CN102330137B - Inorganic colorful electrolysis coloring technology for aluminium profile anodic oxide film - Google Patents
Inorganic colorful electrolysis coloring technology for aluminium profile anodic oxide film Download PDFInfo
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- CN102330137B CN102330137B CN201110258520.9A CN201110258520A CN102330137B CN 102330137 B CN102330137 B CN 102330137B CN 201110258520 A CN201110258520 A CN 201110258520A CN 102330137 B CN102330137 B CN 102330137B
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Abstract
The invention discloses an inorganic colorful electrolysis coloring technology for an aluminium profile anodic oxide film, which is characterized by comprising the following working procedures of: removing oil, etching by alkaline, oxidizing an anode, carrying out intermediate treatment and electrolysis coloring, and sealing holes, wherein the intermediate treatment working procedure is set between the working procedures of oxidizing an anode and electrolysis coloring and comprises three steps: a. DC (Direct Current) section: setting a supply voltage into a direct-current output mode, cleaning the micropores of the anodic oxide film, and reducing the thickness of a barrier layer, wherein a voltage value is 8-14V, and time is 20-50 seconds; b. AC (Alternating Current) section: setting the supply voltage into an alternating-current output mode, and generating a second layer of oxide film in the anodic oxide film; c. DC section: switching the supply voltage to the direct-current output mode, generating a third layer of film on the basis of the second layer of oxide film, wherein the voltage value is 10-20V, and operation time is controlled to 60-500s. According to the inorganic colorful electrolysis coloring technology, the existing electrolysis coloring equipment can be utilized to finish the full-color colorful electrolysis coloring aluminium or aluminium alloy in short time, and the inorganic colorful electrolysis coloring technology has the advantages of low production cost and good coloring quality.
Description
Technical field
The present invention relates to aluminium section bar building materials technology field, relate to a kind of processing method proposing polychrome electrolytic coloring on anodized aluminum alloy product in particular.
Background technology
Aluminium alloy is widely used in the numerous areas such as automobile, aerospace, building decoration, household electrical appliances, instrument, computer, mobile phone, haberdashery and hardware, has become consumption at present and has been only second to iron and steel and occupies the structural metallic materials of second.In order to improve aluminium alloy service life, meet the ornamental requirement of product appearance, Al-alloy products can increase substantially its surface hardness and corrosion resistance nature etc. by anodized surface process simultaneously, and therefore, anode oxidation process uses extremely extensive.
In order to improve the decorate properties of alloy product, aluminium alloy anode oxide film needed to carry out coloring treatment before sealing of hole.Common coloring treatment process is electrolytic coloring and chemical staining.Common electrolytic coloring is merely able to form the limited colors such as bronze-colored series, and color is single, ornamental poor, but good weatherability; Organic dye method can form coloury shades of colour, but the weathering resistance of Al-alloy products is poor, organic dye is easily aging causes alloy product efflorescence, affect work-ing life and the service safety of product, particularly for the boats and ships under ocean environment, freight container aluminium alloy, the various automobiles used under industrial environment, train, subway and other modes of transport aluminium alloy, its weathering resistance and erosion resistance require extremely strict.Therefore, how well ornamental and high-weatherability are realized to alloy product simultaneously, become one of aluminum alloy material surface process gordian technique needing development badly, cause extensive concern both domestic and external.
Summary of the invention
Object of the present invention in order to solve prior art deficiency and provide a kind ofly realize well ornamental with high-weatherability on aluminum alloy building section product simultaneously, change that traditional electrolytic coloring color is single, the inorganic colorful electrolysis coloring technology for aluminium profile anodic oxide film of the shortcoming of the easy efflorescence of organic dye coloring.
The present invention adopts following technical solution to realize above-mentioned purpose: a kind of inorganic colorful electrolysis coloring technology for aluminium profile anodic oxide film, it is characterized in that, comprise oil removing, alkaline etching, anodic oxidation, intermediate treatment operation, electrolytic coloring and sealing pores operation, anodic oxidation needs to carry out under certain conditions, and the intermediate treatment operation that arrangement one is special between anodic oxidation and electrolytic coloring.
Further illustrating as such scheme: the technique of described anodic oxidation operation is the mode adopting water cooling cooling, temperature is made to control at 18-22 DEG C, the sulphuric acid soln of tank liquor to be concentration be 10-200 grams per liter, anodizing time is 20-60 minute, and current density controls at 1.1-1.8A/dm
2.
The described intermediate treatment operation that arrangement one is special between anodic oxidation and electrolytic coloring, this operation is specifically divided into 3 steps:
A, DC section: make voltage of supply be arranged to direct current output mode, the object of this part is the micropore of anode purge oxide film and the thickness on reduction blocking layer, and magnitude of voltage is at 8-14V, and the time was at 20-50 seconds;
B, AC section: make voltage of supply be arranged to exchange output mode, this part is in order to regeneration second layer oxide film in anode oxide film; This part is divided into again three small steps:
B1, power supply wave shape used are alternating-current, and its magnitude of voltage is between 1-9v, and the operating time controls at 10-50s;
B2, power supply wave shape used are alternating-current, and its voltage is between 1-5v, and the operating time controls at 10-170s;
B3, power supply wave shape used are alternating-current, and its voltage is between 1-4v, and the operating time controls at 200-380s;
C, DC section: make voltage of supply be switched to direct current output mode, this part is in order to regeneration third layer film on the basis of the second tunic, which kind of color is this part decide, as long as change this part voltage and time parameter, just can obtain any one colour system in full spectral range; Its magnitude of voltage is between 10-20v, and the operating time controls at 60-500s, need determine according to concrete color.
In the described electrolytic coloring stage, this part is the deposition process of painted main salt, and its magnitude of voltage is between 12-20v, and the operating time controls at 150-300s.
After electrolytic coloring, arrange an operation again, increase the trickle color adjusting stage, same colour system, deep mixed shades of colour can be prepared; This stage is called DC section, and namely pass to suitable direct current, voltage range is at 5-18v; In addition, also comprise following pattern, i.e. repeating step a-c, i.e. DC-AC-DC-AC-DC-AC-DC again after electrolysis completes.
The intermediate treatment operation arranged between described anodic oxidation and electrolytic coloring is all carry out at painted groove, and namely only need prepare a painted groove, the Sn-Ni mixed salt that mainly consists of of its tank liquor adds color additive, and coloration temperature controls at 20 ~ 25 DEG C.
Described color additive, it is composed as follows:
Sulfuric acid: 15-30g/L
Weibull: 3-15g/L
Citric acid: 3-15g/L
Dihydroxy-benzene: 1-3g/L
Dimethyl sulfoxide (DMSO): doubly add by the 2-4 of Sn2+ concentration
Water: surplus.
The beneficial effect that the present invention adopts above-mentioned technical solution to reach is:
1, wide colour system, only needs appropriate change electrical parameter or time parameter just can obtain nearly all colour system.
2, technique is simple, and painted needs changes electrolyzer, is convenient to realize batch production.
3, power supply wave shape is simple, only needs a simple power output apparatus, uses common direct current and common sinusoidal waveform, only requires to control rise time of voltage or electric current well, and can be stabilized to expected value.
4, coloring stabilized, aberration is little, as long as control desired parameters well, color reproducibility is fine, and the aberration of painted oxide film is little.
5, be convenient to realize batch production, available existing electrolytic coloring production line implements the present invention, reduced investment, instant effect, is easy to apply.
6, cell liquid good stability, soon painted, and raw material consumption is few, and production cost is low.
Embodiment
A kind of inorganic colorful electrolysis coloring technology for aluminium profile anodic oxide film of the present invention, comprise oil removing, alkaline etching, anodic oxidation, intermediate treatment operation, electrolytic coloring and sealing pores operation, anodic oxidation needs to carry out under certain conditions, and the intermediate treatment operation that arrangement one is special between anodic oxidation and electrolytic coloring.The technique of anodic oxidation operation is the mode adopting water cooling cooling, makes temperature control at 18-22 DEG C, and the sulphuric acid soln of tank liquor to be concentration be 10-200 grams per liter, anodizing time is 20-60 minute, and current density controls at 1.1-1.8A/dm
2.
Between anodic oxidation and electrolytic coloring, arrange the intermediate treatment operation that is special, this operation is specifically divided into 3 steps:
A, DC section: make voltage of supply be arranged to direct current output mode, the object of this part is the micropore of anode purge oxide film and the thickness on reduction blocking layer, and magnitude of voltage is at 8-14V, and the time was at 20-50 seconds;
B, AC section: make voltage of supply be arranged to exchange output mode, this part is in order to regeneration second layer oxide film in anode oxide film; This part is divided into again three small steps:
B1, power supply wave shape used are alternating-current, and its magnitude of voltage is between 1-9v, and the operating time controls at 10-50s;
B2, power supply wave shape used are alternating-current, and its voltage is between 1-5v, and the operating time controls at 10-170s;
B3, power supply wave shape used are alternating-current, and its voltage is between 1-4v, and the operating time controls at 200-380s;
C, DC section: make voltage of supply be switched to direct current output mode, this part is in order to regeneration third layer film on the basis of the second tunic, which kind of color is this part decide, as long as change this part voltage and time parameter, just can obtain any one colour system in full spectral range; Its magnitude of voltage is between 10-20v, and the operating time controls at 60-500s, need determine according to concrete color.
Embodiment one
By 6063-T5 aluminium alloy test piece (its specification is that the Thin Rectangular of 200mm × 15mm is dull and stereotyped) through conventional oil removing, carry out in the NaOH solution of 60 DEG C alkaline etching, in and bright dipping, after washing, then be in the sulphuric acid soln of 190 grams per liters in concentration, control temperature 18 scholar 2 DEG C, volts DS 15 volts, current density 1.3 pacifies/decimetre
2, carry out the anodic oxidation treatment of 25 minutes, obtain the oxide film of about 12um, finally wash, for subsequent use.
Then in electrolytic colouring liquid, carry out electrolytic coloring process, electrolytic coloring tank liquor composition and painted after colour index list in table one. this part operation will experience following four steps, as follows:
1.DC section: make voltage of supply be arranged to direct current output mode, then makes voltage rise to 11V from 0V, then keeps 20 seconds at this magnitude of voltage of 11V within the time of 0-10 second.
2.AC section, this part is divided into again 3 small steps, as follows respectively:
A.AC(6V) section, the common sinusoidal ac of this part, within 0-5 second, makes voltage rise to 6V from 0V, then keeps 25 seconds on this 6V magnitude of voltage;
B.AC(4V) section, this part, equally with common sinusoidal ac, in 3 seconds, makes voltage drop to 4V from 6V, then keeps 90 seconds on this 4V magnitude of voltage;
C.AC(2.8V) section, this part, equally with common sinusoidal ac, in 3 seconds, makes voltage drop to 2.8V from 4V, then keeps 280 seconds on this 2.8V magnitude of voltage;
3.DC section: make voltage of supply be switched to direct current output mode, then (decide which kind of color, as long as change this part, just can obtain any one colour system in whole body system) in 25 seconds, make voltage rise to 13V from 0V, then keep 60 seconds on this magnitude of voltage;
4.AC section: the electrolytic coloring stage, this part is the deposition process of painted main salt, makes voltage of supply be switched to common interchange output mode, in 25 seconds, in 25 seconds, makes voltage rise to 16V from 0V, then keeps 210 seconds on this magnitude of voltage.
After above step, workpiece surface can be made to obtain the color of light slate gray, then adopt conventional middle temperature sealing of hole, in pore-sealing liquid, soak 30min.Through every test, show: the color reproducibility of painted oxide film is good, aberration deviation is little (Δ E≤3.5), and the light slate gray aluminium alloy type section product over-all properties index of preparation all meets the requirement of GB5237.2-2008 national standard, adopt 313B fluorescent ultraviolet lamp artificial accelerated aging test test, after 300h irradiates, aberration reaches 1 grade, and ageing-resistant performance is better than spray-on coating aluminium section bar.
Embodiment two
Concrete step is substantially with embodiment one, just step 3 is appropriately adjusted: changed 355 seconds in the 13V galvanic hold-time into from 60 seconds, after above step, workpiece surface can be made to obtain bottle-green color, then conventional middle temperature sealing of hole is adopted, 30min is soaked in pore-sealing liquid, through every test, show: the color reproducibility of painted oxide film is good, aberration deviation little (Δ E≤3.5), and the deep green aluminium alloy type section product over-all properties index of preparation all meets the requirement of GB5237.2-2008 national standard, adopt 313B fluorescent ultraviolet lamp artificial accelerated aging test test, after 300h irradiates, aberration reaches 1 grade, ageing-resistant performance is better than spray-on coating aluminium section bar.
Embodiment three
Concrete step is substantially with embodiment one, just suitable amendment is done to step 3: changed 425 seconds in the 13V galvanic hold-time into from 60 seconds, after above step, workpiece surface can be made to obtain mauve color, then conventional middle temperature sealing of hole is adopted, 30min is soaked in pore-sealing liquid, through every test, show: the color reproducibility of painted oxide film is good, aberration deviation little (Δ E≤3.5), and the red-purple aluminium alloy type section product over-all properties index of preparation all meets the requirement of GB5237.2-2008 national standard, adopt 313B fluorescent ultraviolet lamp artificial accelerated aging test test, after 300h irradiates, aberration reaches 1 grade, ageing-resistant performance is better than spray-on coating aluminium section bar.
Embodiment four
Concrete step is substantially with embodiment one, just suitable amendment is done to step 3: changed 195 seconds in the 13V galvanic hold-time into from 60 seconds, after above step, workpiece surface can be made to obtain flavous color, then conventional middle temperature sealing of hole is adopted, 30min is soaked in pore-sealing liquid, through every test, show: the color reproducibility of painted oxide film is good, aberration deviation little (Δ E≤3.5), and the golden yellow aluminium alloy product forms over-all properties index of preparation all meets the requirement of GB5237.2-2008 national standard, adopt 313B fluorescent ultraviolet lamp artificial accelerated aging test test, after 300h irradiates, aberration reaches 1 grade, ageing-resistant performance is better than spray-on coating aluminium section bar.
Embodiment five
Concrete step is substantially with embodiment one, just suitable amendment is done to step 3: changed 305 seconds in the 13V galvanic hold-time into from 60 seconds, after above step, workpiece surface can be made to obtain cyanic color, then conventional middle temperature sealing of hole is adopted, 30min is soaked in pore-sealing liquid, through every test, show: the color reproducibility of painted oxide film is good, aberration deviation little (Δ E≤3.5), and the cyanic colours aluminium alloy type section product over-all properties index of preparation all meets the requirement of GB5237.2-2008 national standard, adopt 313B fluorescent ultraviolet lamp artificial accelerated aging test test, after 300h irradiates, aberration reaches 1 grade, ageing-resistant performance is better than spray-on coating aluminium section bar.
Above-described is only the preferred embodiment of the present invention, it should be pointed out that for the person of ordinary skill of the art, and without departing from the concept of the premise of the invention, can also make some distortion and improvement, these all belong to protection scope of the present invention.
Claims (1)
1. an inorganic colorful electrolysis coloring technology for aluminium profile anodic oxide film, is characterized in that, it comprises oil removing, alkaline etching, anodic oxidation, intermediate treatment operation, electrolytic coloring stage, trickle color adjusting stage and sealing pores operation;
The technique of described anodic oxidation operation is the mode adopting water cooling cooling, and temperature controls at 18-22 DEG C, and anode oxidation process employing concentration is the sulphuric acid soln of 10-200 grams per liter, and anodizing time is 20-60 minute, and current density controls at 1.1-1.8A/dm
2;
The intermediate treatment operation arranged between described anodic oxidation and electrolytic coloring is all carry out at same painted groove, the Sn-Ni mixed salt that mainly consists of of the tank liquor of painted groove adds color additive, coloration temperature controls at 20 ~ 25 DEG C, wherein, and color additive composed as follows:
Sulfuric acid: 15-30g/L,
Weibull: 3-15g/L,
Citric acid: 3-15g/L,
Dihydroxy-benzene: 1-3g/L,
Dimethyl sulfoxide (DMSO): doubly add by the 2-4 of Sn2+ concentration,
Water: surplus;
Described intermediate treatment operation is specifically divided into following 3 steps:
A, DC section: make voltage of supply be arranged to direct current output mode, the micropore of anode purge oxide film and the thickness on reduction blocking layer, magnitude of voltage is at 8-14V, and the time is at 20-50s
B, AC section: make voltage of supply be arranged to exchange output mode, regeneration second layer oxide film in anode oxide film; This part is divided into three small steps:
B1, power supply wave shape used are alternating-current, and its voltage is between 1-9V, and the operating time controls at 10-50s;
B2, power supply wave shape used are alternating-current, and its voltage is between 1-5V, and the operating time controls at 10-170s;
B3, power supply wave shape used are alternating-current, and its voltage is between 1-4V, and the operating time controls at 200-380s;
C, DC section: make voltage of supply be switched to direct current output mode, regeneration third layer film on the basis of second layer oxide film, magnitude of voltage is between 10-20V, and the operating time controls at 60-500s;
The described electrolytic coloring stage is the deposition process of painted main salt, and its magnitude of voltage is between 12-20V, and the operating time controls at 150-300s;
The described trickle color adjusting stage, this stage is DC section, passes to direct current, and voltage range is at 5-18V; And repeating step a-c again after electrolysis completes.
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| CN103305888A (en) * | 2012-03-16 | 2013-09-18 | 苏州春兴精工股份有限公司 | Anodic oxidation treatment method for aerial aluminum alloy surface |
| CN102758235B (en) * | 2012-07-27 | 2015-08-19 | 肇庆亚洲铝厂有限公司 | Black colorant technique by a kind of aluminium section bar |
| CN107937962A (en) * | 2018-01-03 | 2018-04-20 | 广东坚美铝型材厂（集团）有限公司 | A kind of aluminium alloy extrusions coloring process |
| CN109468673A (en) * | 2018-12-16 | 2019-03-15 | 桂林理工大学 | A kind of aluminum alloy surface color method |
| CN109722698B (en) * | 2018-12-18 | 2021-02-09 | 佛山科学技术学院 | Interference coloring method for double-layer microstructure film on surface of aluminum alloy |
| CN110552039A (en) * | 2019-01-23 | 2019-12-10 | 深圳市鹏福创新五金有限公司 | secondary oxidation sealing process |
| CN110565141A (en) * | 2019-01-23 | 2019-12-13 | 深圳市鹏福创新五金有限公司 | Secondary oxidation sealing process |
| CN109989086B (en) * | 2019-04-19 | 2020-11-03 | 河北工业大学 | Preparation method of porous alumina photonic crystal film with high-saturation structural color |
| CN110699731A (en) * | 2019-09-30 | 2020-01-17 | 佛山科学技术学院 | Preparation method of aluminum alloy-based colorful composite oxide film with three-layer microstructure |
| CN110983407A (en) * | 2019-12-19 | 2020-04-10 | 佛山科学技术学院 | Preparation method for in-situ patterning of colorful composite oxide film on surface of aluminum alloy |
| CN112522760A (en) * | 2020-12-18 | 2021-03-19 | 东莞市新东明科技有限公司 | Method for removing nickel from anodic aluminum oxide alloy |
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