CN101619477A - Preparation method for multicolor oxide film - Google Patents
Preparation method for multicolor oxide film Download PDFInfo
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- CN101619477A CN101619477A CN200810129195A CN200810129195A CN101619477A CN 101619477 A CN101619477 A CN 101619477A CN 200810129195 A CN200810129195 A CN 200810129195A CN 200810129195 A CN200810129195 A CN 200810129195A CN 101619477 A CN101619477 A CN 101619477A
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Abstract
The invention relates to a preparation method for multicolor oxide film, comprising that an anode oxide film forming step is repeatedly carried out. The anode oxide film forming step comprises: oxidizing color anode, and forming a protective layer and laser carving on a color anode oxide film. The color anode oxidation comprises anode oxidation, dyeing and hole sealing are carried out in turn on the surface of a base material so as to obtain a color anode oxide film. The protective layer is used for separating electrolyte oxidized by a color anode and a color anode oxide film formed previously. The laser carving is used for removing at least one part of color anode oxide film formed previously so as to cause the surface of parts of base material to be exposed. The integral corrosion resistance and abrasion resistance of the oxide film on the surface of the base material, which is prepared according to the method of the invention, are high, and no other macromolecule materials need to be coated, so that the texture of the oxide film is kept.
Description
Technical field
The present invention relates to a kind of preparation method of oxide film, relate in particular to a kind of preparation method of multi-color oxide film.
Background technology
The preparation method of the colored oxide film on the surface of base material such as aluminium and aluminium alloy forms oxide film with the anodic oxidation in sulfuric acid of base materials such as aluminum or aluminum alloy, the processing of in containing the solution of organic dye, dyeing then, by adsorption, make dyestuff enter into the oxide film hole, handle through sealing of hole again, make substrate surfaces such as aluminium and aluminium alloy have various colors.
But this method can only form single color, therefore, in order to enrich the color of oxide film, discloses the method that can obtain multi-color oxide film as described below among the CN2546462Y.
First method comprises: (1) carries out anodizing with alloy matrix aluminum, forms oxide film; (2) remove partial oxide film by laser sculpture; (3) alloy matrix aluminum is carried out two-step anodization; (4) step of repetition (2)～(3); (5) electrolytic coloring or adsorption coloring are handled; (5) the external coating macromolecular material makes surfacing.
Second method comprises: (1) carries out anodizing with alloy matrix aluminum, forms oxide film; The oxide film surface screen printing acid and alkali-resistance printing ink that (2) need keep; (3) alloy matrix aluminum is put into phosphoric acid solution, the oxide film that is not hidden by printing ink is removed in corrosion; (4) remove removal ink; (5) step of repetition (1)～(4); (6) electrolytic coloring or adsorption coloring are handled; (7) the external coating macromolecular material makes surfacing.
The third method comprises: (1) is not to needing to carry out the Al-alloy based body portion printing acid and alkali-resistance printing ink sealing coat of anodizing; (2) alloy matrix aluminum is carried out anodizing, form oxide film; (3) remove removal ink; (4) alloy matrix aluminum is carried out two-step anodization; (5) step of repetition (1)～(4); (6) electrolytic coloring or adsorption coloring are handled; (7) the external coating macromolecular material makes surfacing.
In above-mentioned three kinds of methods, the wear resistance of the oxide film of Xing Chenging and erosion resistance are all relatively poor first, therefore, need in the end be coated with macromolecular material, but after being coated with macromolecular material, the texture that oxide film had has been lost on the surface of base material.In addition, two-step anodization can not be implemented the oversize time, comes off otherwise the oxide film that anodic oxidation first forms is breakdown easily.Though the shortening time can prevent coming off of oxide film to a certain extent, but oxidization time is short, then cause the degree of oxidation not enough, make that the hole that forms in the oxide film is less, thereby in follow-up dyeing course, can't adsorb too many dyestuff, this can cause the darker color that can't obtain to design in advance.
Summary of the invention
The objective of the invention is in order to overcome the not enough shortcoming of degree of oxidation of the oxide film that the multi-color oxide film wear resistance that forms in the prior art and corrosion-resistant, needs coating macromolecular material, second time and above anodic oxidation for the second time obtain, provide a kind of multi-color oxide film of formation wear resistance and good corrosion resistance, do not need to be coated with the preparation method of the high multi-color oxide film of the degree of oxidation of the oxide film that macromolecular material, the second time and the above anodic oxidation second time obtain.
The invention provides a kind of preparation method of multi-color oxide film; wherein; this method comprises that repeating anode oxide film forms step; this anode oxide film forms step and comprises coloured anodic oxidation of carrying out successively; on the coloured anode oxide film of gained, form protective layer and laser sculpture; described coloured anodic oxidation is included in substrate surface and carries out anodic oxidation successively; dyeing and sealing of hole; obtain coloured anode oxide film; described protective layer used in electrolytic solution in coloured anodic oxidation and the preceding coloured anode oxide film that once forms are isolated; at least a portion of the coloured anode oxide film that forms before described laser sculpture is used to remove is exposed the surface of at least a portion base material.
The method according to this invention, even for the second time and for the second time later anodised degree with anodised degree is identical or longer first, also the performance of the anode oxide film that can not form preceding anodic oxidation impacts, thereby the second time and for the second time later anodised degree can be set as required, carry out sufficient oxidation, obtain the abundant oxide film of hole, thereby improve painted performance, can easily obtain needed color.In addition, since for the second time and the performance of for the second time later anodic oxidation anode oxide film that can not form a preceding anodic oxidation impact, thereby the erosion resistance of the integral body of the oxide film on the surface of the base material that finally obtains and wear resistance are all good, need not to apply other macromolecular material, thereby the own texture that has kept oxide film makes the commodity that are made of the base material with this oxide film have higher added value.
Embodiment
The preparation method of multi-color oxide film of the present invention comprises that repeating anode oxide film forms step; this anode oxide film forms step and comprises coloured anodic oxidation of carrying out successively; on the coloured anode oxide film of gained, form protective layer and laser sculpture; described coloured anodic oxidation is included in substrate surface and carries out anodic oxidation successively; dyeing and sealing of hole; obtain coloured anode oxide film; described protective layer used in electrolytic solution in coloured anodic oxidation and the preceding coloured anode oxide film that once forms are isolated; at least a portion of the coloured anode oxide film that forms before described laser sculpture is used to remove is exposed the surface of at least a portion base material.
As long as the material of described protective layer can be realized above-mentioned purpose, that is to say that described protective layer only otherwise the electrolytic solution corrosion that can be subjected in the anodic oxidation gets final product.Those skilled in the art can easily select suitable material to be used as the material of protective layer according to instruction of the present invention.Specifically, the material of described protective layer for example can be one or more in acid and alkali-resistance printing ink, varnish and the cold coating, and the material of described protective layer all can be commercially available.For example can select acid and alkali-resistance printing ink Resist 1000 for use available from Hangzhou wild Scientific and Technical Industry Co., Ltd difficult to understand.
As long as described protective layer can be realized by arbitrary method attached on the anode oxide film.For example, the material of protective layer can be applied on the anode oxide film and get final product, described coating can be methods such as spraying, spin coating.In addition, the thickness of described protective layer can change in the larger context, and angle optimum from the protection effect and the saving cost considers that the thickness of described protective layer is preferably 5-50 μ m.
Described anodised method can be a method known in those skilled in the art.It is anode that described anodised method comprises with the base material, is negative electrode with the electrolyzer, and base material is carried out oxidation in electrolytic solution.Described electrolytic solution can be one or more in the aqueous solution of sulfuric acid, phosphoric acid, chromic acid and oxalic acid.Under the preferable case, described anodised method comprises with the base material being anode, is negative electrode with the electrolyzer, base material is carried out oxidation in sulphuric acid soln, the concentration of described sulphuric acid soln is the 150-210 grams per liter, and described anodised voltage is the 10-15 volt, and current density is 1-2A/dm
2, temperature is 18-22 ℃, the time is 20-60 minute.Under the preferable case, the erosion resistance and the wear resistance of the anode oxide film that finally obtains are better.
In addition, before carrying out above-mentioned anodic oxidation, base material can also be carried out the pre-treatment of removing oil-removing wax etc.The method of these pre-treatments is conventionally known to one of skill in the art.
Described painted method is the conventional method that is used for anodized stained membrane.This painted method comprises and will flood through anodised base material that described dye liquor is the aqueous solution of dyestuff in dye liquor, described dyestuff is one or more in azoic dyestuff, anthraquinone dye and the peptide cyanine dyes.Described base material makes anode oxide film catch desirable color and gets final product as long as flood in dye liquor.The concentration of dyestuff is preferably 0.1-10g/L in the described dye liquor, and the temperature of described dye liquor is preferably 30-55 ℃, and the time of described dipping is preferably 1-15min.
The method of described sealing of hole can use conventional antianode oxide film to carry out the method for sealing of hole.For example, can hydration sealing of hole or metal salt solution sealing of hole.Described hydration sealing of hole comprises boiling water sealing hole and normal pressure, steam under pressure sealing of hole.Described metal salt solution sealing of hole is exactly anode oxide film to be flooded get final product in metal salt solution.The present invention preferably carries out sealing of hole with the method that dyed base material floods in the aqueous solution of hole sealing agent.Described hole sealing agent is preferably one or more in nickel acetate, nickelous fluoride and the single nickel salt.The concentration of the aqueous solution of described hole sealing agent is preferably 1-10g/L, and the temperature of the described hole sealing agent aqueous solution is preferably 50-95 ℃, and the time of described dipping is preferably 10-50 minute.Under above-mentioned preferable case, the erosion resistance and the wear resistance of the anode oxide film that finally obtains are better.
As long as laser sculpture of the present invention makes the part surface of the base material that protected seam and anode oxide film cover expose, the described part of exposing can be designed to various patterns as required.Described laser sculpture can be realized by the laser machine.The condition of described laser sculpture can be selected as required.For example, can implement under following condition: electric current is the 2-20 peace, and frequency is the 2000-50000 hertz, and wavelength is the 5-1000 nanometer, and the time during engraving is the 2-30 millisecond.
As long as the material that base material of the present invention can be formed anode oxide film by anodic oxidation all can, preferred described base material is a light metal material, described light metal material for example can be a kind of in magnesium, magnesium alloy, aluminium, the aluminium alloy, is preferably aluminium and/or aluminium alloy.
In addition, in the preparation method of multi-color oxide film of the present invention, unqualified to the number of times of coloured anodic oxidation, protective cover.That is, can repeatedly repeat the flow process of coloured anodic oxidation, protective cover, laser sculpture, thereby can obtain two or more multi-color oxide films.Specifically, for example, base material is carried out once after coloured anodic oxidation, protective cover carries out laser sculpture, and the part that laser sculpture is fallen is carried out the coloured anodic oxidation of secondary then; Then, form protective layer at position again, carrying out laser sculpture on the position of this two-step anodization or on other position, carry out coloured anodic oxidation more then through two-step anodization.By that analogy, can form anode oxide film with two or more colors.In addition, method of the present invention also is included in and carries out removing protective layer after last coloured anodic oxidation.Remove protective layer as long as select for use appropriate means to remove according to the character of the material of protective layer.For example for acid and alkali-resistance printing ink, for example can dissolve to remove and get final product by xylene solvent.
In order to improve the sticking power of multi-color oxide film, when impurity such as greasy dirt was arranged when described substrate surface, method provided by the invention preferably also is included in carried out pre-treatment to base material earlier before anodic oxidation forms step.The method of described pre-treatment can adopt method well known in the art, for example can be in removing oil-removing wax, chemical rightenning, mechanical polishing, the sandblast one or more.
Come the present invention is illustrated in greater detail below by embodiment.
Embodiment 1
Present embodiment illustrates the preparation method of multi-color oxide film of the present invention.
(1) pre-treatment
With commercial-purity aluminium (the new Ling Hua die steel in Shenzhen company limited, model 1A85, form: Fe≤0.01 weight %, Si≤0.08 weight %, Cu≤0.01 weight %, all the other are aluminium) to be immersed in 40 grams per liters, temperature as base material be that 60 ℃ alloy removes in oil-bound distemper (purchase in the LD-208 alloy that Shenzhen's moral is contained chemical industry company limited and the remove oil-bound distemper) solution and takes out after 5 minutes, the alloy that water cleans substrate surface removes oil-bound distemper.
Impregnated in the above-mentioned base material that carries out behind the removing oil-removing wax by concentration is chemical rightenning after 5 seconds in the solution formed of the phosphoric acid of 700 grams per liters and sulfuric acid that concentration is 200 grams per liters, impregnated in immediately in the water to clean the residual acid of substrate surface, then base material be impregnated in the sodium hydroxide solution of 10 grams per liters after 10 minutes, impregnated in the residual alkali that cleans substrate surface in the water immediately.
(2) anodic oxidation
To immerse through the base material after the above-mentioned processing and fill in the electrolyzer that concentration is 150 grams per liter aqueous sulfuric acids, as anode, be that 10 volt, current density be 1A/dm at voltage with this base material
2, temperature is anodic oxidation 50 minutes under 22 ℃ the condition, take out and clean up after finishing anodic oxidation.
(3) dyeing
Base material after the anodic oxidation is immersed the dye liquor that has prepared, and (Taiwan is photochemistry limited-liability company forever, and K160) middle dyeing is 10 minutes, and the concentration of this matching stain solution is 5 grams per liters, and pH value is 5.6, and the temperature of described dye liquor is 50 ℃.Take out after finishing and clean up.
(4) sealing of hole, oven dry
With the dipping 10 minutes in the hole sealing agent (nickel sulfate solution, concentration are 10 grams per liters) of the base material after the dyeing, temperature is 85 ℃, finishes that the pure water with 90 ℃ cleans up behind the sealing of hole, and toasts 15 minutes under 60 ℃ of conditions.
(5) form protective layer
In the spraying of the substrate surface behind sealing of hole acid and alkali-resistance printing ink (Hangzhou wild Scientific and Technical Industry Co., Ltd difficult to understand, Resist 1000), and under 60 ℃, toasted 20 minutes, obtain the protective layer that thickness is 20 μ m.
(6) laser sculpture
With laser engraving machine (model is HSLE-SP), is 5 peaces at electric current with the base material that is coated with protective layer, and frequency is 5000 hertz, and wavelength is 50 nanometers, and intermediate retardation is the pattern that laser sculpture forms the flower shape under 5 milliseconds of conditions, and makes base material expose.
(7) two-step anodization, dyeing, sealing of hole, oven dry
Step according to above-mentioned (2) to (4) is carried out two-step anodization, dyeing, sealing of hole, oven dry, and different is that described dyestuff is the TAC RED-BLH of Hangzhou wild Scientific and Technical Industry Co., Ltd difficult to understand.
(8) remove protective layer
The base material that step (7) is obtained soaked 5 minutes in dimethylbenzene under 50 ℃, and the flushing of water water removes removal ink, drying.
Finally obtain the base material A1 of surface for red flower shape and green background.The edge clear of the pattern on this base material A1 surface, integral body has the texture of anode oxide film, has sight.
Comparative Examples 1
Method according to embodiment 1 is handled base material, and different is uncoated protective layer.
Oxide film part breakdown coming off in the two-step anodization process that final anodic oxidation first obtains.Can't obtain 1 described base material with double-colored oxide film as embodiment.
Comparative Examples 2
Method according to Comparative Examples 1 is handled base material, and different is that the time of described two-step anodization is 25 minutes.Finally obtain the base material D1 of surface for red flower shape and green background.This base material D1 redness obviously is shallower than the base material A1 of embodiment, does not have that base material A1's is red bright-coloured.
From Comparative Examples 1 and Comparative Examples 2 as can be seen, under the situation of uncoated protective layer, the time of two-step anodization can not be long, and when long, the oxide film that anodic oxidation first forms is breakdown coming off easily.Though can shorten the time of two-step anodization,, this two-step anodization forms oxide film because degree of oxidation is not enough, can't be coloured to darker color, promptly can only be coloured to light red.
Embodiment 2
Method according to embodiment 1 is handled base material, different is, described base material is an aluminium alloy (Alcoa, 6061-T6), and step (7) afterwards step (8) also comprise anodic oxidation for the third time, dyeing, sealing of hole, oven dry before, and described dyestuff is the Taiwan K520 of photochemistry limited-liability company forever.
Finally obtain the surface and be the base material A2 of red flower shape, yellow flower shape and green background.
Embodiment 3
Method according to embodiment 2 is handled base material, different is, described base material is an aluminium alloy (Alcoa, 5A12, surface-area is 0.1 square metre), and step (8) also comprises the 4th anodic oxidation, dyeing, sealing of hole, oven dry before after anodic oxidation for the third time, dyeing, sealing of hole, oven dry, and described dyestuff is the Skyblue-GLH of Hangzhou wild Scientific and Technical Industry Co., Ltd difficult to understand.
Finally obtain the base material A3 of surface for red flower shape, yellow flower shape, blue flower shape and green background.
Embodiment 4
Method according to embodiment 1 is handled base material, and different is that described anodised process is carried out according to as described below:
To immerse through the base material after the above-mentioned processing and fill in the electrolyzer that concentration is 210 grams per liter aqueous sulfuric acids, as anode, be that 15 volt, current density be 2A/dm at voltage with this base material
2, temperature is anodic oxidation 30 minutes under 19 ℃ the condition, take out and clean up after finishing anodic oxidation.
Finally obtain the base material A4 of surface for red flower shape and green background.The edge clear of the pattern on this base material A4 surface, integral body has the texture of anode oxide film, has sight.
Embodiment 5
Method according to embodiment 1 is handled base material, and different is that described anodised process is carried out according to as described below:
To immerse through the base material after the above-mentioned processing and fill in the electrolyzer that concentration is 140 grams per liter aqueous sulfuric acids, as anode, be that 20 volt, current density be 0.8A/dm at voltage with this base material
2, temperature is anodic oxidation 50 minutes under 22 ℃ the condition, take out and clean up after finishing anodic oxidation.
Finally obtain the base material A5 of surface for red flower shape and green background.The edge clear of the pattern on this base material A5 surface, integral body has the texture of anode oxide film, has sight.
Embodiment 6
Method according to embodiment 1 is handled base material, and different is that described sealing of hole carries out according to as described below:
With the dipping 40 minutes in the hole sealing agent (nickel sulfate solution, concentration are 2 grams per liters) of the base material after the dyeing, temperature is 85 ℃, finishes that the pure water with 90 ℃ cleans up behind the sealing of hole, and toasts 15 minutes under 60 ℃ of conditions.
Finally obtain the base material A6 of surface for red flower shape and green background.The edge clear of the pattern on this base material A6 surface, integral body has the texture of anode oxide film, has sight.
Embodiment 7
Method according to embodiment 1 is handled base material, and different is that described sealing of hole carries out according to as described below:
With the dipping 50 minutes in the hole sealing agent (nickel sulfate solution, concentration are 0.5 grams per liter) of the base material after the dyeing, temperature is 90 ℃, finishes that the pure water with 90 ℃ cleans up behind the sealing of hole, and toasts 15 minutes under 60 ℃ of conditions.
Finally obtain the base material A7 of surface for red flower shape and green background.The edge clear of the pattern on this base material A7 surface, integral body has the texture of anode oxide film, has sight.
Embodiment 8-14
Base material A1-A7 carries out following performance test:
(1) erosion resistance test
Method according to standard ISO 9227-1990 is carried out neutral salt spray corrosion test, and the result is as shown in table 1.
(2) wearability test
Carry out the wear-resisting test of paper tape according to the method for standard A STM F2357-04, the result is as shown in table 1.
Comparative Examples 3
Erosion resistance and wear resistance according to the method testing substrates D1 of embodiment 8.The result is as shown in table 1.
Table 1
| Numbering | Erosion resistance (hour) | Wear resistance (circle) |
| Base material A1 | ??2420 | ??950 |
| Base material D1 | ??1020 | ??200 |
| Base material A2 | ??2250 | ??880 |
| Base material A3 | ??2080 | ??800 |
| Base material A4 | ??2400 | ??940 |
| Base material A5 | ??2250 | ??890 |
| Base material A6 | ??2405 | ??900 |
| Base material A7 | ??2200 | ??880 |
As can be seen from Table 1, the base material A1-A7 that makes of the present invention has superior corrosion resistance and wear resistance.And the erosion resistance of the base material D1 that Comparative Examples 2 makes and wear resistance are obviously relatively poor.In addition, from base material A1, A4 and A5 as can be seen, under preferred anodic oxidation condition, the erosion resistance and the wear resistance of the anode oxide film of the base material that finally obtains are better.From base material A1, A6, A7 as can be seen, under preferred sealing of hole condition, the erosion resistance and the wear resistance of the anode oxide film of the base material that finally obtains are better.
Claims (10)
1; a kind of preparation method of multi-color oxide film; it is characterized in that; this method comprises that repeating anode oxide film forms step; this anode oxide film forms step and comprises coloured anodic oxidation of carrying out successively; on the coloured anode oxide film of gained, form protective layer and laser sculpture; described coloured anodic oxidation is included in substrate surface and carries out anodic oxidation successively; dyeing and sealing of hole; obtain coloured anode oxide film; described protective layer used in electrolytic solution in coloured anodic oxidation and the preceding coloured anode oxide film that once forms are isolated; at least a portion of the coloured anode oxide film that forms before described laser sculpture is used to remove is exposed the surface of at least a portion base material.
2, method according to claim 1, wherein, described anodised method comprises with the base material being anode, with the electrolyzer is negative electrode, base material is carried out oxidation in electrolytic solution, described electrolytic solution is that concentration is the sulphuric acid soln of 150-210 grams per liter, and described anodised voltage is the 10-15 volt, and current density is 1-2A/dm
2, temperature is 18-22 ℃, the time is 20-60 minute.
3, method according to claim 1, wherein, described dyeing comprises and will flood through anodised base material that described dye liquor is the aqueous solution of dyestuff in dye liquor, described dyestuff is one or more in azoic dyestuff, anthraquinone dye and the peptide cyanine dyes.
4, method according to claim 3, wherein, the concentration of dyestuff is the 0.1-10 grams per liter in the described dye liquor, and the temperature of described dye liquor is 30-55 ℃, and the time of described dipping is 1-15 minute.
5, method according to claim 1, wherein, described sealing of hole comprises dyed base material is flooded that described hole sealing agent is one or more in nickel acetate, nickelous fluoride and the single nickel salt in the aqueous solution of hole sealing agent.
6, method according to claim 5, wherein, the concentration of described hole sealing agent is the 1-10 grams per liter, and the temperature of the aqueous solution of described hole sealing agent is 50-95 ℃, and the time of described dipping is 10-50 minute.
7, method according to claim 1, wherein, the material of described protective layer is one or more in acid and alkali-resistance printing ink, varnish and the cold coating, and described protective layer forms by the method for coating, and the thickness of described protective layer is the 5-50 micron.
8, method according to claim 1, wherein, described base material is a light metal material.
9, method according to claim 8, wherein, described base material is an aluminum or aluminum alloy.
10, method according to claim 1, wherein, this method also is included in carries out removing protective layer after last coloured anodic oxidation.
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