CN102181902B - Method for coloring aluminum and alloy surface thereof - Google Patents
Method for coloring aluminum and alloy surface thereof Download PDFInfo
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- CN102181902B CN102181902B CN 201110100145 CN201110100145A CN102181902B CN 102181902 B CN102181902 B CN 102181902B CN 201110100145 CN201110100145 CN 201110100145 CN 201110100145 A CN201110100145 A CN 201110100145A CN 102181902 B CN102181902 B CN 102181902B
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Abstract
The invention discloses a method for coloring aluminum and an alloy surface thereof, which comprises the following steps of: at first, cleaning and polishing the aluminum or the aluminum alloy surface; carrying out constant-pressure anode preoxidization for 20 minutes to 3 hours under the preoxidization voltage of 10 to 20 volts by using sulfuric acid electrolyte with the concentration of 0.1 to 3mol/liter under the conditions that the well-processed aluminum or aluminum alloy is used as an anode and graphite is used as a cathode; and then oxidizing the aluminum or the aluminum alloy by utilizing a voltage which varies periodically based on time to obtain a structurally laminar alumina photonic crystal, and coloring the aluminum or the aluminum alloy surface by the structural color of an optical forbidden band of the alumina photonic crystal, so that different colors can be adjusted within a scope of visible lights by maintaining constant time and changing the voltage only or maintaining constant voltage and changing time only. The coloration method of the invention has the advantages of no need of depositing metal ions, simple process and low cost, wide adjustment scope of colors and less pollution.
Description
Technical field
The present invention relates to the coloring process field that aluminium and alloy surface thereof utilize the anodic oxidation schemochrome, specifically a kind of aluminium and alloy surface thereof are carried out painted method.
Background technology
China was studied aluminum and its alloy coloring mechanism and oxidation film coloring technology since the eighties in 20th century, and the most widely used aluminum and its alloy colorize method is the electrolytic coloring of anodic oxidation method at present.Electrolytic oxidation combines anodic oxidation and electrochemical deposition process, the at first oxidation in acid solution aluminium flake or aluminum alloy sheet, form cellular porous oxide film, then in containing the solution of ionizable metal salt, carry out electrolysis treatment, under electric field action, metal ion is deposited in the hole of oxide film.Different electrolytic coloring of anodic oxidation according to metal refining salt mainly are divided into nickel salt, pink salt, mantoquita electrolytic coloring, and the color that these several metal deposition go out mainly is yellow-brown-black system and bluish-green colour system.The problems such as electrolytic coloring of anodic oxidation exists that color is single, the stability of complex process, coloring liquid and bad dispersibility never obtain fine solution.
Photonic crystal refers to have a class novel material of photonic band gap and energy gap.If the dielectric material that will have a differing dielectric constant by certain periodic arrangement, can occur being similar to semi-conductor forbidden band " photonic band gap " in the space.Light in the photonic band gap is reflected and forms schemochrome is the painted ultimate principle of photonic crystal.Because aluminum oxide photon crystal of the prior art adopts the electric current preparation, can't on the aluminum or aluminum alloy base, directly develop the color, equipment cost is high, and because relevant with sample area and can't be applied on the complex-shaped part, therefore, the concept of aluminum oxide photon crystal is not applied on the aluminum or aluminum alloy coloring process at present.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, provide a kind of aluminium and alloy surface thereof are carried out painted method, the present invention has that technique is simple, stable, environmental protection, color adaptation wide ranges, regulating measure advantage easily.
The present invention program's design considerations:
The stratiform three-dimensional aluminum oxide photon crystal film that anodic oxidation forms, when the light vertical incidence, its photonic band gap performance can represent with the Bragg-Snell formula of following simplification:
2dn
eff＝m
iλ
i
Wherein, d is perpendicular to the interlamellar spacing of sample surfaces; m
iBe positive integer, the progression of corresponding each absorption peak; λ
iIt is the wavelength of each absorption peak; n
EffIt is the effective refractive index of sample.Therefore, by regulating course spacing d value, can accurately regulate linearly the spectral reflectance peak position of sample, namely regulate distinct colors.Therefore, the present invention changes interlamellar spacing d value by regulating oxidization time or periodic voltage, just can be in light be seen optical band the different colours on the painted aluminum or aluminum alloy of fine adjustment surface.
The present invention is achieved by the following technical solutions:
A kind of aluminium and alloy surface thereof are carried out painted method, comprise the steps:
(1) at first Cleaning and polishing is carried out on the aluminum or aluminum alloy surface;
(2) working concentration is the sulfuric acid electrolyte of 0.1～3 mol/L, and take the above-mentioned aluminum or aluminum alloy of handling well as anode, graphite is negative electrode, carries out the preoxidation of constant voltage anode, 10～20 volts of preoxidation voltages, preoxidation time 20 minutes～3 hours;
(3) recycling is in time periodically variable voltage oxidation is carried out on above-mentioned aluminum or aluminum alloy surface, obtain the aluminum oxide photon crystal of laminate structure, utilize the schemochrome of its photonic band gap to realize painted to the aluminum or aluminum alloy surface, and certain by the hold-time, only change voltage or sustaining voltage is certain, change time, can control the different laminate structures of aluminum oxide photon crystal, thereby regulate aluminum or aluminum alloy surface distinct colors.
Described step is periodically variable voltage in (3) in time, comprises that in one-period sinusoidal rising, high pressure keep, straight line descends and two sinusoidal declines, is total to double teachers: time t
1In, voltage is by U
1Sine rises to U
2, at U
2Hold-time is t
2, then at time t
3Interior by U
2Straight line drops to U
3, subsequently at time t
4Interior from U
3Sine drops to U
4, at last at time t
5Interior by U
4Roll back U under sinusoidal
1, time t wherein
1Span is 25～250 seconds, t
2Be 25～250 seconds, t
3Be 12～125 seconds, t
4Be 40～400 seconds, t
5Be 145～1450 seconds, voltage U
1Value between 3～13 volts, U
2Between 7～30 volts, U
3Between 5～22 volts, U
4Between 4～15 volts.
The temperature of described preoxidation and heat-tinting is 0～5 ℃.
Voltage is the number of plies that periodically variable cycle life is the stratiform aluminum oxide photon crystal in time in the described step (3), can control aluminum or aluminum alloy surface color color and luster, and preferably the cycle life of the present invention's employing is 50～300 times.
During the surperficial red coloration of described aluminum or aluminum alloy, in the one-period, time t
1～t
5Value be respectively voltage U 120 seconds, 120 seconds, 60 seconds, 220 seconds and 680 seconds
1～U
5Value be respectively 6.5 volts, 14.5 volts, 11 volts, 7.5 volts, 6.5 volts.
When described aluminum or aluminum alloy surface purple, in the one-period, time t
1～t
5Value be respectively voltage U 85 seconds, 85 seconds, 42.5 seconds, 150 seconds and 485 seconds
1～U
5Value be respectively 6.5 volts, 14.5 volts, 11 volts, 7.5 volts, 6.5 volts.
When described aluminum or aluminum alloy surface blueness, in the one-period, time t
1～t
5Value be respectively voltage U 120 seconds, 120 seconds, 60 seconds, 220 seconds and 680 seconds
1～U
5Value be respectively 6.5 volts, 13.5 volts, 10.5 volts, 7.5 volts, 6.5 volts.
When described aluminum or aluminum alloy surface blueness, in the one-period, time t
1～t
5Value be respectively voltage U 100 seconds, 100 seconds, 50 seconds, 180 seconds and 570 seconds
1～U
5Value be respectively 6.5 volts, 14.5 volts, 11 volts, 7.5 volts, 6.5 volts.
During the surperficial embrown of described aluminum or aluminum alloy, in the one-period, time t
1～t
5Value be respectively voltage U 120 seconds, 120 seconds, 60 seconds, 220 seconds and 680 seconds
1～U
5Value be respectively 6.5 volts, 12.5 volts, 10 volts, 7.5 volts, 6.5 volts.
During the surperficial embrown of described aluminum or aluminum alloy, in the one-period, time t
1～t
5Value be respectively voltage U 70 seconds, 70 seconds, 35 seconds, 126 seconds and 400 seconds
1～U
5Value be respectively 6.5 volts, 14.5 volts, 11 volts, 7.5 volts, 6.5 volts.
Compared with prior art, the present invention has following advantage and beneficial effect:
(1) the present invention has solved the Controllability of aluminum oxide photon crystal scale operation innovatively by the voltage analog method, high with respect to cost, can not be applied to the electric current control method of obform body, voltage analog method of the present invention only needs regulating cycle voltage or oxidization time, have with low costly, equipment is simple, is fit to scale operation, and can be applicable to the advantage of various structural shape complex samples, greatly improved its feasibility that is applied to produce.
(2) the inventive method only needs oxidation step to finish, saved the in the past electrochemical deposition step of electrolytic coloring of anodic oxidation, therefore not only greatly simplified coloring process, and there are not a problem of the unstable and bad dispersibility of electrolytic solution in the electrolytic coloring, painted good reproducibility, process stabilizing, and present method does not relate to the metal-salt deposit fluid of any high pollution, do not add any coating dyestuff, only use the dilution heat of sulfuric acid of reusable edible, therefore environment friendly and pollution-free.
(3) colorize method of the present invention effectively solves the single problem of color, the different colours on the painted aluminum or aluminum alloy of fine adjustment surface in light is seen optical band.
(4) in the colorize method of the present invention voltage to be in time periodically variable cycle life be 50～300 times, the color and luster that can effectively control the aluminum or aluminum alloy surface is attractive in appearance.
Description of drawings
Fig. 1 is voltage curve and the current curve diagram of oxidising process among the embodiment 1.
Fig. 2 is the visible transmission spectrogram of aluminum oxide coloring film among embodiment 1 and the embodiment 2.
Fig. 3 is the visible reflectance spectrogram of painted aluminium flake among embodiment 1 and the embodiment 2.
Embodiment
The invention will be further described below in conjunction with embodiment, but the scope of protection of present invention is not limited to the scope of embodiment statement.
Embodiment 1:
The present embodiment is implemented under following technical requirements condition:
(1) being that high-purity aluminium flake of 99.999% is cut into 6cm * 7.5cm with the purity of thickness 0.3mm, is to carry out electropolishing in the solution that mixes at 4: 1 at ethanol and perchloric acid volume ratio.Polishing time 3 minutes, voltage 21V.
(2) under 0 ℃, working concentration be the sulphuric acid soln of 1.1 mol/L as electrolytic solution, aluminium is anode, graphite is negative electrode, carries out anodic oxidation, the oxidation area is the rectangle of 5cm * 6.5cm.Concrete oxidising process is as follows: at first the preoxidation of 14V constant voltage is 1 hour, then utilizes periodic voltage to carry out oxidation.The periodic voltage waveform of one-period is: rose to 14.5V from the 6.5V sine in 85 seconds, and kept 85 seconds, then in 42.5 seconds, drop to 11V from the 14.5V straight line, in 150 seconds, drop to 7.5V from the 11V sine subsequently, in 485 seconds, drop to 6.5V from the 7.5V sine at last.Periodic voltage repeats 140 times, and the oxidising process voltage-current curve as shown in Figure 1.
Implement above method, can obtain evenly purple coloring film attractive in appearance of color and luster.As shown in Figure 2, coloring film visible transmission bands of a spectrum gap is at 476nm, intensity 0.1%.Painted aluminium reflection peak is positioned at 483nm, and intensity reaches 93.3%, as shown in Figure 3.
Embodiment 2:
The present embodiment is implemented under following technical requirements condition:
Under 1 ℃, other condition is identical with embodiment 1, periodically the oxidation voltage waveform becomes: rose to 14.5V from the 6.5V sine in 120 seconds, and kept 120 seconds, then in 60 seconds, drop to 11V from the 14.5V straight line, in 220 seconds, drop to 7.5V from the 11V sine subsequently, in 680 seconds, drop to 6.5V from the 7.5V sine at last.Periodic voltage repeats 105 times.
Implement above step and can obtain painted bright-coloured uniform red colored film.As shown in Figure 2, coloring film visible transmission bands of a spectrum gap is at 620nm, intensity 3.5%.Painted aluminium reflection peak is positioned at 656nm, and intensity reaches 92.3%, as shown in Figure 3.
Embodiment 3:
The present embodiment is implemented under following technical requirements condition:
Under 2 ℃, other condition is identical with embodiment 1, periodically the oxidation voltage waveform becomes: rose to 13.5V from the 6.5V sine in 120 seconds, and kept 120 seconds, then in 60 seconds, drop to 10.5V from the 13.5V straight line, in 220 seconds, drop to 7.5V from the 10.5V sine subsequently, in 680 seconds, drop to 6.5V from the 7.5V sine at last.Periodic voltage repeats 105 times.
Implement above method, can obtain evenly blue-colored film attractive in appearance of color and luster.
Embodiment 4:
The present embodiment is implemented under following technical requirements condition:
Under 3 ℃, other condition is identical with embodiment 1, periodically the oxidation voltage waveform becomes: rose to 12.5V from the 6.5V sine in 120 seconds, and kept 120 seconds, then in 60 seconds, drop to 10V from the 12.5V straight line, in 220 seconds, drop to 7.5V from the 10V sine subsequently, in 680 seconds, drop to 6.5V from the 7.5V sine at last.Periodic voltage repeats 105 times.
Implement above method, can obtain evenly brown coloring film attractive in appearance of color and luster.
Embodiment 5:
The present embodiment 5 is implemented under following technical requirements condition:
Be that 6061 aluminium alloy is implemented anode oxidation coloration to model.Under 4 ℃, use the sulfuric acid of 1.1 mol/L as electrolytic solution, aluminium alloy is anode, graphite is negative electrode, carries out anodic oxidation.Concrete oxidising process is as follows: at first the preoxidation of 14V constant voltage is 1 hour, then utilizes periodic voltage to carry out oxidation.The oxidation voltage waveform of one-period is as follows: rose to 14.5V from the 6.5V sine in 100 seconds, and kept 100 seconds, then in 50 seconds, drop to 11V from the 14.5V straight line, in 180 seconds, drop to 7.5V from the 11V sine subsequently, in 570 seconds, drop to 6.5V from the 7.5V sine at last.Periodic voltage repeats 120 times.Implement above step and can obtain uniform coloring blue-colored film attractive in appearance in aluminum alloy surface.
Embodiment 6:
The present embodiment is implemented under following technical requirements condition:
Be that 6061 aluminium alloy carries out anode oxidation coloration to model.Under 5 ℃, other condition is identical with embodiment 5, periodically the oxidation voltage waveform becomes: rose to 14.5V from the 6.5V sine in 70 seconds, and kept 70 seconds, then in 35 seconds, drop to 11V from the 14.5V straight line, in 126 seconds, drop to 7.5V from the 11V sine subsequently, in 400 seconds, drop to 6.5V from the 7.5V sine at last.Periodic voltage repeats 170 times.Implement above step, can obtain uniform coloring brown coloring film attractive in appearance in aluminum alloy surface.
Above-described embodiment is the better embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (8)
1. one kind is carried out painted method to aluminium and alloy surface thereof, it is characterized in that, comprises the steps:
(1) at first Cleaning and polishing is carried out on the aluminum or aluminum alloy surface;
(2) working concentration is the sulfuric acid electrolyte of 0.1 ~ 3 mol/L, and take the above-mentioned aluminum or aluminum alloy of handling well as anode, graphite is negative electrode, carry out the preoxidation of constant voltage anode, 10 ~ 20 volts of preoxidation voltages, preoxidation time 20 minutes ~ 3 hours, the temperature of preoxidation is 0～5 ℃;
(3) recycling is in time periodically variable voltage oxidation is carried out on above-mentioned aluminum or aluminum alloy surface, and the temperature of oxidation is 0～5 ℃, obtains the aluminum oxide photon crystal of laminate structure; Described being in time in the periodically variable voltage comprises in the one-period that sinusoidal rising, high pressure keep, straight line descends and two sinusoidal declines, is total to double teachers: time t
1In, voltage is by U
1Sine rises to U
2, at U
2Hold-time is t
2, then at time t
3Interior by U
2Straight line drops to U
3, subsequently at time t
4Interior from U
3Sine drops to U
4, at last at time t
5Interior by U
4Roll back U under sinusoidal
1, time t wherein
1Span is 25 ~ 250 seconds, t
2Be 25 ~ 250 seconds, t
3Be 12 ~ 125 seconds, t
4Be 40 ~ 400 seconds, t
5Be 145 ~ 1450 seconds, voltage U
1Be 3 ~ 13 volts, U
2Be 7 ~ 30 volts, U
3Be 5 ~ 22 volts, U
4It is 4 ~ 15 volts.
2. method according to claim 1 is characterized in that, it is 50 ~ 300 times that the middle voltage of described step (3) is periodically variable cycle life in time.
3. method according to claim 2 is characterized in that, during the red coloration of described aluminum or aluminum alloy surface, and in the one-period, time t
1～t
5Value be respectively voltage U 120 seconds, 120 seconds, 60 seconds, 220 seconds and 680 seconds
1～U
4Value be respectively 6.5 volts, 14.5 volts, 11 volts, 7.5 volts.
4. method according to claim 2 is characterized in that, when described aluminum or aluminum alloy surface purple, and in the one-period, time t
1～t
5Value be respectively voltage U 85 seconds, 85 seconds, 42.5 seconds, 150 seconds and 485 seconds
1～U
4Value be respectively 6.5 volts, 14.5 volts, 11 volts, 7.5 volts.
5. method according to claim 1 is characterized in that, when described aluminum or aluminum alloy surface blueness, and in the one-period, time t
1～t
5Value be respectively voltage U 120 seconds, 120 seconds, 60 seconds, 220 seconds and 680 seconds
1～U
4Value be respectively 6.5 volts, 13.5 volts, 10.5 volts, 7.5 volts.
6. method according to claim 2 is characterized in that, when described aluminum or aluminum alloy surface blueness, and in the one-period, time t
1～t
5Value be respectively voltage U 100 seconds, 100 seconds, 50 seconds, 180 seconds and 570 seconds
1～U
4Value be respectively 6.5 volts, 14.5 volts, 11 volts, 7.5 volts.
7. according to claim 2 described methods, it is characterized in that, during the embrown of described aluminum or aluminum alloy surface, in the one-period, time t
1～t
5Value be respectively voltage U 120 seconds, 120 seconds, 60 seconds, 220 seconds and 680 seconds
1～U
4Value be respectively 6.5 volts, 12.5 volts, 10 volts, 7.5 volts.
8. according to claim 2 described methods, it is characterized in that, during the embrown of described aluminum or aluminum alloy surface, in the one-period, time t
1～t
5Value be respectively voltage U 70 seconds, 70 seconds, 35 seconds, 126 seconds and 400 seconds
1～U
4Value be respectively 6.5 volts, 14.5 volts, 11 volts, 7.5 volts.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI553165B (en) * | 2015-07-17 | 2016-10-11 | 國立成功大學 | Coloring method by dye-free and one-time anodic-aluminum oxidizing process and substrate made therefrom |
| TWI577838B (en) * | 2015-07-17 | 2017-04-11 | 國立成功大學 | Identification barcode is made from dye-free and one-time anodic-aluminum oxidizing process |
| WO2020074754A1 (en) * | 2018-10-10 | 2020-04-16 | Mapsa S. Coop. | Method for surface treatment of a piece of aluminum alloy and a piece made of anodized aluminum alloy |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732933A (en) * | 2012-04-01 | 2012-10-17 | 华南理工大学 | Aluminum material anodization electrolytic coloring method for achieving multiple colors in one tank |
| CN104073857A (en) * | 2014-06-18 | 2014-10-01 | 华南理工大学 | Preparation method of nanoimprint nickel seal |
| RU2620801C1 (en) * | 2015-12-28 | 2017-05-29 | Кирилл Сергеевич Напольский | Method of forming coloured decorative coating by anodisation |
| CN107620104A (en) * | 2017-09-30 | 2018-01-23 | 佛山科学技术学院 | The preparation method of AAO photonic crystal coating for selective absorption of sunlight spectrum |
| CN108660496B (en) * | 2018-05-02 | 2019-12-03 | 珠海市美图金属科技有限公司 | A kind of profile heat tinting process |
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| EP0605354B1 (en) * | 1992-12-31 | 1996-10-30 | Novamax Technologies Holdings Inc. | A process for obtaining a range of colours of the visible spectrum using electrolysis on anodized aluminium |
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| EP0605354B1 (en) * | 1992-12-31 | 1996-10-30 | Novamax Technologies Holdings Inc. | A process for obtaining a range of colours of the visible spectrum using electrolysis on anodized aluminium |
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Non-Patent Citations (1)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI553165B (en) * | 2015-07-17 | 2016-10-11 | 國立成功大學 | Coloring method by dye-free and one-time anodic-aluminum oxidizing process and substrate made therefrom |
| TWI577838B (en) * | 2015-07-17 | 2017-04-11 | 國立成功大學 | Identification barcode is made from dye-free and one-time anodic-aluminum oxidizing process |
| WO2020074754A1 (en) * | 2018-10-10 | 2020-04-16 | Mapsa S. Coop. | Method for surface treatment of a piece of aluminum alloy and a piece made of anodized aluminum alloy |
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