CN102277611A - Method for treating surface of magnesium-based metal to give metallic texture thereof - Google Patents
Method for treating surface of magnesium-based metal to give metallic texture thereof Download PDFInfo
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- CN102277611A CN102277611A CN2010102348088A CN201010234808A CN102277611A CN 102277611 A CN102277611 A CN 102277611A CN 2010102348088 A CN2010102348088 A CN 2010102348088A CN 201010234808 A CN201010234808 A CN 201010234808A CN 102277611 A CN102277611 A CN 102277611A
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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
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/16—Pretreatment, e.g. desmutting
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Abstract
A method for treating a surface of a magnesium-based metal is disclosed for realizing a metallic texture of the magnesium-based metal. The method includes a buffing step of chemically polishing a surface of a magnesium-based metal by using a chemical polishing agent containing sodium nitride and sodium citrate; an immersing step of immersing the magnesium-based metal, which has been subject to the buffing step, into a strongly alkaline electrolyte solution of pH 11 or above; and an anodizing treatment step of forming a transparent anodizing film on the surface of the magnesium-based metal by applying current with a current density of 0.01 to 1 A/dm2 to the magnesium-based metal in the strongly alkaline electrolyte solution.
Description
Technical field
The present invention relates to a kind of method that is used to handle the surface of magnesium-base metal, and more particularly, relate to and a kind ofly handle the surface of magnesium-base metal to give the method for its metal texture with the environmental protection scheme.
Background technology
With regard to weight, expected that magnesium-base metal will be the most promising engineering materials in future, it can replace aluminium based metal.
At present, the price of magnesium is substantially equal to the price of aluminium, but magnesium will be lighter than aluminium.Therefore, magnesium is used in the prior vehicle of light weight, aircraft, laptop computer, the cellular phone etc. more favourable than aluminium.For instance, in vehicular field, used magnesium alloy to replace iron and steel or aluminium alloy recently,, thereby improved fuel efficiency so that alleviate the weight of vehicle.
Recently, even aspect environment, the magnesium alloy with good recycling feature (recycling feature) also tends to be widely used as structural metallic materials.For instance, existing parts of plastics tends to be had the magnesium alloy replacement of good recycling feature, and is especially all the more so the mobile computer in household appliance technical field, Personal Computer and the cellular phone.
In common metal, described magnesium alloy has maximum chemically reactive (chemicalactivity).Therefore, if magnesium alloy without undergoing surface treatment, its feature is corroded under atmosphere or in solution as quick as thought so, therefore it is very important to form under the situation than steel or aluminium alloy finer and close and uniform coating by magnesium alloy surface treatment process.Yet, extremely difficult densification and the uniform coating of on magnesium alloy, forming.This is because the surface of magnesium alloy is irregular for chemistry.It is that chemistry is irregular that macrosegregation and microsegregation make the surface of magnesium alloy, and therefore is difficult to form on magnesium alloy fine and close and uniform coating.In addition, because the oxide film that generates on Mg alloy surface comprises Mg (OH)
2(it is the oxide film of impermeable (impermeable)) formed, and therefore may not can realize magnesium institute inherent metal texture.
In the various surface treatment methods of magnesium alloy, the most frequently used to transformation processing method (conversiontreatment method) or anode oxidative treatment method (anodizing treatment method).These two kinds of methods are all carried out behind any pretreatment technology, for example degreasing process and/or acid cleaning process.Yet, can be only by using anode oxidative treatment method with any functional surface of adding magnesium alloy to.
In the conventional surface treatment method of magnesium alloy, HAE method, DOW17 method and electrochemical method (galvanic method) extensively are called anode oxidative treatment method in this technology, but there is shortcoming, promptly, these methods are used and (are for example contained heavy metal, manganese and/or chromium) electrolyte solution, therefore cause producing the waste water that contains heavy metal and cause products obtained therefrom poisonous.
In addition, in conventional anode oxidative treatment method to magnesium alloy, such as in the early stage publication application case of 10-2004-94105 Korea S announcement, in strong alkaline electrolytes solution, form oxide film with 100V or higher high-voltage, or such as in the early stage publication application case of 10-2003-40824 Korea S announcement, by in the weakly alkaline electrolyte solution with impulse form apply-200V forms impermeable oxide film to the AC voltage of 400V.
Yet,, therefore be difficult to realize institute's inherent metal texture in the magnesium-base metal because above-mentioned routine techniques produces the coloured impermeable film with white or brown.Therefore, need a kind of technology in this technology, it is used for realizing magnesium alloy institute inherent metal texture by form transparent anode oxide film on the surface of magnesium alloy.In addition, in order to form qualified anode oxide film on the surface of magnesium alloy, need a kind of technology, it is used for the surface modification of magnesium alloy is become to be suitable for forming another surface of anode oxide film.As the polishing technology of the pretreatment technology of anode oxidative treatment method, the well-known chemical rightenning technology that is to use the chemical polishing agent (chemical polishingagent) that contains chromic acid and HF in this technology.Yet, because chemical polishing agent as described above extremely costliness and murther, so this technology has been caused serious censure.
This shows that the surface treatment method of above-mentioned existing magnesium-base metal obviously still has inconvenience and defective, and demands urgently further being improved in method and use.In order to solve the problem of above-mentioned existence, relevant manufacturer there's no one who doesn't or isn't seeks solution painstakingly, but do not see always that for a long time suitable design finished by development, and general method does not have appropriate method to address the above problem, this obviously is the problem that the anxious desire of relevant dealer solves.Therefore how to found a kind of surface that is used to handle magnesium-base metal newly to give the method for its metal texture, belong to one of current important research and development problem in fact, also becoming the current industry utmost point needs improved target.
Summary of the invention
The objective of the invention is to, overcome the defective of the surface treatment method existence of existing magnesium-base metal, and provide a kind of new being used to handle the surface of magnesium-base metal to give the method for its metal texture, technical problem to be solved is to make it be formed for realizing the qualified transparent anode oxide film of the metal texture of magnesium-base metal on just can the surface at magnesium-base metal when using the environmental protection electrolyte solution, is very suitable for practicality.
Another object of the present invention is to, provide a kind of new being used to handle the surface of magnesium-base metal to give the method for its metal texture, technical problem to be solved is to make it can realize more qualified anode oxide film by cheap and safe chemical rightenning technology before forming anode oxide film, thereby is suitable for practicality more.
The object of the invention to solve the technical problems realizes by the following technical solutions.For achieving the above object, be used to handle the surface of magnesium-base metal to give the method for its metal texture according to of the present invention, it comprises: polishing step (buffing step), contain the surface of the chemical polishing agent of sodium nitride (sodiumnitride) and Trisodium Citrate (sodium citrate) with chemical mode polishing magnesium-base metal by use; Submergence step (immersing step) is immersed into the magnesium-base metal that is polished step in pH 11 or the higher strong alkaline electrolytes solution; And the anodic oxidation treatment step, applying current density by the magnesium-base metal in strong alkaline electrolytes solution is 0.01A/dm
2To 1A/dm
2Electric current and on the surface of magnesium-base metal, form transparent anode oxide film.
In the anodic oxidation treatment step, electric current preferably has 0.01A/dm
2To 1A/dm
2Current density.If current density surpasses 1A/dm
2, may on the surface of magnesium-base metal, generate irregular oxide film so, and this irregular oxide film can cause being difficult to realize its metal texture.Equally, if current density less than 0.01A/dm
2, be difficult to form transparent anode oxide film so.More preferably, current density is 0.2A/dm
2To 0.7A/dm
2At this moment, anodic oxidation treatment technology was carried out about 3 minutes.In addition, in the anodic oxidation treatment step, voltage preferably is limited to 10V or below the 10V.
In the polishing step, chemical polishing agent preferably includes sulfuric acid, nitric acid, sodium nitride and Trisodium Citrate.
Described electrolyte solution preferably comprises potassium hydroxide, the KF (Potassium monofluoride) of 0.5 to 50 weight part, the NaSiO of 5 to 50 weight parts of 100 to 300 weight parts
4And the Al of 0.1 to 0.5 weight part, and described electrolyte solution preferably maintains under 20 ℃ to 70 ℃ the temperature.The oxide film that obtains after the anodic oxidation treatment step is transparent, and to realize the metal texture of magnesium alloy, described metal texture produces the minor structure of oxide film.Herein, if pigment is immersed in the oxide film, just then magnesium-base metal may seem as the magnesium-base metal surface with metal texture by colouring.Described pigment can be and is selected from the group that is made up of following each person at least one: Cobaltous diacetate (cobalt acetate), potassium permanganate (potassium permanganate), ammonium sulfide (ammonium sulfide), ferric sulfate (ferricsulfate), the Tripotassium iron hexacyanide (potassium ferricyanide), single nickel salt (nickelsulfate), copper sulfate (copper sulfate) and tin sulphate (stannous sulfate).
The present invention compared with prior art has tangible advantage and beneficial effect.By technique scheme, the surface that the present invention is used to handle magnesium-base metal has following advantage and beneficial effect at least with the method that gives its metal texture: according to the present invention, the surface modification of magnesium-base metal might be become another surface, described another surface is suitable for using cheap and safe chemical polishing agent is carried out anodic oxidation by chemical rightenning technology.In addition, anodic oxidation treatment technology is carried out on the gained surface best, might be made the senior magnesium-base metal product that has the transparent anode oxide film on the surface, realize the metal texture of magnesium alloy whereby by using the environmental protection electrolyte solution that does not contain heavy metal.
In sum, the invention relates to and a kind ofly be used to handle the surface of magnesium-base metal to give the method for its metal texture, this method comprises: the polishing step, contain the surface of the chemical polishing agent of sodium nitride and Trisodium Citrate with chemical mode polishing magnesium-base metal by use; The submergence step is immersed into the magnesium-base metal that is polished step in pH 11 or the higher strong alkaline electrolytes solution; And the anodic oxidation treatment step, applying current density by the magnesium-base metal in strong alkaline electrolytes solution is 0.01A/dm
2To 1A/dm
2Electric current and on the surface of magnesium-base metal, form the transparent anode oxide film.
Above-mentioned explanation only is the general introduction of technical solution of the present invention, for can clearer understanding technique means of the present invention, and can be implemented according to the content of specification sheets, and for above-mentioned and other purposes, feature and advantage of the present invention can be become apparent, below especially exemplified by preferred embodiment, and conjunction with figs., be described in detail as follows.
Description of drawings
Fig. 1 is the schema of the ordinary method on the explanation surface that is used to handle magnesium-base metal.
Fig. 2 A-Fig. 2 B is explanation according to the schema of the method on the surface that is used to handle magnesium-base metal of the present invention.
Fig. 3 is a synoptic diagram of showing the surface processing equipment of the magnesium-base metal that is adopted among the present invention.
Fig. 4 be with opticmicroscope obtain be illustrated in chemical rightenning and (or, alkali degreasing) is formed with the magnesium-base metal surface of transparent anode oxide film afterwards photo is adjusted on the surface.
Fig. 5 is the photo that is not formed with the magnesium-base metal surface of anode oxide film above the displaying that obtains with opticmicroscope, for carrying out the comparison of metal texture with the photo of Fig. 4.
Embodiment
Reach technique means and the effect that predetermined goal of the invention is taked for further setting forth the present invention, below in conjunction with accompanying drawing and preferred embodiment, to method its embodiment, method, step, feature and the effect thereof of surface that is used to handle magnesium-base metal that foundation the present invention proposes to give its metal texture, describe in detail as after.
Relevant aforementioned and other technology contents, characteristics and effect of the present invention can clearly present in the following detailed description that cooperates with reference to graphic preferred embodiment.For convenience of description, in following embodiment, components identical is represented with identical numbering.
Fig. 1 is the schema of the ordinary method on the explanation surface that is used to handle magnesium-base metal, and Fig. 2 A-Fig. 2 B is the schema that the method on the surface that is used to handle magnesium-base metal according to an embodiment of the invention is described.
Such as among Fig. 2 A-Fig. 2 B displaying, comprise polishing step 21, degreasing or surperficial set-up procedure 22, anodic oxidation treatment step 23 and water-washing step 24 according to the surface treatment method of present embodiment.
Polishing step 21 is used the chemical rightenning scheme.After having carried out polishing step 21 and degreasing or surperficial set-up procedure 22, magnesium-base metal is immersed in the strong alkaline electrolytes solution carrying out anodic oxidation treatment, and then makes magnesium-base metal in electrolyte solution, stand anodic oxidation treatment step 23.The magnesium-base metal product that is formed with the transparent anode oxide film by the anodic oxidation treatment step then stands any post-processing step above, comprises water-washing step 24.
Hereinafter, only explain polishing step 21 and anodic oxidation treatment step 23 in the above-mentioned steps in more detail.
The polishing step
Preparation contains the chemical polishing agent of the Trisodium Citrate of the sodium nitride of nitric acid, 130g/L of sulfuric acid, the 15g/L of 100g/L and 150g/L.In the chemical polishing agent that the magnesium alloy submergence is at room temperature prepared, continue 5 seconds to 30 seconds with surface with chemical mode polishing magnesium alloy.The component ratio of chemical polishing agent is not limited to above describe, and found that glossing is comparatively good when the component of chemical polishing agent compares in following scope: the Trisodium Citrate of the nitric acid of the sulfuric acid of 50 to 500 weight parts, 10 to 100 weight parts, the sodium nitride of 100 to 300 weight parts and 100 to 300 weight parts.
After chemical rightenning technology, use opticmicroscope to observe and/or check the metal texture of magnesium alloy, and also find in the surface, to produce many holes.These holes help to strengthen the adhesive power (adhesive force) with the transparent anode oxide film, and described transparent anode oxide film will be formed by the anodic oxidation treatment step below it.
Before the polishing step, can carry out the alkali degreasing step.In the alkali degreasing step, the magnesium alloy that does not stand to polish step as yet is immersed in 80 ℃ the skim soln and continues about 5 minutes, described skim soln is to obtain by sodium hydroxide and yellow soda ash are put into distilled water by 7: 1 ratio.
After the polishing step, can carry out surperficial set-up procedure.In surperficial set-up procedure, the magnesium alloy that is polished step is immersed in surperficial the adjustment in the solution (surface adjusting solution) continues about 15 seconds, described surface adjustment solution contains the chromic acid of 100g/L, the nitrided iron of 20g/L and the fluoric acid of 1g/L.At this moment, need in surperficial set-up procedure, be accompanied by stirring.
The anodic oxidation treatment step
In strong alkaline electrolytes solution, carry out the anodic oxidation treatment step.The processing condition that can exert an influence to the coating feature are composition, current density, temperature, working hour of electrolyte solution etc.In these processing condition, the composition and the current density of electrolyte solution are most important.The strong alkaline electrolytes solution that is adopted in the present embodiment should comprise the potassium hydroxide of per 1 liter of total solution 50g to 300g, so that guarantee pH 11 or higher strong basicity.Because potassium hydroxide and non-heavy metal, therefore can be environmental protection.In more detail, in the present embodiment electrolyte solution that uses comprised per 1 liter of total solution 100g arrives 50g/L to the potassium hydroxide of 300g, 0.5 to 50g/L KF, 5 NaSiO
4And 0.1 to 0.5g/L Al.
If magnesium or magnesium alloy are immersed among the pH 11 or higher strong alkaline electrolytes solution of as indicated above and preparation, under 10V or lower voltage, will form oxide film well so.
Simultaneously, if pigment is added in the electrolyte solution, can obtain various grain effects so.
The pigment that adds can be changed according to want color.In the present invention, if at least one in interpolation Cobaltous diacetate, potassium permanganate, ammonium sulfide, ferric sulfate, the Tripotassium iron hexacyanide, single nickel salt, copper sulfate and the tin sulphate, can give the oxide film shades of colour so, for example red, orange, yellow, blue-greenish colour, blueness and black.
In addition, if carry out this anodic oxidation treatment technology, can fundamentally avoid any possibility problem that may in independent japanning process occur relevant so with Working environment so that realize metal texture.
Such as among Fig. 3 displaying, after being immersed in magnesium or magnesium alloy 3 and cathode substrate 4 in the electrolyte solution 2 that is held in the electrolyzer (electrolytic bath) 1, the anode of the power supply after the rectification (rect ified power supply) 5 is connected to magnesium alloy 3, and the negative electrode of the power supply after the rectification 5 is connected to cathode substrate 4, make to apply voltage betwixt, allow to form transparent anode oxide film whereby.
At this moment, current density is adjusted to 0.01A/dm
2To 1A/dm
2, 0.2A/dm more preferably
2To 0.7A/dm
2, and voltage is limited to 10V or below the 10V.Therefore, on the surface of magnesium or magnesium alloy 3, form even and fine and close film.Electrolyte solution is maintained under 20 ℃ to 70 ℃ the temperature.
In the present embodiment, only when needs are adjusted magnesium-base metal surperficial, just carry out the surface adjustment.In other words, just generally carry out surface adjustment for the surface of after polishing technology, adjusting magnesium-base metal.Yet, should suitably carry out surface adjustment according to the pollution level on required performance of surface treatment or pending surface.
Fig. 4 is the photo that forms the thin tissue in the Mg alloy surface of anode oxide film above showing according to an embodiment of the invention by anodic oxidation treatment, and Fig. 5 is the photo that is illustrated in the thin tissue in the surface of carrying out magnesium alloy self before the surface treatment.
Comparison diagram 4 and Fig. 5, although form anode oxide film on the surface of in Fig. 4, being showed, the surface of being showed among Fig. 4 show with Fig. 5 in the top identical metal texture of Mg alloy surface that does not form anode oxide film showed.Only the width between two lines is narrower.This is because the refraction of light changes owing to the formation of transparent anode oxide film.
The above, it only is preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, though the present invention discloses as above with preferred embodiment, yet be not in order to limit the present invention, any those skilled in the art, in not breaking away from the technical solution of the present invention scope, when the technology contents that can utilize above-mentioned announcement is made a little change or is modified to the equivalent embodiment of equivalent variations, in every case be not break away from the technical solution of the present invention content, according to technical spirit of the present invention to any simple modification that above embodiment did, equivalent variations and modification all still belong in the scope of technical solution of the present invention.
Claims (6)
1. a surface that is used to handle magnesium-base metal is characterized in that to give the method for its metal texture it may further comprise the steps:
The polishing step, the described surface of polishing described magnesium-base metal with chemical mode;
The submergence step is immersed into the described magnesium-base metal that stands described polishing step in pH 11 or the higher strong alkaline electrolytes solution; And
The anodic oxidation treatment step, applying current density by the described magnesium-base metal in described strong alkaline electrolytes solution is 0.01A/dm
2To 1A/dm
2Electric current and on the described surface of described magnesium-base metal, form the transparent anode oxide film.
2. according to claim 1ly be used to handle the surface of magnesium-base metal to give the method for its metal texture, it is characterized in that, in described polishing step, the described surface of polishing described magnesium-base metal with chemical mode with the chemical polishing agent that contains sodium nitride and Trisodium Citrate.
3. the surface that is used to handle magnesium-base metal according to claim 1 is characterized in that to give the method for its metal texture, in described anodic oxidation treatment step, voltage is limited to 10V or below the 10V.
4. according to claim 1ly be used to handle the surface of magnesium-base metal to give the method for its metal texture, it is characterized in that, in described anodic oxidation treatment step, described electrolyte solution comprises potassium hydroxide, the KF of 0.5 to 50 weight part, the NaSiO of 5 to 50 weight parts of 100 to 300 weight parts
4And the Al of 0.1 to 0.5 weight part, and described electrolyte solution maintained under 20 ℃ to 70 ℃ the temperature.
5. according to claim 1ly be used to handle the surface of magnesium-base metal to give the method for its metal texture, it is characterized in that, in described anodic oxidation treatment step, following at least one added in the described electrolyte solution: Cobaltous diacetate, potassium permanganate, ammonium sulfide, ferric sulfate, the Tripotassium iron hexacyanide, single nickel salt, copper sulfate and tin sulphate.
6. the surface that is used to handle magnesium-base metal according to claim 2 is characterized in that to give the method for its metal texture in described polishing step, described chemical polishing agent comprises sulfuric acid, nitric acid, sodium nitride and Trisodium Citrate.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR10-2010-0054535 | 2010-06-09 | ||
| KR1020100054535A KR101200526B1 (en) | 2010-06-09 | 2010-06-09 | Method for surface treating available the metallic effect |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102277611A true CN102277611A (en) | 2011-12-14 |
Family
ID=45095350
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010102348088A Pending CN102277611A (en) | 2010-06-09 | 2010-07-21 | Method for treating surface of magnesium-based metal to give metallic texture thereof |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US20110303545A1 (en) |
| JP (1) | JP5074561B2 (en) |
| KR (1) | KR101200526B1 (en) |
| CN (1) | CN102277611A (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103668392A (en) * | 2012-09-13 | 2014-03-26 | 汉达精密电子(昆山)有限公司 | Surface treatment method of magnesium alloy with metal texture and product thereof |
| US10941501B2 (en) | 2013-03-29 | 2021-03-09 | Analytical Specialties, Inc. | Method and composition for metal finishing |
| KR101584413B1 (en) | 2013-12-26 | 2016-01-11 | 주식회사 포스코 | Surface treated metallic material and surface treatment method for metallic material |
| KR101629585B1 (en) | 2014-12-26 | 2016-06-13 | 주식회사 포스코 | Color-treated substrate and color-treatment method thereof |
| WO2015099496A1 (en) | 2013-12-26 | 2015-07-02 | 주식회사 포스코 | Surface-treated substrate and substrate surface treatment method for same |
| KR20160085669A (en) | 2015-01-08 | 2016-07-18 | 주식회사 케이에이치바텍 | The metal exterior case with metal appearance and Method of manufacturing the same |
| KR101655039B1 (en) | 2015-07-24 | 2016-09-23 | 주식회사 포스코 | Color-treated substrate and color-treatment method thereof |
| KR101674316B1 (en) | 2015-09-21 | 2016-11-08 | 주식회사 포스코 | Color-treated substrate and color-treatment method thereof |
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| Publication number | Publication date |
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| US20110303545A1 (en) | 2011-12-15 |
| KR101200526B1 (en) | 2012-11-13 |
| KR20110134769A (en) | 2011-12-15 |
| JP5074561B2 (en) | 2012-11-14 |
| JP2011256458A (en) | 2011-12-22 |
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