CN106757276A - A kind of Mg alloy surface has protection and decoration yellow ceramic layer and preparation method thereof concurrently - Google Patents
A kind of Mg alloy surface has protection and decoration yellow ceramic layer and preparation method thereof concurrently Download PDFInfo
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- CN106757276A CN106757276A CN201611031889.5A CN201611031889A CN106757276A CN 106757276 A CN106757276 A CN 106757276A CN 201611031889 A CN201611031889 A CN 201611031889A CN 106757276 A CN106757276 A CN 106757276A
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- ceramic layer
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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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- 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
- C25D11/024—Anodisation under pulsed or modulated current or potential
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Abstract
Protection and decoration yellow ceramic layer and preparation method thereof are had concurrently the invention discloses a kind of Mg alloy surface, the ceramic layer is made up of metallic element doping MgO in colouring agent；By regulating and controlling colorant content and electric parameter (mainly voltage, oxidization time) in micro-arc oxidation electrolyte, it is capable of achieving the regulation and control of doped metallic elements content in arc differential oxide ceramic layer, and then form the regulatable MgO yellow arc differential oxide ceramic layer of doping, its metallic element doping content is 0.5 10at.%, ceramic layer thickness is 5~30 μm, and yellow color is deepened with the increase of doping.Compared to existing Mg alloy surface yellow arc differential oxide ceramic layer, overcome stability of solution difference and there are the technological problemses of safety risks, especially the more traditional white arc differential oxide ceramic layer of buff arc differential oxide ceramic layer has more excellent barrier propterty, therefore Industry Promotion is more suitable for, can be applied in fields such as 3C, decorations.
Description
First, technical field
The present invention relates to the technical field that metal surface has protection and functional coating concurrently, and in particular to a kind of Mg alloy surface
Have protection and decoration yellow ceramic layer and preparation method thereof concurrently.
2nd, background technology：
Magnesium metal light specific gravity, ductility are good, environmental-protecting performance is strong etc., and advantage makes it obtained on traditional industry field extensively
Concern, make its new lover in being increasingly becoming 26S Proteasome Structure and Function material, and coming into the life of ordinary people more and more,
Such as the extensive use on 3C Product.But, magnesium alloy application in the product is restricted, its change for being primarily due to magnesium
Learn property very active, magnesium standard electrode potential is -2.37V, less than the electrode potential of most of common metals.When itself and these
Metal will form corrosion galvanic cell when being in contact, magnesium serves as efficient anode and galvanic corrosion occurs in the middle of galvanic cell, so that
Component is produced expansion and delamination, cause the decline of component fatigue intensity, ultimately result in the premature failure of component.
Process for modifying surface is an effective means for improving magnesium and its alloy property, and most have development potentiality at present is micro-
Arc oxidation technology.But magnesium alloy micro-arc oxidization ceramic coating technique the most ripe is to prepare white coating, its electrolyte it is main by
Sodium silicate salt is constituted, it is difficult to meet the application requirement of 3C Product.Although researcher has carried out Mg alloy surface different colours
The preparation method research of differential arc oxidation layer, such as height draws intelligent in Na2SiO3To add KMnO in the solution of main salt4Carry out differential of the arc oxygen
Change coloring reaction, obtained that color is uniform, the preferable yellow oxidization film ceramic layer of compactness.The results of study such as Chen Tonghuan show,
In KMnO4To carry out differential arc oxidation reaction in the silicate systems electrolyte for colouring salt, with the change of solution concentration, film layer face
Color is according to faint yellow buff coffee color change.But KMnO4Easily decompose in the electrolytic solution and cause its bad stability, it is difficult to be full
Foot industrialization large-scale production, and there is potential safety hazard during micro-arc discharge as oxidant in KMnO4.
3rd, the content of the invention
Technical purpose of the invention is directed to existing magnesium alloy surface micro-arc oxidation coating color dullness, the yellow developed
Arc differential oxide ceramic layer preparation technology is unstable and there is the technical barrier of potential safety hazard, there is provided a kind of Mg alloy surface has concurrently anti-
Shield and decoration yellow ceramic layer and preparation method thereof, the ceramic layer has more excellent barrier propterty, while having ceramics again
The yellow of layer is adjustable, can promote using magnesium alloy as matrix, in the application of 3C and furnishing fields.
To achieve the above object, the technical solution adopted by the present invention is：A kind of Mg alloy surface has protection concurrently with decoration
Yellow arc differential oxide ceramic layer, it is characterised in that：The ceramic layer is by SnO2Doping MgO compositions；Using differential arc oxidization technique, in tin
In sour sodium electrolyte system, by regulating and controlling stannic acid sodium content and differential arc oxidation electric parameter in electrolyte, realize that differential arc oxidation is made pottery
The regulation and control of Sn constituent contents in enamel coating, and under the HTHP effect of differential arc oxidation electric discharge, form SnO2The yellow of doping MgO
Arc differential oxide ceramic layer.
The concentration of the sodium stannate is 2-30g/L, and adds 5g/L sodium metasilicate, 10g/L potassium hydroxide and 8g/L potassium fluorides.
The electric parameter of yellow arc differential oxide ceramic layer is prepared for pulse output voltage is 280~400V, frequency is
400Hz, dutycycle is 10%, and oxidization time is 5~30min.
A kind of Mg alloy surface has protection concurrently includes following step with the preparation method of the yellow arc differential oxide ceramic layer of decoration
Suddenly：
Step 1：After first passing through oil removing grease removal technique to the magnesium alloy sample of wire cutting, then ground by different waterproof abrasive papers
System, then polished rear washing is in case differential arc oxidation is processed；
Step 2：Chemical reagent is selected according to the matching principle of magnesium alloy differential arc oxidation electrolyte, the stannate system differential of the arc is prepared
Oxidation electrolyte；
Step 3：Using DC pulse mao power source, energy and oxidization time are exported by adjusting pulse, make magnesium
It is 5~30 μm that alloy surface forms thickness, and Sn contents are the magnesium oxide layer of 0.5-10at.%.
Compared with prior art, the invention has the advantages that and effect：
The present invention with magnesium alloy materials as matrix, in sodium stannate electrolyte system, by regulating and controlling differential arc oxidation electric parameter,
Prepare SnO2The ceramic layer of doping MgO, its Sn content is 0.5-10at.%, and thickness is 5~30 μm, with excellent protection
Performance, its excellent properties performance is as follows：
(1) by regulating and controlling the concentration of sodium stannate in electrolyte, simple in Mg alloy surface, stable the yellow differential of the arc can be prepared
Oxidation ceramic layer, color can be by faint yellow to deep yellow color change；
(2) corrosion electric current density of buff arc differential oxide ceramic layer can be substantially less than magnesium-based superficial white differential arc oxidation pottery
Enamel coating, enhances barrier propterty of the coating to magnesium matrix.
Mg alloy surface of the present invention has protection and the L values and b values of decoration yellow ceramic layer concurrently and can respectively reach 54.18 Hes
26.28, it is that 81.90 and b values are 0.49 relative to the L values of white arc differential oxide ceramic layer, obvious yellow is showed, and prepare
The good stability of yellow ceramic layer；The wherein corrosion electric current density of buff arc differential oxide ceramic layer is micro- less than magnesium-based superficial white
Arc oxidation ceramic layer.
Yellow arc differential oxide ceramic layer has differential arc oxidation porous character, the corrosion current of buff arc differential oxide ceramic layer
The more traditional white arc differential oxide ceramic layer order of magnitude lower of density, does not have any after corrosion before surface ceramii layer and corrosion
Difference.
4th, illustrate：
Fig. 1 is magnesium alloy through the yellow arc differential oxide ceramic layer macro morphology photo prepared by different process；Wherein a is tin
The concentration of sour sodium is the yellow arc differential oxide ceramic layer macro morphology photo of 0g/L；B is the yellow of 2g/L for the concentration of sodium stannate
Arc differential oxide ceramic layer macro morphology photo, c are the yellow arc differential oxide ceramic layer macro morphology of 5g/L for the concentration of sodium stannate
Photo, d are for the concentration that the concentration of sodium stannate is the yellow arc differential oxide ceramic layer macro morphology photo of 10g/L, e is sodium stannate
The yellow arc differential oxide ceramic layer macro morphology photo of 15g/L；
Fig. 2 is the XPS High-Resolution Maps that magnesium surface prepares Sn elements in ceramic layer；
Fig. 3 is electrochemical corrosion curve of the magnesium alloy through the arc differential oxide ceramic layer prepared by different process；
Fig. 4 is arc differential oxide ceramic layer through the surface SEM pattern photos after electrochemical corrosion；
5th, specific embodiment
Technical scheme is described in further detail with reference to specific embodiment：
A kind of Mg alloy surface has the yellow arc differential oxide ceramic layer of protection and decoration concurrently, and the ceramic layer is by SnO2Doping
MgO is constituted；Using differential arc oxidization technique, in sodium stannate electrolyte system, by regulate and control in electrolyte stannic acid sodium content and
Differential arc oxidation electric parameter, realizes the regulation and control of Sn constituent contents in arc differential oxide ceramic layer, and high in the high temperature of differential arc oxidation electric discharge
Under pressure effect, SnO is formed2The yellow arc differential oxide ceramic layer of doping MgO,
Prepared solution is stannate electrolyte system, and the concentration of sodium stannate is 2-30g/L, and add 5g/L sodium metasilicate,
10g/L potassium hydroxide and 8g/L potassium fluorides.
The electric parameter of yellow arc differential oxide ceramic layer is prepared for pulse output voltage is 280~400V, frequency is
400Hz, dutycycle is 10%, and oxidization time is 5~30min.
Embodiment 1：
In the present embodiment, Mg alloy surface is faint yellow arc differential oxide ceramic layer, that is, adding a small amount of sodium stannate electrolysis
Arc differential oxide ceramic layer is prepared in liquid, is formed in situ magnesium alloy substrate top layer porous doped with the magnesia of a small amount of Sn elements
Film, the thickness of the ceramic layer is 10 μm.
The preparation method of above-mentioned Mg alloy surface yellow arc differential oxide ceramic layer comprises the following steps：
Step 1：After first passing through oil removing grease removal technique to the magnesium alloy sample of wire cutting, first pass through different waterproof abrasive papers and grind,
Polished rear washing is in case differential arc oxidation is processed again.
Step 2：Chemical reagent is selected according to the matching principle of magnesium alloy differential arc oxidation electrolyte, the stannate system differential of the arc is prepared
The concentration of oxidation electrolyte, wherein sodium stannate is 2g/L, and adds 5g/L sodium metasilicate, 10g/L potassium hydroxide and 8g/L potassium fluorides.
Step 3：Using DC pulse mao power source, it is 300V to set pulse output voltage, and frequency is 400Hz,
Dutycycle is 10%, and oxidization time is 8min.It is 10 μm Mg alloy surface is formed thickness, and Sn contents are the oxygen of 1.70at.%
Change magnesium layer.
As shown in b in Fig. 1, color is in faint yellow, and color point for the macro morphology of arc differential oxide ceramic layer obtained above
Cloth is uniform；Its corrosion electric current density (1.44 × 10-7A/cm2) more traditional white arc differential oxide ceramic layer corrosion electric current density
(1.03×10-8A/cm2) an order of magnitude (such as Fig. 3) high, surface shows more obvious erosion profile, local corrosion occur
Hole is (as shown in Figure 4 b).
Embodiment 2：
In the present embodiment, Mg alloy surface is yellow arc differential oxide ceramic layer, i.e., in the sodium stannate electrolysis of addition more amount
Arc differential oxide ceramic layer is prepared in liquid, is formed in situ magnesium alloy substrate top layer porous doped with the magnesia of relatively large Sn elements
Film, the thickness of the ceramic layer is 15 μm.
The preparation method of above-mentioned Mg alloy surface yellow arc differential oxide ceramic layer comprises the following steps：
Step 1：After first passing through oil removing grease removal technique to the magnesium alloy sample of wire cutting, first pass through different waterproof abrasive papers and grind,
Polished rear washing is in case differential arc oxidation is processed again.
Step 2：Chemical reagent is selected according to the matching principle of magnesium alloy differential arc oxidation electrolyte, the stannate system differential of the arc is prepared
The concentration of oxidation electrolyte, wherein sodium stannate is 5g/L, and adds 5g/L sodium metasilicate, 10g/L potassium hydroxide and 8g/L potassium fluorides.
Step 3：Using DC pulse mao power source, it is 350V to set pulse output voltage, and frequency is 400Hz,
Dutycycle is 10%, and oxidization time is 12min.It is 15 μm Mg alloy surface is formed thickness, and Sn contents are the oxygen of 2.23at.%
Change magnesium layer.
As shown in c in Fig. 1, color is in yellow, and distribution of color for the macro morphology of arc differential oxide ceramic layer obtained above
Uniformly；Its corrosion electric current density (2.24 × 10-7A/cm2) more traditional white arc differential oxide ceramic layer corrosion electric current density
(1.03×10-8A/cm2) an order of magnitude (such as Fig. 3) high, surface shows more obvious erosion profile, and corrosion area is dredged
Pine, etch pit pattern is protruded (as shown in c in Fig. 4).
Embodiment 3：
In the present embodiment, Mg alloy surface is buff arc differential oxide ceramic layer, that is, adding further amounts of sodium stannate electricity
Arc differential oxide ceramic layer is prepared in solution liquid, is formed in situ magnesium alloy substrate top layer porous doped with the magnesia of more Sn elements
Film, the thickness of the ceramic layer is 20 μm.
The preparation method of above-mentioned Mg alloy surface yellow arc differential oxide ceramic layer comprises the following steps：
Step 1：After first passing through oil removing grease removal technique to the magnesium alloy sample of wire cutting, first pass through different waterproof abrasive papers and grind,
Polished rear washing is in case differential arc oxidation is processed again.
Step 2：Chemical reagent is selected according to the matching principle of magnesium alloy differential arc oxidation electrolyte, the stannate system differential of the arc is prepared
The concentration of oxidation electrolyte, wherein sodium stannate is 15g/L, and adds 5g/L sodium metasilicate, 10g/L potassium hydroxide and 8g/L fluorination
Potassium.
Step 3：Using DC pulse mao power source, it is 400V to set pulse output voltage, and frequency is 400Hz,
Dutycycle is 10%, and oxidization time is 18min.It is 20 μm Mg alloy surface is formed thickness, and Sn contents are the oxygen of 4.63at.%
Change magnesium layer.
As shown in d in Fig. 1, color is in buff, and color point for the macro morphology of arc differential oxide ceramic layer obtained above
Cloth is uniform, and further analysis finds that the Sn elements adulterated in ceramic layer form the SnO of yellow2Metal oxide (shown in Fig. 2),
Its corrosion electric current density (3.24 × 10-9A/cm2) more traditional white arc differential oxide ceramic layer corrosion electric current density (1.03 ×
10-8A/cm2) order of magnitude lower (such as Fig. 3), there is not any difference (d in such as Fig. 4 before surface ceramii layer and corrosion after corrosion
It is shown).
Claims (4)
1. a kind of Mg alloy surface has the yellow arc differential oxide ceramic layer of protection and decoration concurrently, it is characterised in that：The ceramic layer by
SnO2Doping MgO compositions；Using differential arc oxidization technique, in sodium stannate electrolyte system, by regulating and controlling sodium stannate in electrolyte
Content and differential arc oxidation electric parameter, realize the regulation and control of Sn constituent contents in arc differential oxide ceramic layer, and in differential arc oxidation electric discharge
HTHP effect under, formed SnO2The yellow arc differential oxide ceramic layer of doping MgO.
2. a kind of Mg alloy surface according to claim 1 has the yellow arc differential oxide ceramic layer of protection and decoration concurrently, its
It is characterised by：The concentration of the sodium stannate is 2-30g/L, and adds 5g/L sodium metasilicate, 10g/L potassium hydroxide and 8g/L fluorination
Potassium.
3. a kind of Mg alloy surface according to claim 1 has the yellow arc differential oxide ceramic layer of protection and decoration concurrently, its
It is characterised by：The electric parameter of yellow arc differential oxide ceramic layer is prepared for pulse output voltage is 280~400V, frequency is
400Hz, dutycycle is 10%, and oxidization time is 5~30min.
4. a kind of Mg alloy surface according to claim 1 has the system of protection and the yellow arc differential oxide ceramic layer of decoration concurrently
Preparation Method, it is characterised in that：Comprise the following steps：
Step 1：After first passing through oil removing grease removal technique to the magnesium alloy sample of wire cutting, then ground by different waterproof abrasive papers, then
Washing after polished is in case differential arc oxidation is processed；
Step 2：Chemical reagent is selected according to the matching principle of magnesium alloy differential arc oxidation electrolyte, stannate system differential arc oxidation is prepared
Electrolyte；
Step 3：Using DC pulse mao power source, energy and oxidization time are exported by adjusting pulse, make magnesium alloy
It is 5~30 μm that surface forms thickness, and Sn contents are the magnesium oxide layer of 0.5-10at.%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109267139A (en) * | 2018-10-31 | 2019-01-25 | 日照微弧技术有限公司 | A kind of electrolyte and preparation method thereof for magnesium alloy differential arc oxidation |
| CN109355643A (en) * | 2018-11-23 | 2019-02-19 | 西安工业大学 | A kind of preprocessing technical method suitable for aluminum alloy chemically copper facing |
| CN114395786A (en) * | 2021-12-23 | 2022-04-26 | 苏州粤辉煌新材料科技有限公司 | Preparation method and application of micro-arc magnesium oxide foil |
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| CN101603173A (en) * | 2009-04-29 | 2009-12-16 | 哈尔滨工程大学 | The method for chemically converting and treating stannate of magnesium alloy under action of alternative electric field |
| CN103614762A (en) * | 2013-12-05 | 2014-03-05 | 桂林电子科技大学 | Method for preparing magnesium alloy with micro-arc oxidation ceramic membrane |
| CN103614717A (en) * | 2013-10-30 | 2014-03-05 | 曾荣昌 | Corrosion resistant film prepared by magnesium alloy surface hydrothermal method and preparation technology thereof |
| CN103924142A (en) * | 2014-05-09 | 2014-07-16 | 重庆大学 | Magnesium alloy and preparing method thereof |
| CN104561980A (en) * | 2015-01-06 | 2015-04-29 | 南昌大学 | Surface treatment method for magnesium alloy |
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| CN1962959A (en) * | 2006-10-20 | 2007-05-16 | 华南理工大学 | Micro-arc oxidation electrolyte and method for surface modification by using same |
| CN101603173A (en) * | 2009-04-29 | 2009-12-16 | 哈尔滨工程大学 | The method for chemically converting and treating stannate of magnesium alloy under action of alternative electric field |
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| CN103614762A (en) * | 2013-12-05 | 2014-03-05 | 桂林电子科技大学 | Method for preparing magnesium alloy with micro-arc oxidation ceramic membrane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109267139A (en) * | 2018-10-31 | 2019-01-25 | 日照微弧技术有限公司 | A kind of electrolyte and preparation method thereof for magnesium alloy differential arc oxidation |
| CN109355643A (en) * | 2018-11-23 | 2019-02-19 | 西安工业大学 | A kind of preprocessing technical method suitable for aluminum alloy chemically copper facing |
| CN114395786A (en) * | 2021-12-23 | 2022-04-26 | 苏州粤辉煌新材料科技有限公司 | Preparation method and application of micro-arc magnesium oxide foil |
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Application publication date: 20170531 |