CN109735887A - A kind of preparation method of magnesium alloy magnesium manganese hydrotalcite/differential arc oxidation anti-corrosion coating - Google Patents
A kind of preparation method of magnesium alloy magnesium manganese hydrotalcite/differential arc oxidation anti-corrosion coating Download PDFInfo
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- CN109735887A CN109735887A CN201910215153.0A CN201910215153A CN109735887A CN 109735887 A CN109735887 A CN 109735887A CN 201910215153 A CN201910215153 A CN 201910215153A CN 109735887 A CN109735887 A CN 109735887A
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Abstract
The present invention is prepared for a kind of coating of magnesium alloy surface of excellent corrosion resistance.The present invention carries out differential arc oxidation to the magnesium alloy sample of pre-treatment in advance, and then differential arc oxidation sample is placed in deionized water again and carries out hydro-thermal reaction, finally forms magnesium manganese hydrotalcite/differential arc oxidation coating in alloy surface.The present invention prepares resulting coating with lower corrosion electric current density, can not only effectively repair the hole and crackle of differential arc oxidation layer, and can adsorb the anion in etchant solution well, effectively improve the corrosion resistance of alloy.Present invention process is simple, and operation is easy, at low cost, has the feasibility being widely popularized.
Description
Technical field
The present invention relates to magnesium alloy surface treatments, and in particular to a kind of magnesium alloy magnesium manganese hydrotalcite/differential arc oxidation is resistance to
The preparation method of erosion resisting coating.
Background technique
Magnesium and its alloy have good mechanical and physical property, and such as specific strength height, shock resistance, damping property be good, electromagnetic screen
Good, good biocompatibility of covering property etc., thus be the ideal material of the application fields such as automotive light weight technology, space flight and aviation and electronics industry
Material.But the disadvantage is that corrosion resistance is poor, thus can not large-scale use, so industrial usually carry out at surface magnesium alloy
Reason is to improve its corrosion resistance.
Mg alloy surface processing such as chemical oxidation, anodic oxidation, metal coating can improve the corrosion resistance of alloy, still
There is also pollution environment, it is at high cost the problems such as, be difficult mass production.Differential arc oxidation has technically simple, efficient pollution-free excellent
Point can form fine and close ceramic layer in alloy surface.Its principle is to be put into impulse electric field ring for magnesium alloy sample as anode
In the electrolyte in border, specimen surface oxidation film is breakdown under high pressure and generates a large amount of micro-arc discharges, and discharge process generates micro-
Area's high temperature and pressure makes magnesium atom react to form magnesia ceramics coating with the oxonium ion in electrolyte.But in micro-arc oxidation process
Easily form hole, crackle etc., it is therefore desirable to which pre-treatment or post-processing improve the corrosion resistance of alloy to reduce defect.
Hydrotalcite is a kind of anion intercalated type lamellar compound, also known as laminated dihydroxy composite metal hydroxide,
Its chemical general formula is [M2+ 1-xM3+ x(OH)2]x+Am- x/m•nH2O, wherein M2+And M3+Indicate the metal cation of main layer board, Am-
For tradable interlayer object anion.Hydrotalcite has because of the adjustability of its Nomenclature Composition and Structure of Complexes, the interchangeability of interlayer ion
There are a series of excellent physical and chemical performances, such as good catalytic, anti-flammability, magnetism, this makes hydrotalcite-like material exist
The fields such as catalytic adsorption, magnetics, fire retardant, anti-corrosion of metal have broad application prospects.The good ion of hydrotalcite coating
Exchange capacity makes it possible to capture by ion exchange and limits Cl-, to effectively inhibit Cl-Corrosion function.
In recent years, about aluminum alloy differential arc oxidation/hydrotalcite coating existing research is prepared, people are in aluminum alloy differential arc oxidation
Layer surface prepares hydrotalcite coating, and the corrosion of alloy can be effectively relieved.However related magnesium alloy differential arc oxidation/hydrotalcite coating
Research it is few and preparation process is complicated, need to additionally introduce divalent ion, increase cost and process flow.
There are a large amount of crackle and hole, these coarse crackles and holes easily to constitute for the differential arc oxidation coating of magnesium alloy
Etching channels, to accelerate the corrosion of alloy.Differential arc oxidation sample is subjected to hydro-thermal process in a kettle, to obtain the differential of the arc
Oxidation/hydrotalcite coating.The preparation process directlys adopt deionized water as reaction solution and carries out hydro-thermal process, without configuring hydro-thermal
Reaction mixture introduces trivalent ion, synthesizes neatly with Manganic ion by the divalent magnesium ion of differential arc oxidation layer itself
Stone, process simply and readily operate, and the corrosion of magnesium alloy can be effectively relieved in resulting coating.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of magnesium alloy magnesium manganese hydrotalcite/differential arc oxidation anti-corrosion coating,
Deionized water is directlyed adopt as reaction solution and carries out hydro-thermal process, without configuring hydro-thermal reaction mixed solution, introduces trivalent ion,
By the divalent magnesium ion and Manganic ion synthetic hydrotalcite of differential arc oxidation layer itself, process is simply and readily operated, gained
Coating the corrosion of magnesium alloy can be effectively relieved.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method of magnesium alloy magnesium manganese hydrotalcite/differential arc oxidation anti-corrosion coating, comprising the following steps:
(1) pre-treatment: magnesium alloy sample surface grinding is smooth, it is then washed and is dried；
(2) magnesium alloy differential arc oxidation: the magnesium alloy sample after drying is subjected to differential arc oxidation using constant current mode, obtains manganese-
Differential arc oxidation sample；
(3) hydro-thermal reaction: manganese-differential arc oxidation sample that step (2) obtain being placed in deionized water and carries out hydro-thermal reaction, is prepared
Magnesium manganese hydrotalcite/differential arc oxidation coating out.
The electrolyte composition of step (2) described differential arc oxidation is as follows: sodium metasilicate 5-20g/L, potassium hydroxide 5-30g/L, fluorine
Change potassium 1-10g/L, potassium permanganate 0-2g/L.
The processing time of step (2) the constant current mode differential arc oxidation is 5-20min, frequency 600-800Hz.
The temperature of step (3) described hydro-thermal reaction is 100-150 DEG C, reaction time 1-30h.
Further, above-mentioned preparation method is applied in the preparation of anticorrosion magnesium alloy.
The present invention has the advantages that
(1) hydrotalcite is as novel inorganic functional material, due to the adjustability of its Nomenclature Composition and Structure of Complexes, with memory effect,
The characteristics such as interchangeability of thermal stability, interlayer anion, have a extensive future.
(2) present invention is prepared for magnesium manganese hydrotalcite/differential arc oxidation coating, the unique stratiform knot of hydrotalcite using hydro-thermal method
Structure effectively improves the corrosion resistance of differential arc oxidation alloy sample.
(3) the method for the present invention does not have to configuration hydro-thermal reaction mixed solution, and simple process is efficient and at low cost, environmentally friendly no dirt
Dye, and Corrosion Behaviors of Magnesium Alloys current density can be significantly reduced, widen the application range of magnesium alloy.
(4) magnesium manganese hydrotalcite/differential arc oxidation coating can effectively delay the corrosion rate of magnesium alloy, extend making for magnesium alloy
Use the service life.
(5) magnesium manganese hydrotalcite/differential arc oxidation coating has certain characterization of adsorption, can be used as absorbent coating use.
Detailed description of the invention
Fig. 1 is differential arc oxidation, manganese-differential arc oxidation and magnesium manganese hydrotalcite/differential arc oxidation coating XRD.
Fig. 2 is differential arc oxidation, and manganese-differential arc oxidation and magnesium manganese hydrotalcite/differential arc oxidation coating SEM scheme；Wherein (a) is the differential of the arc
Oxidation, (b) is manganese-differential arc oxidation, and (c-d) is magnesium manganese hydrotalcite/differential arc oxidation coating.
Fig. 3 is magnesium manganese hydrotalcite/differential arc oxidation coating EDS figure.
Fig. 4 is differential arc oxidation, manganese-differential arc oxidation and the dynamic polarization curve of magnesium manganese hydrotalcite/differential arc oxidation coating.
Specific embodiment
1 magnesium manganese hydrotalcite of embodiment/differential arc oxidation coating preparation method
(1) pre-treatment: magnesium alloy sample surface grinding is smooth, it is then washed and is dried；
(2) magnesium alloy differential arc oxidation: the magnesium alloy sample after drying is subjected to differential arc oxidation using constant current mode, handles the time
20min, frequency 800Hz obtain manganese-differential arc oxidation sample；The electrolyte composition of differential arc oxidation is as follows: sodium metasilicate 20g/L, hydrogen-oxygen
Change potassium 30g/L, potassium fluoride 10g/L, potassium permanganate 2g/L.
(3) hydro-thermal reaction: manganese-differential arc oxidation sample that step (2) obtain being placed in deionized water and carries out hydro-thermal reaction,
Reaction temperature is 120 DEG C, reaction time 15h, and magnesium manganese hydrotalcite/differential arc oxidation coating is prepared.
Embodiment 2
(1) pre-treatment: magnesium alloy sample surface grinding is smooth, it is then washed and is dried；
(2) magnesium alloy differential arc oxidation: the magnesium alloy sample after drying is subjected to differential arc oxidation using constant current mode, handles the time
5min, frequency 600Hz obtain manganese-differential arc oxidation sample；The electrolyte composition of differential arc oxidation is as follows: sodium metasilicate 5g/L, hydroxide
Potassium 5g/L, potassium fluoride 1g/L, potassium permanganate 1g/L.
(3) hydro-thermal reaction: manganese-differential arc oxidation sample that step (2) obtain being placed in deionized water and carries out hydro-thermal reaction,
Reaction temperature is 100 DEG C, reaction time 10h, and magnesium manganese hydrotalcite/differential arc oxidation coating is prepared.
Embodiment 3
(1) pre-treatment: magnesium alloy sample surface grinding is smooth, it is then washed and is dried；
(2) magnesium alloy differential arc oxidation: the magnesium alloy sample after drying is subjected to differential arc oxidation using constant current mode, handles the time
10min, frequency 700Hz obtain manganese-differential arc oxidation sample；The electrolyte composition of differential arc oxidation is as follows: sodium metasilicate 10g/L, hydrogen-oxygen
Change potassium 10g/L, potassium fluoride 5g/L, potassium permanganate 2g/L.
(3) hydro-thermal reaction: manganese-differential arc oxidation sample that step (2) obtain being placed in deionized water and carries out hydro-thermal reaction,
Reaction temperature is 120 DEG C, reaction time 15h, and magnesium manganese hydrotalcite/differential arc oxidation coating is prepared.
The preparation method of 1 differential arc oxidation coating of comparative example
(1) pre-treatment: magnesium alloy sample surface grinding is smooth, it is then washed and is dried；
(2) magnesium alloy sample after drying magnesium alloy differential arc oxidation: is subjected to differential arc oxidation, differential arc oxidation using constant current mode
Electrolyte composition it is as follows: sodium metasilicate 20g/L, potassium hydroxide 30g/L, potassium fluoride 10g/L；Handle time 20min, frequency
800Hz obtains differential arc oxidation sample.
2 manganese of comparative example-differential arc oxidation coating preparation method
(1) pre-treatment: magnesium alloy sample surface grinding is smooth, it is then washed and is dried；
(2) magnesium alloy sample after drying magnesium alloy differential arc oxidation: is subjected to differential arc oxidation, differential arc oxidation using constant current mode
Electrolyte composition it is as follows: sodium metasilicate 20g/L, potassium hydroxide 30g/L, potassium fluoride 10g/L, potassium permanganate 2g/L；Handle the time
10min, frequency 800Hz obtain manganese-differential arc oxidation sample.
The coating that embodiment and comparative example is prepared carries out X-ray diffraction, analyzes its diffracting spectrum it is found that embodiment
There is the diffraction maximum of (003) and (006) crystal face of hydrotalcite in 1 magnesium manganese hydrotalcite/differential arc oxidation coating, shows differential arc oxidation
Specimen surface forms hydrotalcite coating (Fig. 1).
The coating that embodiment and comparative example is prepared carries out SEM characterization, as shown in Figure 2,1 magnesium alloy sample of comparative example
Fine and close coating is formd after carrying out differential arc oxidation, but there are the volcano shape holes for taking measurements greatly different, and are dispersed with
Apparent crackle, these cavities and crackle fast erosion channel easy to form, accelerate Mg alloy surface corrosion.Comparative example 2 is electrolysed
After adding potassium permanganate in liquid, there are more tiny holes in manganese-differential arc oxidation specimen surface, and pore quantity increases, and passes through
After hydro-thermal reaction (embodiment 1), magnesium manganese hydrotalcite/differential arc oxidation specimen surface forms lamellar hydrotalcite coating, hydrotalcite
Coating can effectively cover hole, while the special layer structure of hydrotalcite coating can be run through ion exchange and capture and limit
Chloride ion processed significantly reduces the corrosion rate of magnesium alloy.
Known to EDS map (Fig. 3), sample surfaces are mainly dispersed with by Mg, O, this is because alloy passes through differential arc oxidation
Rear surface forms fine and close MgO ceramic layer.Furthermore Al, Si, Mn are also evenly distributed in sample surfaces, and wherein Si is differential of the arc oxygen
It is introduced from electrolyte during change, the hydrotalcite of the formation such as Al, Mn homoepitaxial on differential arc oxidation layer effectively covers
Cap bore hole and crackle, and without destroying differential arc oxidation layer.
Embodiment and comparative example magnesium alloy differential arc oxidation, manganese-differential arc oxidation and magnesium manganese hydrotalcite/differential arc oxidation coating exist
Dynamic polarization curve in 3.5%wt sodium chloride solution is shown in Fig. 4.Corrosion electric current density in dynamic polarization curve, corrosion potential are weighing apparatuses
The corrosion proof major criterion of sample is measured, corrosion electric current density is smaller, and corrosion potential is higher, and the corrosion resistance of magnesium alloy is better.Such as
Shown in Fig. 4, formation manganese-differential arc oxidation coating corrosion potential is held essentially constant after adding potassium permanganate, while corrosion current
Increase, potassium permanganate is added under the conditions of showing current experiment, in electrolyte and is unfavorable for improving the corrosion resistance of alloy, but passes through water
After thermal response, magnesium manganese hydrotalcite/differential arc oxidation coating corrosion potential is constant, but its corrosion electric current density is then substantially reduced,
Show that magnesium manganese hydrotalcite/differential arc oxidation coating corrosion stability is apparently higher than differential arc oxidation coating, this is because magnesium manganese hydrotalcite covers
The hole of lid differential arc oxidation coating and crack, the effective infiltration for stopping chloride ion, while the peculiar property of hydrotalcite coating, i.e.,
With good ion exchangeable, chloride ion can be captured and be limited, therefore effectively delays the extent of corrosion of magnesium alloy.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (5)
1. a kind of preparation method of magnesium alloy magnesium manganese hydrotalcite/differential arc oxidation anti-corrosion coating, which is characterized in that including following step
It is rapid:
(1) pre-treatment: magnesium alloy sample surface grinding is smooth, it is then washed and is dried；
(2) magnesium alloy differential arc oxidation: the magnesium alloy sample after drying is subjected to differential arc oxidation using constant current mode, obtains manganese-
Differential arc oxidation sample；
(3) hydro-thermal reaction: manganese-differential arc oxidation sample that step (2) obtain being placed in deionized water and carries out hydro-thermal reaction, is prepared
Magnesium manganese hydrotalcite/differential arc oxidation coating out.
2. a kind of preparation method of magnesium alloy magnesium manganese hydrotalcite/differential arc oxidation anti-corrosion coating according to claim 1, feature
It is, the electrolyte composition of step (2) described differential arc oxidation is as follows: sodium metasilicate 5-20g/L, potassium hydroxide 5-30g/L, potassium fluoride
1-10g/L, potassium permanganate 0-2g/L.
3. a kind of preparation method of magnesium alloy magnesium manganese hydrotalcite/differential arc oxidation anti-corrosion coating according to claim 1, feature
It is, the processing time of step (2) the constant current mode differential arc oxidation is 5-20min, frequency 600-800Hz.
4. a kind of preparation method of magnesium alloy magnesium manganese hydrotalcite/differential arc oxidation anti-corrosion coating according to claim 1, feature
It is, the temperature of step (3) described hydro-thermal reaction is 100-150 DEG C, reaction time 1-30h.
5. a kind of application of preparation method as described in claim 1-4 is any in preparation anticorrosion magnesium alloy.
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| CN110424039A (en) * | 2019-09-16 | 2019-11-08 | 东北大学 | The preparation method of the anti-corrosion selfreparing differential arc oxidation coating of magnesium alloy based on hydrotalcite nano inhibition microcapsules |
| CN114262923A (en) * | 2020-09-16 | 2022-04-01 | 华中科技大学 | Magnesium alloy surface double-layer composite film, preparation method and application thereof |
| CN114657621A (en) * | 2020-12-24 | 2022-06-24 | 中国科学院上海硅酸盐研究所 | Method for improving corrosion resistance of micro-arc porous magnesium oxide coating on surface of magnesium alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114657621A (en) * | 2020-12-24 | 2022-06-24 | 中国科学院上海硅酸盐研究所 | Method for improving corrosion resistance of micro-arc porous magnesium oxide coating on surface of magnesium alloy |
| CN114657621B (en) * | 2020-12-24 | 2023-11-10 | 中国科学院上海硅酸盐研究所 | Method for improving corrosion resistance of micro-arc porous magnesium oxide coating on magnesium alloy surface |
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