WO2016201935A1 - 一种在铝合金表面形成金黄色膜层的方法 - Google Patents

一种在铝合金表面形成金黄色膜层的方法 Download PDF

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WO2016201935A1
WO2016201935A1 PCT/CN2015/098070 CN2015098070W WO2016201935A1 WO 2016201935 A1 WO2016201935 A1 WO 2016201935A1 CN 2015098070 W CN2015098070 W CN 2015098070W WO 2016201935 A1 WO2016201935 A1 WO 2016201935A1
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aluminum alloy
golden yellow
sodium
oxidation
film layer
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PCT/CN2015/098070
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English (en)
French (fr)
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马迪
李树白
李申
杨梦�
倪萍
汤晓烨
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海安县申菱电器制造有限公司
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
    • C23C22/66—Treatment of aluminium or alloys based thereon

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  • the invention belongs to the technical field of metal material surface treatment, and in particular relates to a non-toxic aluminum alloy surface chemical oxidation golden yellow process.
  • Aluminum is currently the world's largest metal in addition to steel.
  • Aluminum alloys are widely used in various industries due to their small specific gravity and high specific strength.
  • the potential of aluminum is relatively negative, and the addition of other metal elements in the alloy makes it susceptible to electrochemical corrosion, resulting in serious economic losses.
  • the surface treatment of the aluminum alloy can not only effectively solve the above-mentioned anti-corrosion problem, but also improve the decorative value of the aluminum alloy.
  • the golden yellow is beautiful and precious. It is a popular color for the surface decoration of metal and non-metal materials at home and abroad in recent years, but the price of gold is expensive and the decoration with gold is limited.
  • the emergence of imitation gold technology solved this problem.
  • the existing aluminum alloy imitation gold technology mostly adopts the traditional electrolytic coloring method, but this method has large electric energy consumption, requires special equipment and fixtures, and has large investment and high cost, and is not suitable for large-scale, ultra-small workpieces and complex structural parts. Processing. Chemical oxidation of gold-like techniques can alleviate these deficiencies.
  • the traditional aluminum alloy surface treatment uses chromate conversion, and the appearance is golden yellow. It is used for interior decoration and is very popular among users.
  • hexavalent chromium is a carcinogen, it causes serious pollution to the environment.
  • China has implemented the EU RoHS Directive since March 1, 2007, prohibiting the use of toxic and hazardous substances such as hexavalent chromium in the metal surface treatment production process.
  • many new chrome-free processes have emerged, but the surface treated by these processes is other colors, which cannot meet the current industrial corrosion resistance of aluminum alloys and golden yellow.
  • the decorative requirements of the appearance it is necessary to study and develop an industrial yellow gold chromate treatment replacement process.
  • Xu Long, Guo Ruiguang and others used a mixture of non-toxic potassium permanganate, Na 2 S 2 O 8 , NaF and sodium dodecylbenzene sulfonate under normal temperature conditions to carry out conversion treatment on the surface of aluminum alloy.
  • Gold-free chromium-free conversion film The conversion film formed by this process is mainly composed of Al, O, F, Mn elements, and has good corrosion resistance; Yi Aihua, Li Xuefen et al. contain Ti(H 2 TiF 6 )/Zr(H 2 ZrF 6 ), NaF.
  • Tannin acid, an organic corrosion inhibitor and manganese sulfate are added to the treatment liquid, and a golden yellow conversion film excellent in corrosion resistance is obtained on the aluminum alloy substrate.
  • the oxide film obtained by these scholars has good coloring effect and excellent corrosion resistance.
  • fluorine-containing substances such as NaF used in the oxidative coloring formula are harmful to human health and the environment, and need to be improved.
  • An object of the present invention is to provide a method for forming a golden yellow film layer on the surface of an aluminum alloy which overcomes the above-mentioned drawbacks of the prior art and is harmless in the preparation process.
  • the clean aluminum alloy is oxidized in an oxidative coloring liquid composed of potassium permanganate, sodium persulfate, sodium acetate and sodium chlorate, and then an aluminum alloy having a golden yellow film layer on the surface is obtained.
  • the chemical oxidation process formula used in the past is mostly a harmful substance such as chromium or fluorine.
  • the present invention uses a chemical oxidation method to coat a uniform golden yellow film layer on the surface of the aluminum alloy, and the process recipe of the invention is non-toxic, environmentally friendly and colored.
  • the liquid component is simple, the preparation is convenient, the treatment process is simple, and the coloring effect is good, which is convenient for actual production.
  • the golden yellow colored film formed on the surface of the aluminum alloy by the chemical oxidation described in the present invention has a characteristic that the color is deepened as the oxidation temperature and the oxidation time increase.
  • the surface oxidation of the aluminum alloy by the chemical oxidation method of the invention is simple, the electric energy consumption is small, the special equipment and the fixture are not needed, the investment is small, the cost is low, and the utility model is suitable for large and super Handling of small workpieces and complex structures.
  • the coloring of the aluminum alloy by the invention does not contain substances harmful to human health and the environment, and is non-toxic and environmentally friendly.
  • the oxidizing solution of the invention contains only four constituent materials, the dosage, the oxidation time and the temperature are moderate, the coloring liquid component is simple, the preparation is convenient, the treatment process is simple, the coloring effect is good, and the actual production is convenient.
  • potassium permanganate, sodium persulfate, sodium acetate and sodium chlorate are respectively 0.5 to 2.5 g/L, 2 to 6 g/L, 0.5 to 2.5 g/L and 2.5 to ⁇ . 12.5 g / L.
  • the formula can effectively remove the fluoride in the original coloring formula, and the sodium acetate and sodium chlorate composite oxidizing agent can increase the vividness of the color of the film layer.
  • the pH of the oxidative coloring liquid of the present invention is from 10.0 to 12.0. It can make the oxidation film into the darkest color and the golden yellow effect is stronger.
  • the oxidation coloring liquid has a temperature of 20 to 70 ° C and an oxidation time of 5 to 30 minutes during oxidation. As the temperature increases, the film from pale yellow to yellowish brown gradually becomes darker. The change in oxidation time, the color of the film has turned golden yellow at 5 min, but the film thickness increases with time.
  • the above temperature and time are selected in the invention to achieve better results in energy efficiency and quality.
  • the oxidation coloring liquid has a temperature of 55 to 65 ° C and an oxidation time of 5 to 10 minutes.
  • the present invention first cleans the aluminum alloy with anhydrous ethanol, removes the oil stain on the surface of the aluminum alloy, and then washes with deionized water and then puts the alkaline sodium hydroxide at 60 ° C.
  • the solution is treated for 30-60 s to remove the thin natural oxide layer on the surface of the aluminum alloy, and then washed with deionized water, then immersed in a 1.5 mol/L aqueous solution of nitric acid for 5-20 s to achieve neutralization, and finally washed with water. After drying, the aluminum alloy is clean.
  • the present invention In order to remove the deposit on the surface of the film layer and improve the appearance quality of the product, the present invention also ultrasonically cleans the oxidized aluminum alloy with deionized water for 3 to 5 minutes, and then dried by hot air.
  • 1, 2, and 3 are the Tafel pieces of the aluminum alloy products having the golden yellow surface formed by the methods of the first, second, and third embodiments, respectively. line graph.
  • the surface of the aluminum alloy is cleaned with anhydrous ethanol to remove the oil on the surface; then washed with deionized water and placed in an alkaline sodium hydroxide solution at 60 ° C for 30 s to remove the thin natural oxide layer; after washing with deionized water It was immersed in a 1.5 mol/l dilute nitric acid solution for 10 s to neutralize; finally, the water was washed with water, dried, and set aside.
  • the surface-pretreated aluminum alloy was directly placed in the oxidative coloring solution, and after 10 minutes of oxidative coloring reaction, the aluminum alloy was taken out.
  • the aluminum alloy is ultrasonically cleaned with deionized water for 3 minutes, and dried by hot air to obtain an aluminum alloy product with a golden yellow surface.
  • the surface of the aluminum alloy is cleaned with anhydrous ethanol to remove the oil on the surface; then washed with deionized water and placed in an alkaline sodium hydroxide solution at 60 ° C for 35 s to remove the thin natural oxide layer; after washing with deionized water It was immersed in a 1.5 mol/l dilute nitric acid solution for 15 s to neutralize; finally, the water was washed with water, dried, and set aside.
  • the surface-pretreated aluminum alloy was directly placed in the oxidative coloring solution, and after 5 minutes of oxidative coloring reaction, the aluminum alloy was taken out.
  • the surface of the aluminum alloy is cleaned with anhydrous ethanol to remove the oil on the surface; then washed with deionized water and placed in an alkaline sodium hydroxide solution at 60 ° C for 30 s to remove the thin natural oxide layer; after washing with deionized water It was immersed in a 1.5 mol/l dilute nitric acid solution for 15 s to neutralize; finally, the water was washed with water, dried, and set aside.
  • the surface-pretreated aluminum alloy was directly placed in the oxidative coloring solution, and after 5 minutes of oxidation coloring reaction, the aluminum alloy was taken out.
  • the aluminum alloy is ultrasonically cleaned with deionized water for 5 min, and dried by hot air to obtain an aluminum alloy product with a golden yellow surface.

Abstract

在铝合金表面形成金黄色膜层的方法，将洁净的铝合金置于由高锰酸钾、过硫酸钠、乙酸钠和氯酸钠组成的氧化着色液中进行氧化后，取得表面具有金黄色膜层的铝合金。

Description

一种在铝合金表面形成金黄色膜层的方法 技术领域
本发明属于金属材料表面处理技术领域，尤其涉及一种无毒的铝合金表面化学氧化着金黄色工艺方法。
背景技术
铝是目前世界上除钢铁外用量最大的金属。铝合金由于比重小、比强度高而广泛应用于各个行业。但铝的电位较负，合金中其他金属元素的加入使其容易发生电化学腐蚀，造成严重的经济损失。对铝合金进行表面处理不仅可以有效的解决上述防腐问题，同时还能提高铝合金的装饰价值。
金黄色华丽贵重，是近年来国内外金属、非金属材料表面装饰的一种流行色，但金价昂贵，用金装饰受到限制。仿金工艺的出现解决了这个问题。已有的铝合金仿金技术多采用传统的电解着色方法，但这种方法电能消耗大、需专用设备及工夹具，投资大、成本高，且不适用于大型、超小型工件及结构复杂工件的处理。化学氧化着仿金色技术可改善上述不足。
传统的铝合金表面处理使用铬酸盐转化，外表为金黄色，用于室内装饰显得富丽堂皇，深受用户喜爱，但由于六价铬为致癌物质，对环境造成了严重的污染。我国已于2007年3月1日起执行欧盟RoHS指令，禁止在金属表面处理生产过程中使用六价铬等有毒有害物质。近年来，随着环保产业的发展以及人们的环保意识的提高，出现了许多无铬新工艺，但这些工艺处理后的表面为其他颜色，不能满足目前工业对于铝合金耐蚀性能好和金黄色外表装饰性的要求，因此有必要研究开发一种工业需要的金黄色铬酸盐处理替代工艺。
许龙、郭瑞光等人在常温条件下，采用无毒的高锰酸钾、Na2S2O8、NaF、十二烷基苯磺酸钠混合液，进行转化处理，在铝合金表面制备金黄色无铬转化膜。采用此工艺形成的转化膜主要由Al，O，F，Mn元素组成，耐腐蚀性能良好；易爱华、黎雪芬等人在含有Ti(H2TiF6)/Zr(H2ZrF6)、NaF、的处理液中加入单宁酸、有机缓蚀剂和硫酸锰，在铝合金基体上得到了耐蚀性能优异的金黄色转化膜。这些学者研究的工艺条件所得的氧化膜着色效果良好，且耐蚀性优良，但氧化着色配方中均用到的NaF等含氟物质，对人体健康、环境有害，还有待改进。
发明内容
本发明的目的在于提出一种能克服以上现有技术缺陷、制备过程无害化的在铝合金表面形成金黄色膜层的方法。
本发明技术方案是：将洁净的铝合金置于由高锰酸钾、过硫酸钠、乙酸钠和氯酸钠组成的氧化着色液中进行氧化后，取得表面具有金黄色膜层的铝合金。
以往采用的化学氧化工艺配方中多为含铬或含氟等有害物质，本发明利用化学氧化法在铝合金表面着上一层均匀的金黄色膜层，本发明的工艺配方无毒环保、着色液成分简单，配制便捷，处理工艺简单，且着色效果良好，便于实际生产。另外，本发明中所述的化学氧化在铝合金表面形成的金黄色着色膜具有随氧化温度、氧化时间的增大颜色加深的特点。
本发明相对于现有技术，其优点如下：
1、采用本发明中的化学氧化方法对铝合金进行表面着色，相较于电解等其他方法操作简单，电能消耗小、无需专用设备及工夹具，投资小、成本低，且适用于大型、超小型工件及结构复杂工件的处理。
2、相比已提出的含铬、含氟等有害物质的氧化着色配方，采用本发明对铝合金进行着色不含对人体健康、环境有害的物质，无毒环保。
3、本发明的氧化溶液只含有四种组成物质，用量、氧化时间、温度均适中，着色液成分简单，配制便捷，处理工艺简单，且着色效果良好，便于实际生产。
进一步地，本发明所述氧化着色液中高锰酸钾、过硫酸钠、乙酸钠和氯酸钠组成分别为0.5～2.5g/L、2～6g/L、0.5～2.5g/L和2.5～12.5g/L。该配方下可有效去除原有着色配方中的氟化物，采用乙酸钠和氯酸钠复合氧化剂可增加膜层颜色的鲜艳度。
本发明所述氧化着色液的pH为10.0～12.0。可使氧化成膜颜色最深，金黄色效果更强。
氧化时所述氧化着色液的温度为20～70℃，氧化时间为5～30min。随着温度的升高，由淡黄色到黄棕色膜层逐渐变深。氧化时间的变化，在5min时膜层颜色就已变成金黄色，但随着时间延长，膜厚增加。本发明选用以上温度和时间使能效和质量都达到了较理想的结果。
更优选的氧化时所述氧化着色液的温度为55～65℃，氧化时间为5～10min。
为了达到较高的洁净度，以利于后续氧化膜的形成，本发明先以无水乙醇清洗铝合金，去除铝合金表面的油污，然后以去离子水洗后放入60℃的碱性氢氧化钠溶液中处理30～60s，去除铝合金表面的薄天然氧化物层，再经去离子水水洗后，放入1.5mol/L的硝酸水溶液中浸渍5～20s达到中和的目的，最后以清水水洗，制干后即得洁净的铝合金。
为了去除膜层表面附着物，提高产品的外观质量，本发明还将氧化后的铝合金以去离子水超声清洗3～5min后，经热风烘干。
附图说明
图1、2、3分别为实施例1、2、3方法制成的表面呈金黄色的铝合金制品的Tafel曲 线图。
具体实施方式
实施例1：
1、铝合金表面预处理：
先采用无水乙醇对铝合金表面进行清洗，去除表面的油污；再以去离子水洗后放入60℃的碱性氢氧化钠溶液30s，去除表面薄天然氧化物层；经去离子水水洗后，放入1.5mol/l的稀硝酸溶液中浸渍10s中和；最后清水水洗，凉干，待用。
2、配置氧化着色溶液：
以高锰酸钾(KMnO4，分析纯)0.5g/l、过硫酸钠(Na2S2O8，分析纯)3g/l、乙酸钠(NaAc、分析纯)1g/l和氯酸钠(NaClO3、分析纯)5g/l混合后，以1.0mol/1的NaOH调整混合体系的pH为10.00，待用。
3、氧化着色：
将氧化着色溶液放入水浴锅中加热至55℃后，将表面预处理后的铝合金直接放入氧化着色溶液中，经过10min氧化着色反应后，取出铝合金。
4、用去离子水对铝合金进行超声清洗3min，热风烘干，即得表面呈金黄色的铝合金制品。
5、产品效果如图1所示。
实施例2：
1、铝合金表面预处理：
先采用无水乙醇对铝合金表面进行清洗，去除表面的油污；再以去离子水洗后放入60℃的碱性氢氧化钠溶液35s，去除表面薄天然氧化物层；经去离子水水洗后，放入1.5mol/l的稀硝酸溶液中浸渍15s中和；最后清水水洗，凉干，待用。
2、配置氧化着色溶液：
将高锰酸钾(KMnO4，分析纯)2g/l、过硫酸钠(Na2S2O8，分析纯)3g/l、乙酸钠(NaAc、分析纯)2.5g/l和氯酸钠(NaClO3、分析纯)12.5g/l混合后，以1.0mol/l的NaOH调整混合体系的pH为11.00，待用。
3、氧化着色：
将氧化着色溶液放入水浴锅中加热至65℃后，将表面预处理后的铝合金直接放入氧化着色溶液中，经过5min氧化着色反应后，取出铝合金。
4、用去离子水对铝合金进行超声清洗4min，热风烘干，即得表面呈金黄色的铝合金 制品。
5、产品效果如图2所示。
实施例3：
1、铝合金表面预处理：
先采用无水乙醇对铝合金表面进行清洗，去除表面的油污；再以去离子水洗后放入60℃的碱性氢氧化钠溶液30s，去除表面薄天然氧化物层；经去离子水水洗后，放入1.5mol/l的稀硝酸溶液中浸渍15s中和；最后清水水洗，凉干，待用。
2、配置氧化着色溶液：
将高锰酸钾(KMnO4，分析纯)2.5g/l、过硫酸钠(Na2S2O8，分析纯)3g/l、乙酸钠(NaAc、分析纯)1.5g/l和氯酸钠(NaClO3、分析纯)7.5g/l混合后，以1.0mol/l的NaOH调整混合体系的pH为12.00，待用。
3、氧化着色：
将氧化着色溶液放入水浴锅中加热至60℃后，将表面预处理后的铝合金直接放入氧化着色溶液中，经过5min氧化着色反应后，取出铝合金。
4、用去离子水对铝合金进行超声清洗5min，热风烘干，即得表面呈金黄色的铝合金制品。
5、产品效果如图3所示。

Claims (7)

  1. 一种在铝合金表面形成金黄色膜层的方法，其特征在于将洁净的铝合金置于由高锰酸钾、过硫酸钠、乙酸钠和氯酸钠组成的氧化着色液中进行氧化后，取得表面具有金黄色膜层的铝合金。
  2. 根据权利要求1所述方法，其特征在于所述氧化着色液中高锰酸钾、过硫酸钠、乙酸钠和氯酸钠组成分别为0.5～2.5g/L、2～6g/L、0.5～2.5g/L和2.5～12.5g/L。
  3. 根据权利要求1或2所述方法，其特征在于所述氧化着色液的pH为10.0～12.0。
  4. 根据权利要求1所述方法，其特征在于氧化时所述氧化着色液的温度为20～70℃，氧化时间为5～30min。
  5. 根据权利要求4所述方法，其特征在于氧化时所述氧化着色液的温度为55～65℃，氧化时间为5～10min。
  6. 根据权利要求1所述方法，其特征在于先以无水乙醇清洗铝合金，然后以去离子水洗后放入60℃的碱性氢氧化钠溶液中处理30～60s，再经去离子水水洗后，放入1.5mol/L的硝酸水溶液中浸渍5～20s，最后以清水水洗，制干后即得洁净的铝合金。
  7. 根据权利要求1所述方法，其特征在于将氧化后的铝合金以去离子水超声清洗3～5min后，经热风烘干。
PCT/CN2015/098070 2015-06-19 2015-12-21 一种在铝合金表面形成金黄色膜层的方法 WO2016201935A1 (zh)

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