidity or liquid medium from can consider aspect two: the one, improve the corrosion resisting property of magnesium alloy component itself by the surface-treated method; The 2nd, can attempt at the Mg alloy surface constructing super-drainage structure.The corrosion of magnesium alloy mainly is owing between magnesium alloy and medium on every side such as damp atmosphere, water, the electrolytic solution etc. chemistry taking place or electrochemical action has generated metal oxide, oxyhydroxide and mixture etc., thereby cause the corrosion failure of magnesium alloy, by reducing the direct corrosion resisting property that can improve magnesium alloy that contacts of magnesium alloy and aqueous vapor medium.Can play at the surface construction super-drainage structure and to reduce the chance that magnesium alloy and media such as water, solution directly contact, thereby improve its corrosion resisting property.Therefore, function modified by Mg alloy surface, can improve the scope of application of magnesium alloy at industrial circle.
At present, method at the super-hydrophobic processing of Mg alloy surface is seldom reported, Chinese patent (CN101469425A) has been announced a kind of little/nano porous structure that adopts micro-arc oxidation process to construct roughening at sample surfaces, handle through acrylic acid solution then, in its surperficial spin coating vinyldimethicone, obtain magnesium alloy super-hydrophobic surface at last, this method micro-arc oxidation process and annealing more complicated, the condition harshness is difficult for scale operation; The chemistry LiuKesong of institute of the Chinese Academy of Sciences etc. are at Applied Physics Letters, 2008,183103-1-3 reported a kind of utilize chemical etching and surperficial self-assembly fluorizated method in the magnesium lithium alloy surface preparation super hydrophobic surface, yet the process of surface fluorination is consuming time long, test button need be immersed in the spirituous solution of 1.0wt% ten trifluoro octyltri-ethoxysilane, take out after soaking 12h under the room temperature, in baking oven, heat 2h again under 100 ℃, the time of this technology fluoridation is long, efficiency ratio is lower, industrial production utilization and popularization are comparatively difficult on a large scale for this reason, and adopt the HCl processing to make the metallic surface get rusty than being easier to.The preparation method that Chinese patent (CN101476142A) adopts chemical etching to combine with organic film plating prepares super-hydrophobic organic nano film in magnesium, steel or stainless steel metallic surface.This method organic film plating process complexity, wayward, be difficult to realize scale operation.
Summary of the invention
Purpose of the present invention is exactly to provide a kind of novel method for preparing super-hydrophobic coat at Mg alloy surface in order to overcome above-mentioned the deficiencies in the prior art, this method cost is low, technology is simple, and controllability is relatively good, is easy to produce in batches, the time ratio of finishing is shorter, the efficient height;
The preparation method of a kind of superhydrophobic coating on magnesium alloy surface involved in the present invention, step is as follows:
(1) clean: the magnesium alloy sample of preparing is put into deionized water for ultrasonic clean, to remove particle such as surface dirt; Ultrasonic cleaning in acetone then is to remove surface and oil contaminant; Use pure water drip washing clean afterwards again;
(2) chemical corrosion: will handle 2～5 minutes in the cleaned magnesium alloy immersion chemical corrosion liquid, treatment temp is a room temperature; Ultrasonic cleaning after handling dries up, and puts into baking oven and toasts, and is stand-by; Described chemical corrosion liquid is by 2～5wt%HNO
3Form with the aqueous solution of the nitrate of 0.5～2g/L;
(3) hydrophobization is handled: will put into hydrophobic treatment liquid through the magnesium alloy sample after the chemical corrosion and soak 0.5～2h, take out, dry with putting into baking oven after the ethanol drip washing, can obtain the magnesium alloy super-hydrophobic coating, described hydrophobic treatment liquid is the ethanolic soln of 2～10wt% silane.
The present invention has the following advantages compared with prior art: the present invention adopts the method for chemical etching to compare additive method does not need expensive equipment, and cost is low, controllability is relatively good, is easy to produce in batches; The time ratio of finishing is shorter, the efficient height; Prepared magnesium alloy super-hydrophobic coating has little/nano porous structure, and this surface has good super-hydrophobicity, and contact angle on average reaches 155 °.
Description of drawings
Fig. 1:, (a) be the SEM photo of low multiple with the SEM photo of the different amplification of the superhydrophobic coating on magnesium alloy surface of the inventive method preparation; (b) be the SEM photo of high multiple
Fig. 2: with the contact angle photo of the superhydrophobic coating on magnesium alloy surface of the inventive method preparation: a, b) be untreated AZ31 matrix; C, d) be the AZ31 super hydrophobic surface after chemical corrosion and the finishing
Fig. 3: with the AZ31 magnesium alloy super-hydrophobic coating sample and the untreated sample Tafel curve of the inventive method preparation
The contact angle photo of Fig. 4: embodiment 2.
Embodiment
Further specify as follows below in conjunction with drawings and Examples to the preparation method of a kind of superhydrophobic coating on magnesium alloy surface involved in the present invention:
Test materials AZ31 magnesium alloy, size is the bulk of 20mm * 15mm * 1mm, the concrete operations step is as follows:
(1) clean: the magnesium alloy sample of preparing is put into deionized water for ultrasonic clean 10min, to remove particle such as surface dirt; Ultrasonic cleaning 10min in acetone then is to remove surface and oil contaminant; Use pure water drip washing clean afterwards again;
(2) chemical corrosion: cleaned magnesium alloy sample immersed in the chemical corrosion liquid that contains 5wt% nitric acid and 1.0g/L Gerhardite handled 5 minutes, treatment temp is a room temperature; Use pure water rinsing after handling, ultrasonic cleaning 5min dries up, and puts into 150 ℃ of bakings of baking oven 10min, and is stand-by;
(3) hydrophobization is handled: will put into the ethanolic soln that contains 2wt% n-octyl triethoxyl silane through the magnesium alloy sample after the chemical corrosion and soak 0.5h, and take out, and with putting into 150 ℃ of bakings of baking oven 1h after the ethanol drip washing, can obtain the magnesium alloy super-hydrophobic coating.
Method for testing performance is as follows: with the variable vacuum scanning electron microscope analysis of the Tescan coating pattern of being furnished with the INCA350X-gamma spectrometer; Measure contact angle with contact angle measurement; Estimate the corrosion resisting property of coating again with the Tafel curve, tester is the micro electronmechanical chemical analysis system of LK98B II (Tianjin Lanllike Chemistry Electronic High-tech Co., Ltd.), make reference electrode with mercurous chloride electrode, platinum electrode is made supporting electrode, working electrode is a sample, a face that stays 1 * 1cm is at 3.5% NaCl solution, and its lap is with the sealing of AB glue.0.0100 volt/second of sweep velocity, scanning accuracy 10mA.Detected result as shown in Figure 1-Figure 3.
Wherein Fig. 1 is that the Mg alloy surface structure that is prepared as can be known by picture is little/nano porous structure with the SEM photo of the different amplification of the AZ31 superhydrophobic coating on magnesium alloy surface of present embodiment preparation.Fig. 2 is that the contact angle that is visible as untreated AZ31 matrix is 47 ° with the contact angle photo of the AZ31 superhydrophobic coating on magnesium alloy surface of present embodiment preparation, and the AZ31 super hydrophobic surface contact angle after chemical corrosion and the finishing is 160 °.Fig. 3 is AZ31 magnesium alloy super-hydrophobic coating sample and the untreated sample Tafel curve with the present embodiment preparation.
Static contact angle is up to 160 ° in its surface for water droplet, and roll angle embodies excellent ultra-hydrophobicity less than 10 °.Electrochemical results shows, the corrosion potential that contains super-hydrophobic coat magnesium alloy sample is shuffled, become-1.17V by-1.43V, and corrosion current compares with untreated samples and reduce by 2 orders of magnitude, illustrate that the existence of super-hydrophobic coat system can improve the corrosion resistance nature of magnesium alloy.Contact angle result and patent (CN101007304A) are approaching in result's (159.7 ° of average contact angles) that aluminum alloy surface prepares super-hydrophobic coat with similarity method; The contact angle result is slightly higher than patent (CN101469425A) is modified the magnesium alloy super-hydrophobic surface that obtains with the differential arc oxidation mating surface result's (155 ° of average contact angles).
Test materials AZ31 magnesium alloy, size is the bulk of 20mm * 15mm * 1mm, the concrete operations step is as follows:
(1) clean: the magnesium alloy sample of preparing is put into deionized water for ultrasonic clean 10min, to remove particle such as surface dirt; Ultrasonic cleaning 10min in acetone then is to remove surface and oil contaminant; Use pure water drip washing clean afterwards again;
(2) chemical corrosion: cleaned magnesium alloy sample immersed in the chemical corrosion liquid that contains 2wt% nitric acid and 1.0g/L three nitric hydrate nickel handled 2-5 minute, treatment temp is a room temperature; Use pure water rinsing after handling, ultrasonic cleaning 5min dries up, and puts into 150 ℃ of bakings of baking oven 10min, and is stand-by;
(3) hydrophobization is handled: will put into the ethanolic soln that contains 2wt% 17 fluorine certain herbaceous plants with big flowers ethyl triethoxy silicane alkane through the magnesium alloy sample after the chemical corrosion and soak 2h, take out, with putting into 150 ℃ of bakings of baking oven 1h after the ethanol drip washing, can obtain the magnesium alloy super-hydrophobic coating.
The pattern of the super-hydrophobic coat that present embodiment obtains, the Tafel curve of Electrochemical Detection is close with embodiment 1, no longer provides with graphics mode.The contact angle detection result of the super-hydrophobic coat that present embodiment obtains as shown in Figure 4, visible water droplet static contact angle in its surface reaches 154 °, roll angle embodies excellent ultra-hydrophobicity less than 10 °.Electrochemical results shows, the corrosion potential that contains super-hydrophobic coat magnesium alloy sample is shuffled, become-1.18V by-1.43V, and corrosion current compares with untreated samples and reduce by 2 orders of magnitude, illustrate that the existence of super-hydrophobic coat system can improve the corrosion resistance nature of magnesium alloy.(CN101469425A) is approaching for contact angle result and patent.
Claims (3)
1. the preparation method of a superhydrophobic coating on magnesium alloy surface is characterized in that step is as follows:
(1) clean: the magnesium alloy sample of preparing is put into deionized water for ultrasonic clean, to remove particle such as surface dirt; Ultrasonic cleaning in acetone then is to remove surface and oil contaminant; Use pure water drip washing clean afterwards again;
(2) chemical corrosion: will handle 2～5 minutes in the cleaned magnesium alloy immersion chemical corrosion liquid, treatment temp is a room temperature; Ultrasonic cleaning after handling dries up, and puts into baking oven and toasts, and is stand-by;
(3) hydrophobization is handled: will put into hydrophobic treatment liquid through the magnesium alloy sample after the chemical corrosion and soak 0.5～2h, take out, and dry with putting into baking oven after the ethanol drip washing, can obtain the magnesium alloy super-hydrophobic coating.
2. method according to claim 1 is characterized in that described chemical corrosion liquid is by 2～5wt%HNO
3Form with the aqueous solution of the nitrate of 0.5～2g/L.
3. method according to claim 1 and 2 is characterized in that described hydrophobic treatment liquid is the ethanolic soln of 2～10wt% silane.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103205789A (en) * | 2013-03-15 | 2013-07-17 | 哈尔滨工程大学 | Method for preparing magnesium-lithium alloy surface micro-arc oxidation self-assembling super hydrophobic composite coating |
| CN104213112A (en) * | 2014-09-09 | 2014-12-17 | 重庆大学 | Method for manufacturing metal surface self-cleaning high-protection film |
| CN104846376A (en) * | 2015-05-29 | 2015-08-19 | 清华大学 | Preparation method of metal-based super-hydrophobic surface |
| CN107616826A (en) * | 2017-09-27 | 2018-01-23 | 吉林大学 | A kind of preparation method of the medical super-hydrophobic puncture needle of lower resistance |
| CN107916421A (en) * | 2017-11-13 | 2018-04-17 | 常州麒通国际贸易有限公司 | A kind of preparation method of corrosion resistance magnesium alloy super-hydrophobic surface |
| CN108342742A (en) * | 2018-05-11 | 2018-07-31 | 北京石油化工学院 | A kind of magnesium lithium alloy surface pre-treatment |
| CN112175430A (en) * | 2020-09-28 | 2021-01-05 | 榆林学院 | Preparation method of copper myristate super-hydrophobic coating |
| CN113897616A (en) * | 2021-10-18 | 2022-01-07 | 南京理工大学 | Magnesium alloy surface anticorrosion treatment process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN100558472C (en) * | 2007-01-12 | 2009-11-11 | 华南理工大学 | The preparation method of aluminium and aluminium alloy super hydrophobic surface |
-
2010
- 2010-05-07 CN CN 201010165310 patent/CN101824620A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100558472C (en) * | 2007-01-12 | 2009-11-11 | 华南理工大学 | The preparation method of aluminium and aluminium alloy super hydrophobic surface |
| 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 |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103205789A (en) * | 2013-03-15 | 2013-07-17 | 哈尔滨工程大学 | Method for preparing magnesium-lithium alloy surface micro-arc oxidation self-assembling super hydrophobic composite coating |
| CN104213112A (en) * | 2014-09-09 | 2014-12-17 | 重庆大学 | Method for manufacturing metal surface self-cleaning high-protection film |
| CN104213112B (en) * | 2014-09-09 | 2016-04-06 | 重庆大学 | The preparation method of a kind of metallic surface automatically cleaning, high protection rete |
| CN104846376A (en) * | 2015-05-29 | 2015-08-19 | 清华大学 | Preparation method of metal-based super-hydrophobic surface |
| CN107616826A (en) * | 2017-09-27 | 2018-01-23 | 吉林大学 | A kind of preparation method of the medical super-hydrophobic puncture needle of lower resistance |
| CN107916421A (en) * | 2017-11-13 | 2018-04-17 | 常州麒通国际贸易有限公司 | A kind of preparation method of corrosion resistance magnesium alloy super-hydrophobic surface |
| CN108342742A (en) * | 2018-05-11 | 2018-07-31 | 北京石油化工学院 | A kind of magnesium lithium alloy surface pre-treatment |
| CN112175430A (en) * | 2020-09-28 | 2021-01-05 | 榆林学院 | Preparation method of copper myristate super-hydrophobic coating |
| CN113897616A (en) * | 2021-10-18 | 2022-01-07 | 南京理工大学 | Magnesium alloy surface anticorrosion treatment process |
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Open date: 20100908 |