WO2017166995A1 - 镁合金阳极氧化液及其制备方法和镁合金阳极氧化的方法 - Google Patents

镁合金阳极氧化液及其制备方法和镁合金阳极氧化的方法 Download PDF

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WO2017166995A1
WO2017166995A1 PCT/CN2017/076296 CN2017076296W WO2017166995A1 WO 2017166995 A1 WO2017166995 A1 WO 2017166995A1 CN 2017076296 W CN2017076296 W CN 2017076296W WO 2017166995 A1 WO2017166995 A1 WO 2017166995A1
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magnesium alloy
anodizing
anodizing solution
silicate
ethylene glycol
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韦家亮
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BYD Co Ltd
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BYD Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/30Anodisation of magnesium or alloys based thereon

Definitions

  • the invention relates to metal surface treatment, in particular to a magnesium alloy surface anodizing liquid and a preparation method thereof and a magnesium alloy anodizing method.
  • Magnesium alloys have been widely concerned for their unique properties and abundant resources. However, due to the immature magnesium alloy treatment process, the problem of poor corrosion resistance has become a major obstacle to its superior performance, thus limiting magnesium alloy to a large extent. Promote applications on a larger scale. From the 1940s and 1950s, the research and development of magnesium alloy surface treatment technology was carried out abroad.
  • the surface coloration of magnesium alloy is one of the hotspots of current research, and anodizing and dyeing is a popular research process.
  • the aluminum alloy is subjected to a coloring method after the anodizing process, and there are usually a secondary coloring method, an electrolytic coloring method, and a multicolor coloring method, and these processes have entered the industrialization stage.
  • the structure of the anodized film of the magnesium alloy is similar to that of the aluminum alloy, and is also composed of a non-porous barrier layer and a porous oxide surface, except that the pores of the anodized surface of the aluminum alloy are fine and uniform, and the anodized film of the magnesium alloy The pores are related to the fracture of the barrier layer and the subsequent oxidation behavior.
  • the surface layer pores are large and irregular, and the porosity of the membrane is high.
  • Many methods for the anodizing coloring reaction of aluminum alloys are not suitable for coloring the anodized film layer of magnesium alloys. Due to the characteristics of magnesium itself, industrialization and production are far less than the anodization of aluminum alloy, the pores of the formed oxide film are not uniform, and the film layer is easy to fall off under pressure conditions; especially when the magnesium alloy is colored, there is uneven coloration. The problem of poor adhesion of the dyed layer.
  • the present invention provides a magnesium alloy anodizing solution which is an aqueous solution containing a hydroxide, a silicate, a metaaluminate, a phosphate, a glyoxylic acid, and an ethylene glycol.
  • the anodizing liquid provided by the invention adds glyoxylic acid and ethylene glycol, and can effectively control the pore size on the oxide film and improve the uniformity of the oxide film under the action of other raw materials, thereby making the subsequent dyeing effect uniform.
  • the dyed layer does not easily fall off.
  • the invention also provides a method for preparing a magnesium alloy anodizing solution, which comprises adding hydroxide, silicate, metaaluminate, phosphate, glyoxylic acid and ethylene glycol to water, and stirring until dissolved.
  • the invention also provides a method for anodizing a magnesium alloy, comprising: immersing a magnesium alloy in the above-mentioned magnesium alloy anodizing solution for anodizing.
  • the magnesium alloy anodizing liquid provided by the invention is compounded by various components, and due to the interaction between the components, the The anodizing solution can effectively control the pore size and the uniformity of the oxide film on the oxide film, which is favorable for subsequent dyeing.
  • the invention provides a magnesium alloy anodizing solution.
  • the anodizing solution is an aqueous solution containing hydroxide, silicate, metaaluminate, phosphate, glyoxylic acid and ethylene glycol. Therefore, ethylene glycol and glyoxylic acid are added to the anodizing solution, and under the combined action of the two substances, the pore size of the oxide film after anodization can be effectively reduced, and the uniformity of the pore size can be improved;
  • the formed oxide film layer has better uniformity and a smaller color difference from the magnesium alloy substrate, which is advantageous for dyeing the magnesium alloy in the subsequent step.
  • the hydroxide content is 80-150 g/L
  • the silicate content is 1-10 g/L
  • the metaaluminate content is 30-60 g/L
  • phosphate The content is 1-20 g/L
  • the content of glyoxylic acid is 0.5-5 g/L
  • the content of ethylene glycol is 0.5-5 g/L.
  • the hydroxide used is a hydroxide commonly used in the art, specifically one or more of sodium hydroxide and potassium hydroxide.
  • the inventors have found that hydroxides ensure the stable presence of magnesium alloys in solution.
  • the hydroxide content is from 80 to 150 g/L.
  • the silicate used is a silicate commonly used in the art, specifically one or more of potassium silicate and sodium silicate.
  • the inventors have found that silicate is involved in the film formation process during the anodization of the magnesium alloy, and the obtained anodized film contains magnesium silicon oxide with good performance and good corrosion resistance, which can improve the corrosion resistance of the film.
  • the silicate content is 1-10 g/L.
  • the metaaluminate used is a metaaluminate commonly used in the art, and specifically one or more of sodium metaaluminate and potassium metaaluminate.
  • the inventors have found that the role of metaaluminate is to provide an aluminum salt, especially when a silicate system is present in the solution, and anodization can form a composite of Al and Si, further increasing the corrosion resistance of the film.
  • the metaaluminate content is from 30 to 60 g/L.
  • the phosphate used is a phosphate commonly used in the art, specifically one or more of sodium tripolyphosphate and sodium phosphate.
  • the inventors have found that the role of phosphate is to provide a phosphorus element, which contains a certain phosphorus element in the oxide film, thereby improving the corrosion resistance of the oxide film.
  • the phosphate content is from 1 to 20 g/L.
  • Ethylene glycol and glyoxylic acid are added to the magnesium alloy anodizing solution of the present invention.
  • Ethylene glycol can play a role in improving the uniformity of pores; glyoxylic acid can effectively control the pore size, and can reduce the pores of the anodized film under the action of ethylene glycol, so that the dyeing stage can obtain better coloration. effect.
  • the content of ethylene glycol is 0.5-5 g/L
  • the content of glyoxylic acid is 0-5-5 g/L;
  • the weight ratio of ethylene glycol to glyoxylic acid is 1:0.1-1, further preferably 1:0.1-0.3, at this time, the average pore size of the oxide film
  • the diameter can be controlled below 50 ⁇ m.
  • the invention provides a method of preparing the above anodizing solution.
  • the method comprises adding hydroxide, silicate, metaaluminate, phosphate, glyoxylic acid and ethylene glycol to water and stirring until dissolved.
  • the hydroxide, the metaaluminate, the silicate and the phosphate, the ethylene glycol and the glyoxylic acid are sequentially added to the water to be dissolved, and the mixture is uniformly stirred.
  • the invention provides a method of anodizing a surface of a magnesium alloy.
  • the method comprises: immersing the magnesium alloy in the magnesium alloy anodizing solution described above for anodization.
  • the temperature of the magnesium alloy anodizing solution is 30-40 ° C
  • the anodizing current is 3-7 A
  • the anodizing time is 5-30 min. Therefore, the magnesium alloy anodizing solution provided by the invention is compounded by various components, and the anodizing liquid can effectively control the pore size and the uniformity of the oxide film on the oxide film due to the interaction between the components. Conducive to subsequent dyeing. It should be noted that the above described features and advantages for the anodizing solution are also applicable to the preparation method of the anodizing liquid, and are not described herein again.
  • the magnesium alloy may be pretreated prior to anodization; the pretreatment is a pretreatment method commonly used in the art, specifically mechanical removal of the oxide layer, ash removal, oil removal and water washing.
  • magnesium alloy anodizing solution Preparation of magnesium alloy anodizing solution: adding hydroxide, silicate, metaaluminate, phosphate, ethylene glycol and glyoxylic acid to deionized water.
  • the magnesium alloy anodizing liquids A1-A5 were obtained according to the group distribution ratio in Table 1, and the specific amounts of the respective components are shown in Table 1.
  • the 5cm ⁇ 3cm magnesium alloy sample (brand AZ91D) is subjected to pretreatment such as deoxidation layer removal, ash removal, oil removal and water washing; and the pretreated magnesium alloy sample is placed in the magnesium alloy anodizing in step (1).
  • the solution was oxidized for 10 min under the condition of a solution temperature of 35 ° C and a current of 5 A; the above-mentioned oxidized magnesium alloy was taken out, washed with water, and dried to obtain experimental samples Y1-Y5. All of the raw materials in the examples described in the present invention are commercially available products, unless otherwise specified.
  • the formulation of the comparative formulation D1 was the same as that of the anodizing solution A1 of Example 1 except that ethylene glycol and glyoxylic acid were not contained. After oxidative drying in D1 according to the method in the examples, experimental sample M1 was obtained.
  • the formulation of the comparative formulation D2 was the same as that of the anodizing solution A1 of Example 1 except that ethylene glycol was not contained. After oxidative drying in D2 according to the method in the examples, experimental sample M2 was obtained.
  • the anodizing solution of the example disclosed in CN103938253A is D3, and the formula is: potassium silicate 90g/L, potassium gluconate 25g/L, sodium hydroxide 100g/L, sodium acetate 60g/L, potassium fluoride 8g/ L, ethylene glycol 15g / L.
  • Electron microscopy test Y1-Y5 and M1-M3 were scanned 2000 times under electron microscope to observe the pore uniformity.
  • Pore uniformity Whether the entire surface is uniformly distributed with obvious visible cracks or pores; the pores and cracks on the good oxide film layer are uniform in size, uniform in distribution, light in color and metallic luster.
  • Dyeing effect test Y1-Y5 and M1-M3 were dyed with the light-resistant peach red G dye; the dye concentration was 3 g/L, the liquid temperature was 65 ° C, and the dyeing time was 2 min. After dyeing, the sample was dried and the staining effect was observed.
  • Adhesion test According to the test method in the Baige standard, the adhesion of the dye layer is tested; the test results are in accordance with the ASTM grade, from good to bad: 5B, 4B, 3B, 2B, 1B, 0B.
  • the anodizing solution provided by the present invention can have a good oxidation effect on the magnesium alloy, and the obtained oxide film layer has uniform pores and uniform pore distribution.

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
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  • Chemical Treatment Of Metals (AREA)

Abstract

一种镁合金阳极氧化液,该阳极氧化液为含有氢氧化物、硅酸盐、偏铝酸盐、磷酸盐、乙二醇和乙醛酸的水溶液。还提供了该种镁合金阳极氧化液的制备方法,以及采用该种镁合金阳极氧化液对镁合金进行阳极氧化的方法。所述的镁合金阳极氧化液可以有效降低氧化膜上的孔隙大小,并提高孔隙均匀度,从而提高后段的染色效果。

Description

镁合金阳极氧化液及其制备方法和镁合金阳极氧化的方法 技术领域
本发明涉及金属表面处理,尤其涉及一种镁合金表面阳极氧化液及其制备方法和镁合金阳极氧化的方法。
背景技术
镁合金因其独特的性能和丰富的资源一直受到广泛关注,但由于镁合金处理工艺尚不成熟,耐蚀性差的问题成为发挥其优越性能的主要障碍,因而在很大程度上限制了镁合金在更大范围内的推广应用。从上世纪四五十年代,国外就对镁合金表面处理技术进行了开发研究。
镁合金表面着色是目前研究的热点之一,其中阳极氧化加染色是较为热门的研究工艺。目前铝合金在进行阳极氧化工艺后再采用着色方法,通常有二次着色法、电解着色法和多色着色法等,这些工艺已进入工业化阶段。镁合金的阳极氧化膜的构造与铝合金类似,也是由无孔的阻挡层和多孔的氧化物表面组成,不同之处在于铝合金阳极氧化表面孔洞细小、均匀,而镁合金的阳极氧化膜的孔隙与阻挡层的断裂和随后的氧化行为有关,表面层孔隙大且无规则,膜的孔隙率较高。许多用于铝合金阳极氧化着色反应的方法不适用于镁合金的阳极氧化膜层的着色。由于镁本身的特性,工业化和生产远不及铝合金阳极氧化,生成的氧化膜孔隙不均匀,而且膜层在压力的条件下易脱落;特别是当对镁合金着色时,会有着色不均匀,染色层附着力差的问题。
发明内容
为解决上述问题,本发明提供了一种镁合金阳极氧化液,该阳极氧化液为含有氢氧化物、硅酸盐、偏铝酸盐、磷酸盐、乙醛酸和乙二醇的水溶液。
本发明提供的阳极氧化液中添加了乙醛酸和乙二醇,在与其他原料的共同作用下可以有效控制氧化膜上的孔隙大小,提高氧化膜的均匀性,从而使得后续的染色效果均匀,染色层不容易脱落。
本发明还提供了一种镁合金阳极氧化液的制备方法,包括将氢氧化物、硅酸盐、偏铝酸盐、磷酸盐、乙醛酸和乙二醇加入水中,搅拌至溶解。
本发明还提供了一种镁合金阳极氧化的方法,包括:将镁合金浸入上述镁合金阳极氧化液中进行阳极氧化。
本发明提供的镁合金阳极氧化液由多种成分复配而成,由于各组分间的相互作用,该 阳极氧化液能有效控制氧化膜上的孔隙大小和氧化膜均匀性,有利于后续的染色。
本发明的附加方面和优点将在下面的描述中部分给出,部分将从下面的描述中变得明显,或通过本发明的实践了解到。
发明详细描述
下面详细描述本发明的实施例。下面描述的实施例是示例性的,旨在用于解释本发明,而不能理解为对本发明的限制。
在本发明的一个方面,本发明提出了一种镁合金阳极氧化液。根据本发明的实施例,所述阳极氧化液为含有氢氧化物、硅酸盐、偏铝酸盐、磷酸盐、乙醛酸和乙二醇的水溶液。由此,该阳极氧化液中添加了乙二醇和乙醛酸,在两种物质的共同作用下,可以有效减小阳极氧化后氧化膜的孔隙大小,提高孔隙大小的均匀性;不仅如此,所形成的氧化膜层均匀度更好,且与镁合金基材的色差更小,有利后续步骤中的镁合金染色。
在本发明的阳极氧化液中,所述氢氧化物的含量为80-150g/L,硅酸盐的含量为1-10g/L,偏铝酸盐的含量为30-60g/L,磷酸盐的含量为1-20g/L,乙醛酸的含量为0.5-5g/L,乙二醇的含量为0.5-5g/L。
在本发明的实施例中,采用的氢氧化物为本领域内常用的氢氧化物,具体为氢氧化钠、氢氧化钾中的一种或几种。发明人发现,氢氧化物可以确保镁合金在溶液中稳定存在。优选情况下,氢氧化物的含量为80-150g/L。
在本发明的实施例中,采用的硅酸盐为本领域常用的硅酸盐,具体为硅酸钾、硅酸钠中的一种或几种。发明人发现,在镁合金的阳极氧化时,硅酸盐参与了成膜过程,得到的阳极氧化膜中含有性能稳定、耐蚀性较好的镁硅氧化物,能够提高膜层的耐蚀性,优选情况下,硅酸盐的含量为1-10g/L。
在本发明的实施例中,采用的偏铝酸盐为本领域内常用的偏铝酸盐,具体为偏铝酸钠、偏铝酸钾中的一种或几种。发明人发现,偏铝酸盐的作用在于提供铝盐,尤其是当溶液中有硅酸盐体系时,阳极氧化可形成Al与Si的复合物,进一步增加了膜层耐蚀性。优选情况下,偏铝酸盐的含量为30-60g/L。
本发明中的实施例中,采用的磷酸盐为本领域内常用的磷酸盐,具体为三聚磷酸钠、磷酸钠中的一种或几种。发明人发现,磷酸盐的作用在于提供磷元素,使氧化膜中含有一定磷元素,进而提高氧化膜的耐蚀性能。优选情况下,磷酸盐的含量为1-20g/L。
本发明的镁合金阳极氧化液中添加入乙二醇和乙醛酸。乙二醇可以起到提高孔隙均匀性的作用;乙醛酸能有效控制孔隙大小,在与乙二醇的共同作用下可以减小阳极氧化膜的孔隙,从而使染色阶段可以获得更好的着色效果。优选情况下,乙二醇的含量为0.5-5g/L, 乙醛酸的含量为0-5-5g/L;乙二醇与乙醛酸的重量比为1:0.1-1,进一步优选情况下为1:0.1-0.3,此时,氧化膜的平均孔隙直径可以控制在50μm以下。
在本发明在再一个方面,本发明提出了一种上述阳极氧化液的制备方法。根据本发明的实施例,所述方法包括:将氢氧化物、硅酸盐、偏铝酸盐、磷酸盐、乙醛酸和乙二醇加入水中,搅拌至溶解。优选情况下,依次将氢氧化物、偏铝酸盐、硅酸盐和磷酸盐、乙二醇和乙醛酸加入水中溶解,搅拌均匀即可。需要说明的是,上述针对阳极氧化液所描述的特征和优点同样适用于该阳极氧化液的制备方法,此处不再赘述。
在本发明的第三个方面,本发明提出了一种镁合金表面阳极氧化的方法。根据本发明的实施例,该方法包括:将镁合金浸入上述的镁合金阳极氧化液中进行阳极氧化。优选情况下,镁合金阳极氧化液的温度为30-40℃,所述阳极氧化电流为3-7A,所述阳极氧化的时间为5-30min。由此,本发明提供的镁合金阳极氧化液由多种成分复配而成,由于各组分间的相互作用,该阳极氧化液能有效控制氧化膜上的孔隙大小和氧化膜均匀性,有利于后续的染色。需要说明的是,上述针对阳极氧化液所描述的特征和优点同样适用于该阳极氧化液的制备方法,此处不再赘述。
优选情况下,可以在阳极氧化之前对镁合金进行预处理;预处理为本领域内常用的预处理方法,具体为机械去除氧化层,除灰除油及水洗。
下面参考具体实施例,对本发明进行描述,需要说明的是,这些实施例仅仅是描述性的,而不以任何方式限制本发明。
实施例1-5
1、制备镁合金阳极氧化液:将氢氧化物、硅酸盐、偏铝酸盐、磷酸盐、乙二醇和乙醛酸加入去离子水中。按照表1中组分配比得到镁合金阳极氧化液A1-A5,各组分具体用量见表1。
2、将5cm×3cm的镁合金样品(牌号AZ91D)进行去除氧化层、除灰除油及水洗等预处理;将上述预处理后的镁合金样品放入步骤(1)中的镁合金阳极氧化液内,在溶液温度35℃、电流5A的条件下,氧化10min;取出上述氧化后的镁合金,水洗后烘干获得实验样品Y1-Y5。本发明中所述实施例中的所有原料如非特指,均为市售产品。
表1
组分(g/L) A1 A2 A3 A4 A5 D1 D2
氢氧化钾 100 80 150 100 100 100 100
硅酸钠 3 1 10 3 5 3 3
偏铝酸钠 40 30 60 40 40 40 40
三聚磷酸钠 3 1 20 3 10 3 3
乙二醇 1 0.5 5 2 2 / /
乙醛酸 1 0.5 5 0.5 0.2 / 1
对比例1
对比配方D1中除不含有乙二醇和乙醛酸外,其余配方与实施例1中阳极氧化液A1的相同。并按照实施例中的方法在D1中氧化烘干后,获得实验样品M1。
对比例2
对比配方D2中除不含有乙二醇外,其余配方与实施例1中阳极氧化液A1的相同。并按照实施例中的方法在D2中氧化烘干后,获得实验样品M2。
对比例3
以公开号为CN103938253A中实施例的阳极氧化液为D3,配方为:硅酸钾90g/L,葡萄糖酸钾25g/L,氢氧化钠100g/L,乙酸钠60g/L,氟化钾8g/L,乙二醇15g/L。
按照实施例中的方法在D3中氧化烘干后,获得实验样品M3。
性能测试及结果
1、电镜测试:将Y1-Y5、M1-M3在电镜下放大2000倍进行扫描,观察孔隙均匀度。
孔隙均匀度:整个表面是否均匀分布明显可见的裂纹或孔隙;好的氧化膜层上孔隙和裂纹大小均匀、分布均匀,且色泽较浅,有金属光泽。
2、染色效果测试:使用耐晒桃红G染料对Y1-Y5、M1-M3进行染色;染料浓度3g/L,液温65℃,将染色时间2min。染色后吹干样品,观察染色效果。
3、附着力测试:根据百格标准中的测试方法,对染色层附着力进行测试;测试结果按ASTM等级,从好到差依次为:5B、4B、3B、2B、1B、0B。
测试结果见表2。
表2
Figure PCTCN2017076296-appb-000001
Figure PCTCN2017076296-appb-000002
从表2中可以看出,使用本发明提供的阳极氧化液可以对镁合金起到良好的氧化效果,所获的氧化膜层孔隙均匀、且孔隙的分布均匀。
在本说明书的描述中,参考术语“一个实施例”、“一些实施例”、“示例”、“具体示例”、或“一些示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不必须针对的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任一个或多个实施例或示例中以合适的方式结合。此外,在不相互矛盾的情况下,本领域的技术人员可以将本说明书中描述的不同实施例或示例以及不同实施例或示例的特征进行结合和组合。
尽管上面已经示出和描述了本发明的实施例,可以理解的是,上述实施例是示例性的,不能理解为对本发明的限制,本领域的普通技术人员在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。

Claims (20)

  1. 一种镁合金阳极氧化液,其特征在于,所述阳极氧化液为含有氢氧化物、硅酸盐、偏铝酸盐、磷酸盐、乙二醇和乙醛酸的水溶液。
  2. 根据权利要求1所述的镁合金阳极氧化液,其特征在于,所述氢氧化物的含量为80-150g/L。
  3. 根据权利要求1或2所述的镁合金阳极氧化液,其特征在于,所述硅酸盐的含量为1-10g/L。
  4. 根据权利要求1-3中任一项所述的镁合金阳极氧化液,其特征在于,所述偏铝酸盐的含量为30-60g/L。
  5. 根据权利要求1-4中任一项所述的镁合金阳极氧化液,其特征在于,所述磷酸盐的含量为1-20g/L。
  6. 根据权利要求1-5中任一项所述的镁合金阳极氧化液,其特征在于,所述乙醛酸的含量为0.5-5g/L。
  7. 根据权利要求1-6中任一项所述的镁合金阳极氧化液,其特征在于,所述乙二醇的含量为0.5-5g/L。
  8. 根据权利要求1-7中任一项所述的镁合金阳极氧化液,其特征在于,所述氢氧化物为氢氧化钠和/或氢氧化钾。
  9. 根据权利要求1-8中任一项所述的镁合金阳极氧化液,其特征在于,所述硅酸盐为硅酸钠和/或硅酸钾。
  10. 根据权利要求1-9中任一项所述的镁合金阳极氧化液,其特征在于,所述偏铝酸盐为偏铝酸钠和/或偏铝酸钾。
  11. 根据权利要求1-10中任一项所述的镁合金阳极氧化液,其特征在于,所述磷酸盐为三聚磷酸钠和/或磷酸钠。
  12. 根据权利要求1-11中任一项所述的镁合金阳极氧化液,其特征在于,所述乙二醇和所述乙醛酸的重量比例为1:0.1-1。
  13. 根据权利要求1-12中任一项所述的镁合金阳极氧化液,其特征在于,所述乙二醇和所述乙醛酸的重量比例为1:0.1-0.3。
  14. 一种镁合金阳极氧化液的制备方法,其特征在于,包括将氢氧化物、硅酸盐、偏铝酸盐、磷酸盐、乙醛酸和乙二醇加入水中,搅拌至溶解。
  15. 一种镁合金阳极氧化的方法,其特征在于,包括:将镁合金浸入镁合金阳极氧化液中进行阳极氧化,
    其中,所述镁合金阳极氧化液为权利要求1-13中任一项所述的镁合金阳极氧化液。
  16. 根据权利要求15所述的方法,其特征在于,所述镁合金阳极氧化液的温度为30-40℃。
  17. 根据权利要求15或16所述的方法,其特征在于,所述阳极氧化电流为3-7A。
  18. 根据权利要求15-17中任一项所述的方法,其特征在于,所述阳极氧化时间为5-30min。
  19. 根据权利要求15-18中任一项所述的方法,其特征在于,在将所述镁合金放入所述镁合金阳极氧化液之前进行预处理。
  20. 根据权利要求15-19中任一项所述的方法,其特征在于,所述预处理包括去除氧化层、除灰除油及水洗。
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113737249A (zh) * 2021-10-08 2021-12-03 东莞市恒核机电科技有限公司 一种镁合金黑色弧光放电陶瓷层的制备方法

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107620106A (zh) * 2017-11-10 2018-01-23 吉林大学 一种铁铬铝合金阳极氧化的电解液及氧化的方法
CN108468077B (zh) * 2018-03-29 2020-11-10 山西银光华盛镁业股份有限公司 一种镁合金自封闭阳极氧化方法
CN110629267A (zh) * 2018-06-25 2019-12-31 比亚迪股份有限公司 一种铝制品碱性阳极氧化液及阳极氧化方法
CN113774462B (zh) * 2021-10-22 2023-03-28 上海康德莱医疗器械股份有限公司 一种镁合金表面处理方法和处理后的镁合金
CN114011672A (zh) * 2021-11-23 2022-02-08 上海金泛斯标识有限公司 一种铝型材喷涂工艺

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003166098A (ja) * 2001-11-30 2003-06-13 Kasatani:Kk マグネシウム合金の陽極酸化処理用組成物および処理方法
KR20040028908A (ko) * 2004-03-18 2004-04-03 (주)케이엠티 마그네슘 합금의 대면적 양산성을 고려한 내식성 향상을위한 시약 합성방법
CN101040066A (zh) * 2004-07-23 2007-09-19 坎梅陶尔股份有限公司 在由可阳极氧化金属或合金制成的物品上形成高抗腐蚀性硬涂层的方法
CN101239009A (zh) * 2008-01-29 2008-08-13 乐普(北京)医疗器械股份有限公司 可控降解的微弧氧化金属支架及其制备方法
CN101285193A (zh) * 2007-04-09 2008-10-15 比亚迪股份有限公司 一种用于处理镁合金表面的酸性溶液及处理方法
CN101510501A (zh) * 2008-01-22 2009-08-19 东京毅力科创株式会社 基板处理装置用的部件以及皮膜形成方法
CN101623944A (zh) * 2009-08-10 2010-01-13 北京华盛荣镁业科技有限公司 镁合金夹层板及镁合金夹层板的制备方法
CN102234803A (zh) * 2010-05-07 2011-11-09 中国科学院金属研究所 镁合金等离子氧化陶瓷膜表面复合涂层制备方法
CN103088384A (zh) * 2011-11-04 2013-05-08 和淞科技股份有限公司 阀金属等离子体电解氧化表面处理方法
CN103938253A (zh) * 2013-01-23 2014-07-23 汉达精密电子(昆山)有限公司 镁合金阳极氧化电解液及其对镁合金处理的方法

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1772968A (zh) * 2005-11-02 2006-05-17 哈尔滨工业大学 一种镁合金表面微弧氧化的方法
CN100585023C (zh) * 2006-07-25 2010-01-27 台山市金桥铝型材厂有限公司 一种铝型材的硬质阳极氧化膜的制备工艺
CN101928976B (zh) * 2010-08-20 2012-05-30 上海交通大学 镁合金阳极氧化用离子交换膜电解槽及其氧化方法
CN102409383B (zh) * 2011-11-09 2014-05-14 嘉兴学院 镁合金阳极氧化方法
EP2937447B1 (en) * 2012-12-21 2018-10-10 Okuno Chemical Industries Co., Ltd. Conductive coating film forming bath
CN103088389B (zh) * 2013-01-08 2015-07-22 重庆研镁科技有限公司 镁合金阳极氧化溶液及阳极氧化着色工艺
CN105063722B (zh) * 2015-09-21 2017-08-25 四川理工学院 一种硅烷偶联剂抑弧的微弧氧化电解质溶液及微弧氧化膜制备方法

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003166098A (ja) * 2001-11-30 2003-06-13 Kasatani:Kk マグネシウム合金の陽極酸化処理用組成物および処理方法
KR20040028908A (ko) * 2004-03-18 2004-04-03 (주)케이엠티 마그네슘 합금의 대면적 양산성을 고려한 내식성 향상을위한 시약 합성방법
CN101040066A (zh) * 2004-07-23 2007-09-19 坎梅陶尔股份有限公司 在由可阳极氧化金属或合金制成的物品上形成高抗腐蚀性硬涂层的方法
CN101285193A (zh) * 2007-04-09 2008-10-15 比亚迪股份有限公司 一种用于处理镁合金表面的酸性溶液及处理方法
CN101510501A (zh) * 2008-01-22 2009-08-19 东京毅力科创株式会社 基板处理装置用的部件以及皮膜形成方法
CN101239009A (zh) * 2008-01-29 2008-08-13 乐普(北京)医疗器械股份有限公司 可控降解的微弧氧化金属支架及其制备方法
CN101623944A (zh) * 2009-08-10 2010-01-13 北京华盛荣镁业科技有限公司 镁合金夹层板及镁合金夹层板的制备方法
CN102234803A (zh) * 2010-05-07 2011-11-09 中国科学院金属研究所 镁合金等离子氧化陶瓷膜表面复合涂层制备方法
CN103088384A (zh) * 2011-11-04 2013-05-08 和淞科技股份有限公司 阀金属等离子体电解氧化表面处理方法
CN103938253A (zh) * 2013-01-23 2014-07-23 汉达精密电子(昆山)有限公司 镁合金阳极氧化电解液及其对镁合金处理的方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113737249A (zh) * 2021-10-08 2021-12-03 东莞市恒核机电科技有限公司 一种镁合金黑色弧光放电陶瓷层的制备方法

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