CN108251839A - A kind of preparation method of magnesium nickel hydrotalcite/differential arc oxidation composite coating - Google Patents
A kind of preparation method of magnesium nickel hydrotalcite/differential arc oxidation composite coating Download PDFInfo
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- CN108251839A CN108251839A CN201810344032.1A CN201810344032A CN108251839A CN 108251839 A CN108251839 A CN 108251839A CN 201810344032 A CN201810344032 A CN 201810344032A CN 108251839 A CN108251839 A CN 108251839A
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- arc oxidation
- differential arc
- composite coating
- hydrotalcite
- magnesium
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
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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
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
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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
- C25D11/02—Anodisation
- C25D11/30—Anodisation of magnesium or alloys based thereon
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Abstract
The present invention is prepared for a kind of preparation method of magnesium nickel hydrotalcite/differential arc oxidation composite coating, is pretreated magnesium alloy first to be carried out differential arc oxidation, then through hydro-thermal reaction, so as to form magnesium nickel hydrotalcite coating on the surface of magnesium alloy differential arc oxidation layer.Magnesium nickel hydrotalcite/differential arc oxidation composite coating prepared by the present invention has high impedance modulus, can effectively improve the corrosion stability of Mg alloy surface.In addition, present invention process is simple, and it is easy to operate, it is at low cost, there is the feasibility being widely popularized.
Description
Technical field
The invention belongs to technical field of alloy material, and in particular to a kind of magnesium nickel hydrotalcite/differential arc oxidation composite coating
Preparation method.
Background technology
Magnesium and its alloy are and wide due to many excellent properties such as low-density, high intensity, good biocompatibilities
It is general to be applied to the fields such as automobile making, space flight and aviation.But magnesium alloy chemical activity is high, easily corrodes, limits magnesium alloy
Application industrially therefore, it is necessary to be modified to Mg alloy surface, improves the corrosion resistance of alloy.
Process for treating surface such as ultrasound assisted chemical plating, stannate conversion film, lanthanum conversion film etc. can effectively improve magnesium alloy
Corrosion resistance, or but these coatings are harmful or of high cost, be not suitable for being widely applied.Differential arc oxidation is a kind of new
Grain husk, the processing method of environmental protection are when the voltage of application is more than critical voltage, and Mg alloy surface generates high temperature, the height of moment
Pressure, matrix surface oxidation film is breakdown, a large amount of micro-arc discharge occurs, and regional area melts, and forms discharge channel, complicated electricity
Chemistry carries out in the channel, so as to generate the ceramic layer based on matrix oxide.But it can be formed in micro-arc oxidation process intrinsic
Defect such as volcano shape hole, crackle, is unfavorable for being further improved for alloy property, and hydrone and corrosive medium can be by lacking
It is trapped into alloy substrate, causes serious destruction.Therefore, it is necessary to by differential arc oxidation pre-treatment or post processing to reduce defect,
Further improve the corrosion-proof wear performance of alloy.
Hydrotalcite is a kind of typically anionic intercalation material, also known as laminated dihydroxy composite metal hydroxide,
It, with good ion-exchange capacity, is a kind of coating of environment friendly, in fields such as photoelectricity, medicament transport, anticorrosions
Application obtained the extensive concern of people.The ingredient of hydrotalcite coating is usually written as [M2+ 1-xM3+ x(OH)2]x+Am- x/m•nH2O,
Wherein, M2+And M3+Represent the metal cation of divalent and trivalent, Am-For tradable anion.The unique knot of hydrotalcite coating
Structure and ion-exchange capacity can adsorb the chlorion in corrosive liquid, improve the corrosion resistance of material.
By forming hydrotalcite coating at differential arc oxidization surface and its hole, differential arc oxidation sample can be effectively improved
Corrosion resistance.In recent years, existing research prepares neatly rock layers on aluminum alloy differential arc oxidation, forms super hydrophobic composite coating.
However, the composite coating that differential arc oxidation is combined with hydrotalcite is developed in few research on magnesium alloy.The present invention is existed using hydro-thermal method
Magnesium nickel hydrotalcite coating is formed on differential arc oxidation, to significantly improve the corrosion resistance of magnesium alloy, and the technique prepares simple, efficiency
Height, the composite coating of generation can significantly improve the corrosion resistance of magnesium alloy compared with original single MAO coatings.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of magnesium nickel hydrotalcite/differential arc oxidation composite coating, this is compound
Coating can effectively improve the corrosion stability of Mg alloy surface, and its is simple for process, easy to operate, at low cost, can with what is be widely popularized
Row.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of magnesium nickel hydrotalcite/differential arc oxidation composite coating, includes the following steps：
1）Magnesium alloy the pretreatments such as be ground to, washed, being dried；
2）Pretreated magnesium alloy is subjected to differential arc oxidation；The constituent of electrolyte used in differential arc oxidation is：Sodium metasilicate 5-
30g/L, sodium phosphate 5-20g/L, sodium hydroxide 1-10g/L；Differential arc oxidation uses constant current mode, processing time 20min, frequency
Rate is 800Hz；
3）Magnesium alloy after differential arc oxidation in mixed solution is subjected to hydro-thermal reaction, the magnesium nickel hydrotalcite/differential of the arc oxygen is made
Change composite coating；The ammonium nitrate of the nickel nitrate containing 0.01-0.05mol/L, 0.01-0.1mol/L, are used in combination in the mixed solution
The ammonium hydroxide of 1wt.% adjusts its pH as 5-9；The temperature of hydro-thermal reaction is 50-120 DEG C, reaction time 1-24h.
Hydrotalcite is a kind of important inorganic functional material, due to its special anion type laminated structure, with
The characteristics such as the adjustable property of cation, interlayer anion interchangeability, industrially extensive use in alkalinity, laminate.Profit of the invention
The performance of differential arc oxidation is improved with the property of hydrotalcite, is prepared for magnesium nickel hydrotalcite/differential arc oxidation composite coating, energy
The corrosion resistance of magnesium alloy is enough significantly improved, increases the service life of material, widens the application range of magnesium alloy, and it has
The characteristic of hydrotalcite coating, is used as absorbent coating；Meanwhile the method for the present invention is efficient, inexpensive, process is simple, to ring
Border is pollution-free.
Patent of invention（CN 106400079A）In disclose a kind of preparation of aluminum alloy surface multilayer super-hydrophobic composite film layer
Method, but compared with aluminium alloy, magnesium alloy has relatively negative electrode potential, is defeated by-the 2.31V of aluminium, chemism is big, easily
Corrode, significantly limit its application, therefore the corrosion resistance for improving magnesium alloy is particularly important.And compared with the patent, this
Invent easy to operate, the reaction time is short, and the interlayer anion in hydrotalcite can be exchanged for nitrate ion with chlorion, can
The corrosion resistance of magnesium alloy is significantly improved, there is the feasibility being widely popularized.
Description of the drawings
Fig. 1 is that the EDS of magnesium nickel hydrotalcite/differential arc oxidation composite coating schemes.
Fig. 2 is the XRD comparison diagrams of differential arc oxidation and magnesium nickel hydrotalcite/differential arc oxidation composite coating.
Fig. 3 is differential arc oxidation（A）With magnesium nickel hydrotalcite/differential arc oxidation composite coating（B）SEM comparison diagrams.
Fig. 4 is the dynamic polarization curve of differential arc oxidation and magnesium nickel hydrotalcite/differential arc oxidation composite coating.
Fig. 5 is impregnated for differential arc oxidation sample with magnesium nickel hydrotalcite/differential arc oxidation composite coating sample in 1M NaCl solutions
Comparison diagram after different number of days, wherein（a）It is impregnated in NaCl solution 0 day for differential arc oxidation sample,（b）For differential arc oxidation sample
It is impregnated 5 days in NaCl solution,（c）It is impregnated in NaCl solution 0 day for composite coating sample,（d）Exist for composite coating sample
It is impregnated 5 days in NaCl solution.
Specific embodiment
In order to which content of the present invention is made to easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further, but the present invention is not limited only to this.
Embodiment 1
1）Magnesium alloy the pretreatments such as be ground to, washed, being dried；
2）Water is added to be configured to 10g/L containing sodium metasilicate, sodium phosphate 10g/L, sodium hydroxide 5g/ sodium metasilicate, sodium phosphate, sodium hydroxide
Pretreated magnesium alloy is placed in electrolyte by the electrolyte of L, and differential arc oxidation, differential arc oxidation are carried out using constant current mode
Processing time is 20min, frequency 800Hz；
3）Water is added to be configured to the mixed solution of 0.03mol/L containing nickel nitrate, ammonium nitrate 0.05mol/L using nickel nitrate, ammonium nitrate,
And it is 6 to adjust its pH with the ammonium hydroxide of 1wt.%, the magnesium alloy after differential arc oxidation is placed in mixed solution, 80 DEG C of hydro-thermal reaction 1h,
Magnesium nickel hydrotalcite/differential arc oxidation composite coating is made.
Fig. 1 is that the EDS of magnesium nickel hydrotalcite/differential arc oxidation composite coating schemes.By in figure it is found that sample surfaces mainly by Ni,
Mg, O element form（Si elements may be due to being introduced from electrolyte in differential arc oxidation processing procedure）, wherein based on Ni
Element is wanted, this shows that the hydrotalcite that Ni elements are formed is evenly distributed on differential arc oxidation layer, effectively covers hole and crackle,
And without destroying MAO layers.
Fig. 2 is the XRD comparison diagrams of differential arc oxidation and magnesium nickel hydrotalcite/differential arc oxidation composite coating.From Figure 2 it can be seen that by
Occur the diffraction maximum of (003) and (006) crystal face of hydrotalcite after hydro-thermal reaction, suggest the formation of hydrotalcite coating.
Fig. 3 is differential arc oxidation（A）With magnesium nickel hydrotalcite/differential arc oxidation composite coating（B）SEM comparison diagrams.It can from Fig. 3
To be evident that, differential arc oxidation specimen surface is there are volcano shape hole, and surrounding is dispersed with crackle, these defects are
Differential arc oxidization technique is inevitable；And after hydro-thermal process, sheet hydrotalcite is formd in differential arc oxidization surface and hole
Coating using the ion-exchange capacity of hydrotalcite coating, enables to the chlorine ion concentration in corrosive environment to decline, is obviously improved
The corrosion stability of alloy.
Differential arc oxidation and magnesium nickel hydrotalcite/differential arc oxidation composite coating are studied in 3.5%wt sodium chloride using dynamic polarization curve
Corrosion resistance in solution, is as a result shown in Fig. 4.The complexity that corrosion potential representing sample is corroded, corrosion potential is smaller,
Then easier to corrode, the corrosion rate of corrosion current representing sample, corrosion current is smaller, then corrosion rate is smaller.From Fig. 4
It is found that the corrosion current of magnesium nickel hydrotalcite/differential arc oxidation composite coating is significantly less than differential arc oxidation, it was demonstrated that magnesium nickel hydrotalcite/
The corrosion stability of differential arc oxidation composite coating is higher than differential arc oxidation.The reason of causing this phenomenon is since neatly rock layers are with unique
Structure, nitrate ion can be exchanged with the chlorion in corrosive liquid, therefore form hydrotalcite coating in differential arc oxidization surface,
The concentration of chlorion in corrosive environment can be reduced so that the performance boost of sample.
Fig. 5 is impregnated for differential arc oxidation sample with magnesium nickel hydrotalcite/differential arc oxidation composite coating sample in 1M NaCl solutions
Comparison diagram after different number of days, wherein（a）It is impregnated in NaCl solution 0 day for differential arc oxidation sample,（b）For differential arc oxidation sample
It is impregnated 5 days in NaCl solution,（c）It is impregnated in NaCl solution 0 day for composite coating sample,（d）Exist for composite coating sample
It is impregnated 5 days in NaCl solution.It can be seen that after impregnating 5 days, serious peeling occurs for differential arc oxidation specimen surface, and magnesium closes
Auri body exposes；And magnesium nickel hydrotalcite/differential arc oxidation composite coating sample is still intact, shows to prepare on differential arc oxidation layer
Hydrotalcite is conducive to improve the corrosion resistance of sample.
Embodiment 2
1）Magnesium alloy the pretreatments such as be ground to, washed, being dried；
2）Water is added to be configured to 5g/L containing sodium metasilicate, sodium phosphate 5g/L, sodium hydroxide 1g/L sodium metasilicate, sodium phosphate, sodium hydroxide
Electrolyte, pretreated magnesium alloy is placed in electrolyte, differential arc oxidation is carried out using constant current mode, at differential arc oxidation
The reason time is 20min, frequency 800Hz；
3）Water is added to be configured to the mixed solution of 0.01mol/L containing nickel nitrate, ammonium nitrate 0.01mol/L using nickel nitrate, ammonium nitrate,
And it is 5 to adjust its pH with the ammonium hydroxide of 1wt.%, the magnesium alloy after differential arc oxidation is placed in mixed solution, 50 DEG C of hydro-thermal reactions
For 24 hours, magnesium nickel hydrotalcite/differential arc oxidation composite coating is made.
Embodiment 3
1）Magnesium alloy the pretreatments such as be ground to, washed, being dried；
2）Water is added to be configured to 30g/L containing sodium metasilicate, sodium phosphate 20g/L, sodium hydroxide sodium metasilicate, sodium phosphate, sodium hydroxide
Pretreated magnesium alloy is placed in electrolyte by the electrolyte of 10g/L, and differential arc oxidation, the differential of the arc are carried out using constant current mode
Oxidation treatment time is 20min, frequency 800Hz；
3）Water is added to be configured to the mixed solution of 0.05mol/L containing nickel nitrate, ammonium nitrate 0.1mol/L using nickel nitrate, ammonium nitrate,
And it is 9 to adjust its pH with the ammonium hydroxide of 1wt.%, the magnesium alloy after differential arc oxidation is placed in mixed solution, 120 DEG C of hydro-thermal reactions
Magnesium nickel hydrotalcite/differential arc oxidation composite coating is made in 2h.
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 should all belong to the covering scope of the present invention.
Claims (5)
1. a kind of preparation method of magnesium nickel hydrotalcite/differential arc oxidation composite coating, it is characterised in that：Magnesium alloy is ground, is washed,
Differential arc oxidation is carried out after drying, hydro-thermal reaction is carried out in mixed solution, it is compound that the magnesium nickel hydrotalcite/differential arc oxidation is made
Coating.
2. the preparation method of magnesium nickel hydrotalcite/differential arc oxidation composite coating according to claim 1, it is characterised in that：The differential of the arc
The constituent of electrolyte used is during oxidation：Sodium metasilicate 5-30g/L, sodium phosphate 5-20g/L, sodium hydroxide 1-10g/L.
3. the preparation method of magnesium nickel hydrotalcite/differential arc oxidation composite coating according to claim 1, it is characterised in that：The differential of the arc
Oxidation is using constant current mode, processing time 20min, frequency 800Hz.
4. the preparation method of magnesium nickel hydrotalcite/differential arc oxidation composite coating according to claim 1, it is characterised in that：It is described
The ammonium nitrate of nickel nitrate containing 0.01-0.05mol/L, 0.01-0.1mol/L in mixed solution, and adjusted with the ammonium hydroxide of 1wt.%
Its pH is 5-9.
5. the preparation method of magnesium nickel hydrotalcite/differential arc oxidation composite coating according to claim 1, it is characterised in that：Hydro-thermal
The temperature of reaction is 50-120 DEG C, reaction time 1-24h.
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Citations (7)
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|---|---|---|---|---|
| CN102345150A (en) * | 2010-07-29 | 2012-02-08 | 比亚迪股份有限公司 | Magnesium alloy surface treating method and magnesium alloy prepared by same |
| CN103173765A (en) * | 2013-03-26 | 2013-06-26 | 哈尔滨工业大学 | Method for preparing composite film layer through depositing hydroxylapatite on magnesium alloy micro-arc oxidation film |
| CN104878377A (en) * | 2015-05-20 | 2015-09-02 | 哈尔滨工业大学 | Method for preparing graphene oxide and micro-arc oxidized ceramic composite coating on surface of magnesium alloy |
| CN105018999A (en) * | 2015-07-09 | 2015-11-04 | 哈尔滨工程大学 | Method for growing layered doubled hydroxide on aluminum alloy micro-arc oxidation film in situ |
| CN106086984A (en) * | 2016-08-23 | 2016-11-09 | 苏州库浩斯信息科技有限公司 | A kind of Microarc Oxidation of Al-mg Alloy method and electrolyte |
| CN106086992A (en) * | 2016-06-07 | 2016-11-09 | 重庆大学 | A kind of preparation method of the double hydroxy metal oxide closing membrane layer of Mg alloy surface |
| CN106702238A (en) * | 2017-02-17 | 2017-05-24 | 中国科学院上海硅酸盐研究所 | Surface modified magnesium alloy material as well as preparation method thereof and application thereof |
-
2018
- 2018-04-17 CN CN201810344032.1A patent/CN108251839B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102345150A (en) * | 2010-07-29 | 2012-02-08 | 比亚迪股份有限公司 | Magnesium alloy surface treating method and magnesium alloy prepared by same |
| CN103173765A (en) * | 2013-03-26 | 2013-06-26 | 哈尔滨工业大学 | Method for preparing composite film layer through depositing hydroxylapatite on magnesium alloy micro-arc oxidation film |
| CN104878377A (en) * | 2015-05-20 | 2015-09-02 | 哈尔滨工业大学 | Method for preparing graphene oxide and micro-arc oxidized ceramic composite coating on surface of magnesium alloy |
| CN105018999A (en) * | 2015-07-09 | 2015-11-04 | 哈尔滨工程大学 | Method for growing layered doubled hydroxide on aluminum alloy micro-arc oxidation film in situ |
| CN106086992A (en) * | 2016-06-07 | 2016-11-09 | 重庆大学 | A kind of preparation method of the double hydroxy metal oxide closing membrane layer of Mg alloy surface |
| CN106086984A (en) * | 2016-08-23 | 2016-11-09 | 苏州库浩斯信息科技有限公司 | A kind of Microarc Oxidation of Al-mg Alloy method and electrolyte |
| CN106702238A (en) * | 2017-02-17 | 2017-05-24 | 中国科学院上海硅酸盐研究所 | Surface modified magnesium alloy material as well as preparation method thereof and application thereof |
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