EP1207221A1 - Verfahren zur elektrolytischen beschichtung von aluminiummaterial - Google Patents

Verfahren zur elektrolytischen beschichtung von aluminiummaterial Download PDF

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Publication number
EP1207221A1
EP1207221A1 EP00939163A EP00939163A EP1207221A1 EP 1207221 A1 EP1207221 A1 EP 1207221A1 EP 00939163 A EP00939163 A EP 00939163A EP 00939163 A EP00939163 A EP 00939163A EP 1207221 A1 EP1207221 A1 EP 1207221A1
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EP
European Patent Office
Prior art keywords
coloring
voltage
aluminum material
current
alternating current
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Application number
EP00939163A
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English (en)
French (fr)
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EP1207221A4 (de
Inventor
Ken c/o Nippon Light Metal Co. Ltd. EBIHARA
Daisuke c/o Nippon Light Metal Co. Ltd. NAGASAWA
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Nippon Light Metal Co Ltd
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Nippon Light Metal Co Ltd
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Publication date
Priority claimed from JP17956499A external-priority patent/JP3379482B2/ja
Priority claimed from JP17956399A external-priority patent/JP3379481B2/ja
Application filed by Nippon Light Metal Co Ltd filed Critical Nippon Light Metal Co Ltd
Publication of EP1207221A1 publication Critical patent/EP1207221A1/de
Publication of EP1207221A4 publication Critical patent/EP1207221A4/de
Withdrawn legal-status Critical Current

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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
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C25D11/20—Electrolytic after-treatment
    • C25D11/22—Electrolytic after-treatment for colouring layers

Definitions

  • This invention relates to a process for electrolytically coloring an aluminum material consisting of anodized aluminum or an anodized aluminum alloy (hereinafter simply referred to as "aluminum material"); more particularly, this invention relates to a process for electrolytically coloring an aluminum material which can attain uniformity in color tone during alternating current electrolytic coloring and, still more, to a process for electrolytically coloring an aluminum material which can keep the color tone from changing irregularly not only in a given energizing lot but also in different energizing lots during electrolytic coloring thereby producing an aluminum material colored in a uniform tone.
  • aluminum material an aluminum material consisting of anodized aluminum or an anodized aluminum alloy
  • An aluminum material is used frequently in many areas such as construction materials, vehicle parts and furniture on account of its good processability and corrosion resistance and, for the purpose of enhancing the aesthetic effect of the material, electrolytic coloring has been practiced wherein an aluminum material is subjected to electrolysis in an electrolyte containing a soluble salt of metal such as Ni, Co, Cu, and Sn thereby causing the electrolysis product of the metal salt to deposit in the porous anodic oxide film.
  • a soluble salt of metal such as Ni, Co, Cu, and Sn
  • alternating current electrolytic coloring (Asada process) wherein an alternating current is passed through an electrolyte to effect electrolysis and direct current electrolytic coloring wherein a direct current is passed through an electrolyte.
  • Ada process alternating current electrolytic coloring
  • direct current electrolytic coloring wherein a direct current is passed through an electrolyte.
  • This pretreatment prior to coloring by constant voltage electrolysis aims at eliminating irregular coloring by passing a direct current at constant voltage for a certain length of time thereby making the resistance of the anodic oxide film uniform in various parts and creating a condition for a relatively uniform current to flow through the oxide film during alternating current electrolytic coloring which follows the pretreatment; this process is commercially admissible in the cases in which an aluminum material is electrolytically colored in a relatively dark tone.
  • Another process proposes the following procedure for electrolytic coloring of an aluminum material; a stable color tone is attained by repeating passage and stoppage of electric current in multiple stages intermittently and meanwhile setting the voltage successively higher from one stage to the subsequent stage [Japan Kokai Tokkyo Koho Hei 8-41,685 (1996)]. It is said that the process undoubtedly attains a stable color tone and additionally shortens the time required for coloring in black, and controls the influence of trace amounts of impurities thereby preventing white streak defects.
  • Any of the aforementioned processes can attain a relatively stable color tone in a given energizing lot, but is unable to control irregularities in color tone in different energizing lots completely and, in consequence, produces with difficulty an aluminum material colored in a uniform tone in different energizing lots.
  • alternating current electrolytic coloring which is effected by changing the total current density that is the sum total of the absolute values of positive and negative current densities of the current waveform stepwise from the first step to at least the fourth step [Japan Tokkyo Koho Hei 3-32,637 (1991)].
  • This process can somehow manage to do as much as keeping the difference in color tone from becoming real in the case of electrlolytic coloring of an aluminum material in a relatively light tone.
  • the present inventors have conducted studies to develop a process for producing an aluminum material colored in a uniform tone stably and commercially advantageously while preventing irregular coloring in different energizing lots as much as possible in alternating current electrolytic coloring and found that a uniform color tone can be attained in different energizing lots even in electrolytic coloring in a relatively light tone by performing a pretreatment prior to coloring that precedes alternating current electrolytic coloring until the voltage and current respectively reach the preset ultimate values.
  • the bath voltage in the pretreatment prior to coloring is affected by the temperature and pH of the electrolytic coloring bath and, still more, by the water washing time and the pH of the water washing bath during the step for water washing of the anodized aluminum material before immersion in the electrolytic coloring bath (the aforementioned conditions are hereinafter collectively referred to as "the bath conditions") and the bath voltage changes with the bath conditions.
  • the bath voltage in the pretreatment prior to coloring by constant current electrolysis is decided primarily by the resistance of the electrolytic coloring bath and the resistance of the anodic oxide film on the surface of aluminum material immersed in the bath.
  • changes in the resistance of the electrolytic coloring bath from energizing lot to energizing lot are not very large, at most 0.1-0.2 V in terms of the corresponding voltage, changes in the bath voltage in the pretreatment prior to coloring are considered to be due chiefly to the resistance of the anodic oxide film.
  • the anodic oxide film on the surface of aluminum material consists of the so-called "barrier layer” which is a fine aluminous layer formed on the aluminum substrate of an aluminum material and a porous layer formed on the barrier layer and the resistance of the anodic oxide film is practically that of the barrier layer.
  • the efficiency for formation of the barrier layer in the pretreatment prior to coloring by constant current electrolysis is considered to be 60% or so in terms of apparent efficiency that is the ratio of the theoretical amount formed with the current efficiency assumed to be 100% to the actual amount increased with the dissolution of the barrier layer taken into account (amount increased/theoretical amount formed).
  • apparent efficiency changes under the influence of the bath conditions like the aforementioned bath voltage in the pretreatment prior to coloring; as a result, the resistance of the anodic oxide film on the surface of aluminum material changes from energizing lot to energizing lot.
  • the present inventors have conducted studies to find a commercially adequate solution to the aforementioned problem, found that the thickness of the barrier layer of the anodic oxide film to be formed and adjusted in the pretreatment prior to coloring is dependent on the ultimate voltage and current to be reached finally in the pretreatment, for example, the thickness in question is proportional to the ultimate voltage in the case of the pretreatment prior to coloring by constant current electrolysis, and, as a result, the thickness of the barrier layer is directly related to the color tone given to the aluminum material by alternating current electrolytic coloring, and completed this invention.
  • an object of this invention is to provide a process for electrolytically coloring an aluminum material which is capable of preventing as much as possible irregularities in coloring not only in a given energizing lot but also in different energizing lots in alternating current electrolytic coloring of an aluminum material and producing an aluminum material colored in a uniform tone stably and easily on a commercial scale.
  • this invention relates to an improved process for electrolytically coloring an aluminm material which comprises performing said pretreatment prior to coloring until the voltage and current respectively reach the preset ultimate voltage and current.
  • a particularly desirable mode of execution of the process for electrolytically coloring an aluminum material comprises performing a pretreatment prior to coloring by constant current electrolysis wherein a direct current is passed until the voltage reaches the ultimate value while maintaining the current at the preset ultimate value and then performing alternating current electrolytic coloring wherein a voltage-controlled alternating current waveform that has the peak voltage 0.55-0.8 times the final voltage in the pretreatment prior to coloring by constant current electrolysis is passed through the aluminum material.
  • an aluminum material to be electrolytically colored in this invention there is no specific restriction on an aluminum material to be electrolytically colored in this invention and, as in the conventional anodizing, a direct current, an alternating current, or an alternating current superimposed on a direct current is passed through an electrolytic bath containing an aqueous solution of acid such as sulfuric acid, oxalic acid, sulfonic acid, and chromic acid with an aluminum raw material consisting of ordinary aluminum or an aluminum alloy serving as the anode to form an anodic oxide film on the surface of the aluminum raw material.
  • acid such as sulfuric acid, oxalic acid, sulfonic acid, and chromic acid
  • Soluble metal salts include inorganic salts such as sulfates, nitrates, phosphates, chlorides, and chromates and organic salts such as oxalates, acetates, and tartrates of metals such as nickel (Ni), cobalt (Co), copper (Cu), tin (Sn), chromium (Cr), magnesium (Mg), iron (Fe), cadmium (Cd), titanium (Ti), manganese (Mn), molybdenum (Mo), calcium (Ca), vanadium (V), lead (Pb), and zinc (Zn).
  • Soluble metal salts include inorganic salts such as sulfates, nitrates, phosphates, chlorides, and chromates and organic salts such as oxalates, acetates, and tartrates of metals such as nickel (Ni), cobalt (Co), copper (Cu), tin (Sn), chromium (Cr), magnesium
  • dithionites such as sodium dithionite and zinc dithionite
  • thiosulfates such as ammonium thiosulfate and sodium thiosulfate
  • hydrogen sulfites such as sodium hydrogen sulfite, sulfurous acid
  • sulfites such as sodium sulfite, thioglycolic acid
  • thioglycolates such as ammonium thioglycolate.
  • the pretreatment prior to coloring preceding alternating current electrolytic coloring in this invention is performed by immersing an aluminum material in the electrolytic coloring bath, passing a direct current waveform (that is, direct current or an alternating current superimposed on a direct current) with the aluminum material serving as the anode, and completing the operation at the point when the voltage (the peak voltage in case the direct current waveform is that of an alternating current superimposed on a direct current) and the current respectively reach the preset ultimate values.
  • a direct current waveform that is, direct current or an alternating current superimposed on a direct current
  • a concrete procedure is to pass a direct current while keeping the current at the preset value of ultimate current and terminate the pretreatment when the voltage reaches the preset value of ultimate voltage.
  • the current flows preferentially to the portion where the barrier layer of the anodic oxide film on the surface of aluminum material is relatively thin and offers a low resistance and to the portion near the cathode where the resistance of the bath is low; the barrier layers either get compensated for small thickness or grow relatively thicker by the amount corresponding to the difference in resistance of the bath in these portions and a constant anodic current distribution is obtained when the voltage reaches the ultimate value.
  • the ultimate voltage and current in the pretreatment prior to coloring varies with what color tone is required for the aluminum material as product; the ultimate voltage is preferably set at 30-50 V for electrolytic coloring in a relatively light tone or at 20-30 V for electrolytic coloring in a relatively dark tone and the ultimate current is preferably set in the range 20-50 A/m 2 .
  • this invention Upon completion of the pretreatment prior to coloring in this manner, this invention performs alternating current electrolytic coloring in the same electrolytic coloring bath by passing an alternating current waveform or a superimposed AC-DC waveform through the aluminum material.
  • the peak voltage of the alternating current waveform or superimposed AC-DC waveform in use is set at a value preferably 0.55-0.8 times, more preferably 0.65-0.75 times, the value of the preset ultimate voltage in the pretreatment prior to coloring. If the peak voltage is lower than 0.55 times, coloring does not occur or the rate of coloring becomes extremely low. On the other hand, if the peak voltage exceeds 0.8 times, the current becomes difficult to stay constant in alternating current electrolytic coloring and a uniform color tone cannot be obtained even if the time for treatment is fixed.
  • making the color tone uniform is nothing less than making the current distribution in the aluminum material uniform when electrolytic coloring is performed with the aluminum material serving as the anode.
  • the film resistance corresponding to the bath resistance in each part is generated and the current distribution of the aluminum material can be made constant and nearly uniform at the end of the pretreatment prior to coloring.
  • the present inventors have found that the changes in film resistance in alternating current electrolytic coloring is dependent on and closely related to the ratio of the final voltage in the current-controlled pretreatment prior to coloring to the peak voltage of the alternating current waveform in alternating current electrolytic coloring. That is, the current-controlled pretreatment prior to coloring is performed first by passing a direct current while regulating the final voltage and then alternating current electrolytic coloring is performed in the same electrolytic coloring bath by passing a voltage-controlled alternating current waveform having the peak voltage 0.55-0.8 times the final voltage in the aforementioned current-controlled pretreatment prior to coloring and this procedure makes it possible to obtain a uniform current distribution corresponding to the changes in film resistance at the end of the pretreatment prior to coloring and obtain a uniform color tone.
  • a preferable procedure is to scan the aluminum material pretreated and placed in the electrolytic coloring bath with alternating current voltage to plot a voltage-current curve, determine the boundary voltage E 0 that is the intersection of the respective extension lines of the flat region and the rising region in the curve, and set the peak voltage in alternating current electrolytic coloring at this boundary voltage E 0 .
  • the boundary voltage E 0 thus determined is normally 0.65-0.75 times the ultimate voltage preset in the current-controlled pretreatment prior to coloring and, although varying somewhat with the conditions for the pretreatment prior to coloring or other conditions (such as treatment of anodic oxide film and the subsequent water washing), it can be determined unambiguously as a suitable peak voltage of an alternating current waveform or a superimposed AC-DC waveform.
  • an electric current flows with ease in the parts near the counter electrode in the initial and intermediate stages of the pretreatment prior to coloring and the barrier layer grows there preferentially.
  • the film resistance increases as the barrier layer grows and the ease of flow of the current in this part is held in check. That is, preferential growth of the barrier layer in the part where the current flows with ease in the pretreatment prior to coloring helps to eliminate the difference in site-dependent ease of current flow in alternating current electrolytic coloring thereby causing the current to flow with a nearly uniform current distribution over the whole surface of the aluminum material in a given energizing lot and eliminating irregularities in color tone in a given energizing lot.
  • the aforementioned pretreatment prior to coloring is peformed until the voltage and current reach the preset ultimate values and, even if the bath conditions change in different energizing lots, the condition of the barrier layer finally adjusted by the pretreatment prior to coloring becomes constant in different energizing lots and the current flows with a nearly uniform current distribution over the whole surface of the aluminum material in different energizing lots and this eliminates irregularities in color tone in different energizing lots.
  • Fig. 1 is a voltage-current curve plotted in the determination of the boundary voltage E 0 in Example 1.
  • An aluminum raw material A6063S-T5
  • 20% H 2 SO 4 at a current density of 100 A/m 2 for 30 minutes to form an anodic oxide film with a thickness of 10 ⁇ m on the surface of the aluminum raw material and then washed in an acid bath at pH 1 for 5 minutes to prepare an aluminum material.
  • An electrolytic coloring bath composed of 25 g/l of CuSO 4 and 5 g/l of H 2 SO 4 was prepared and the aforementioned aluminum material was submitted to the current-controlled pretreatment prior to coloring with the aluminum material serving as the anode at a current density of 25 A/m 2 , a bath temperature of 25°C, and an ultimate voltage of 20 V for approximately 20 seconds.
  • the pretreated aluminum material was scanned with alternating current voltage in the same coloring bath while raising the peak voltage from 0 V at a rate of 1 V/sec and a voltage-current curve was plotted.
  • Alternating current electrolytic coloring was performed in the same coloring bath by setting the peak voltage of a commercial alternating current at this boundary voltage which is 14 V and passing the current for 50 seconds, 100 seconds, and 150 seconds to give the aluminum material electrolytically colored pink.
  • the current-controlled pretreatment prior to coloring and alternating current electrolytic coloring were performed as in the aforementioned Example 1 except using the the conditions and the peak voltage of a commercial alternating current shown in Table 1 to give the electrolytically colored aluminum material.
  • the constant voltage pretreatment prior to coloring was performed by placing the aluminum material as the anode, passing a direct current at a voltage of 15 V initially, switching the voltage over to 20 V thereafter at the point when the current density dropped to 32 A/m 2 , and continuing the operation until the final current density became 25 A/m 2 .
  • Example 2 Upon completion of the constant voltage pretreatment prior to coloring, the material was scanned with commerical alternating current voltage in the same electrolytic coloring bath as in Example 1 and a voltage-current curve was plotted. The results are similar to those in Example 1 and the boundary voltage E 0 determined from the intersection of the respective extension lines of the flat and rising region was 14 V.
  • Alternating current electrolytic coloring was performed in the same electrolytic coloring bath by setting the peak voltage of a commercial alternating current at this boundary voltage E 0 of 14 V and passing the current for 100 seconds to give the aluminum material electrolytically colored pink.
  • the colored aluminum material was submitted to color measurement to examine the uniformity of color tone (color difference; ⁇ E * ab ) in a given energizing lot. The results are shown in Table 1.
  • Example 1 The current-controlled pretreatment prior to coloring and alternating current electrolytic coloring were performed as in the aforementioned Example 1 except applying the peak voltage of a commercial alternating current shown in Table 1 and the electrolytically colored aluminum material thus obtained was examined for the uniformity of color tone as in Example 1. The results are shown in Table 1.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Coloring (AREA)
EP00939163A 1999-06-25 2000-06-26 Verfahren zur elektrolytischen beschichtung von aluminiummaterial Withdrawn EP1207221A4 (de)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
JP17956499 1999-06-25
JP17956499A JP3379482B2 (ja) 1999-06-25 1999-06-25 アルミニウム材の電解着色法
JP17956399 1999-06-25
JP17956399A JP3379481B2 (ja) 1999-06-25 1999-06-25 アルミニウム材の電解着色方法
PCT/JP2000/004179 WO2001000904A1 (fr) 1999-06-25 2000-06-26 Procede de coloration electrolytique d'un materiau en aluminium

Publications (2)

Publication Number Publication Date
EP1207221A1 true EP1207221A1 (de) 2002-05-22
EP1207221A4 EP1207221A4 (de) 2002-09-11

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EP00939163A Withdrawn EP1207221A4 (de) 1999-06-25 2000-06-26 Verfahren zur elektrolytischen beschichtung von aluminiummaterial

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EP (1) EP1207221A4 (de)
KR (1) KR100718427B1 (de)
CN (1) CN1200146C (de)
AU (1) AU5430200A (de)
CA (1) CA2377953A1 (de)
NO (1) NO20016306L (de)
WO (1) WO2001000904A1 (de)

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101509891B (zh) * 2009-04-01 2012-05-30 西南铝业（集团）有限责任公司 一种罐盖料转化膜均匀性检测方法
CN101831681B (zh) * 2010-06-04 2012-02-01 天津大学 一种铝合金着有色复合膜的制备方法
CN102330137B (zh) * 2011-09-03 2015-07-08 广亚铝业有限公司 铝型材阳极氧化膜无机彩色电解着色工艺
CN102534722B (zh) * 2011-11-28 2014-09-10 珠海市奥美伦精细化工有限公司 用于铝合金焊接区域、盲孔工件表面的染色前处理剂及其应用工艺
CN103076487B (zh) * 2013-01-10 2015-05-27 安徽省临泉县嘉柏列科技有限公司 大功率电池测试设备采样负载突变电压峰值算法
CN106480486A (zh) * 2015-08-26 2017-03-08 侊东Hitech株式会社 铝材的分级着色方法及利用其的铝材
CN110592638A (zh) * 2019-09-17 2019-12-20 佛山市海化表面处理科技有限公司 一种铝及铝合金的阳极氧化电解着色工艺
CN111876812B (zh) * 2020-08-01 2021-11-05 东莞市慧泽凌化工科技有限公司 一种无镍电解着色增黑添加剂及其使用方法
CN112301398B (zh) * 2020-09-29 2022-02-18 九牧厨卫股份有限公司 一种金色薄膜的制备方法

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1022927A (en) * 1966-12-12 1966-03-16 Tahei Asada Improvements in and relating to coloring aluminium articles by electrolytic depositions of colored compounds
JPS5423664B2 (de) * 1975-03-06 1979-08-15
JPS5825495A (ja) * 1981-08-05 1983-02-15 Mitsubishi Keikinzoku Kogyo Kk アルミニウムの電解着色方法
JPS59173294A (ja) * 1983-03-23 1984-10-01 Pilot Pen Co Ltd:The アルミニウム又はその合金の電解着色方法
DE3741456A1 (de) * 1987-12-08 1989-06-22 Erbsloeh Julius & August Verfahren zum elektrolytischen einfaerben anodisch erzeugter oxidschichten auf aluminium und aluminiumlegierungen
IT1240224B (it) * 1989-08-17 1993-11-27 Eliseo Benitez-Garriga Procedimento elettrolitico per colorare alluminio anodizzato e relativo prodotto.
US5674371A (en) * 1989-11-08 1997-10-07 Clariant Finance (Bvi) Limited Process for electrolytically treating aluminum and compositions therefor
DE4034854C2 (de) * 1989-11-08 2000-08-17 Clariant Finance Bvi Ltd Verfahren zum elektrolytischen Färben von Aluminium und Aluminiumlegierungen
JP3266084B2 (ja) * 1997-12-26 2002-03-18 日本軽金属株式会社 アルミニウム又はアルミニウム合金の電解着色方法

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Publication number Publication date
EP1207221A4 (de) 2002-09-11
CN1200146C (zh) 2005-05-04
CA2377953A1 (en) 2001-01-04
KR100718427B1 (ko) 2007-05-14
KR20020029870A (ko) 2002-04-20
CN1358239A (zh) 2002-07-10
AU5430200A (en) 2001-01-31
WO2001000904A1 (fr) 2001-01-04
NO20016306D0 (no) 2001-12-21
NO20016306L (no) 2002-02-15

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