技术领域technical field
本发明涉及轻金属表面处理技术领域，具体是一种表面具有军绿色微弧氧化陶瓷膜的铝合金及其制备方法。The invention relates to the technical field of light metal surface treatment, in particular to an aluminum alloy with a military green micro-arc oxidation ceramic film on the surface and a preparation method thereof.
背景技术Background technique
铝合金以重量轻、比强度高、导电率高、传热性好等特性被人们所熟知，而且在机械、电子、航天、航空领域已广泛应用，但由于其硬度低、耐蚀性差、耐磨性低使其受到限制。因此提高铝合金的表面硬度、耐蚀性能、耐磨性能和装饰性能成为现在铝合金发展的关键问题。Aluminum alloy is well known for its light weight, high specific strength, high electrical conductivity, and good heat transfer, and has been widely used in the fields of machinery, electronics, aerospace, and aviation. However, due to its low hardness, poor corrosion resistance, and Low abrasiveness limits it. Therefore, improving the surface hardness, corrosion resistance, wear resistance and decorative properties of aluminum alloys has become a key issue in the development of aluminum alloys.
微弧氧化技术又名等离子体微弧氧化，它是在普通阳极氧化技术的基础上，通过升高外加电压等措施获得。普通阳极氧化技术外加的电压比较低，一般低于30V，随着外加电压的升高，铝合金表面已经生成的阳极氧化膜就会被击穿、产生孔洞，最终局部的氧化膜脱落。前苏联科学家在20世纪60年代末发现，继续升高电压会在轻金属表面生成新的氧化膜，一般此氧化膜称陶瓷膜。这样得到的一层陶瓷层其耐磨性、耐蚀性等表面性能明显高于其它的表面强化处理技术，比如阳极氧化等等。测量其涂覆铝合金陶瓷层的显微硬度为2100HV，结合强度一般为56MPa左右。这种技术工艺简单，是轻金属材料表面强化处理的一项新技术，近年来已成为轻金属表面强化处理的研究热点之一。Micro-arc oxidation technology, also known as plasma micro-arc oxidation, is obtained by increasing the applied voltage on the basis of ordinary anodizing technology. The applied voltage of ordinary anodizing technology is relatively low, generally lower than 30V. As the applied voltage increases, the anodized film formed on the surface of the aluminum alloy will be broken down, holes will be formed, and eventually the local oxide film will fall off. Former Soviet scientists discovered in the late 1960s that continuing to increase the voltage would generate a new oxide film on the surface of light metals. Generally, this oxide film is called a ceramic film. The wear resistance, corrosion resistance and other surface properties of the ceramic layer obtained in this way are obviously higher than other surface strengthening treatment technologies, such as anodic oxidation and the like. The microhardness of the coated aluminum alloy ceramic layer is measured to be 2100HV, and the bonding strength is generally about 56MPa. This technique is simple and is a new technology for surface strengthening treatment of light metal materials. It has become one of the research hotspots in surface strengthening treatment of light metal materials in recent years.
随着微弧氧化应用范围的不断扩大，除了要求微弧氧化处理过的铝合金有高硬度、耐磨损、耐腐蚀、耐电压绝缘等特性，还要求经处理的铝合金表面具有某些特殊的颜色。比如适合野外作战的军用产品，除了要求上述性能，还要求产品表面是军绿色，以便于伪装。而现在的铝合金微弧氧化陶瓷膜大多是白色或者灰色，颜色单一。目前，有关绿色陶瓷膜的制备研究很多，不足之处为：（1）溶液中含有强腐蚀性物质，微弧氧化过程中溶液会挥发出有毒氟化氢，易对实验人员身体造成伤害（潘利华，稀土镁合金微弧氧化绿色陶瓷膜制备方法，中国科学院长春应用化学研究所）；（2）绿色陶瓷膜颜色太浅；如吉利大学在Na2SiO3、NaoH、EDTA-Na2、K2Cr2O7 的电解液中处理16min获得绿色陶瓷膜（李佳庆，铝合金表面不同颜色微弧氧化陶瓷膜的制备工艺研究，2009年吉林大学硕士学位论文）；（3）制出的绿色陶瓷膜基底有黑斑且表面绿色很淡，如兰州理工大学用NaAlO2、K2Cr2O7、少量NaOH和H2O2在镁合金表面制备绿色陶瓷膜（阎峰云，镁合金微弧氧化绿色陶瓷膜的制备）。With the continuous expansion of the application range of micro-arc oxidation, in addition to requiring the aluminum alloy treated by micro-arc oxidation to have high hardness, wear resistance, corrosion resistance, voltage insulation and other characteristics, it is also required that the surface of the treated aluminum alloy has some special properties. s color. For example, military products suitable for field operations, in addition to the above-mentioned performance, also require the surface of the product to be military green to facilitate camouflage. However, the current aluminum alloy micro-arc oxidation ceramic film is mostly white or gray, and the color is single. At present, there are many studies on the preparation of green ceramic membranes. The shortcomings are: (1) The solution contains strong corrosive substances. Micro-arc oxidation of magnesium alloy green ceramic film preparation method, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences); (2) The color of the green ceramic film is too light; such as Geely University in Na2 SiO3 , NaoH, EDTA-Na2 , K2 Cr2 O7 in the electrolyte for 16 minutes to obtain a green ceramic film (Li Jiaqing, research on the preparation process of micro-arc oxidation ceramic film of different colors on the surface of aluminum alloy, 2009 Jilin University master's degree thesis); (3) The green ceramic film substrate produced has Black spots and the surface green is very light, such as Lanzhou University of Technology with NaAlO2 , K2 Cr2 O7 , a small amount of NaOH and H2 O2 to prepare a green ceramic film on the surface of magnesium alloy (Yan Fengyun, micro-arc oxidation of magnesium alloy green ceramic film preparation).
发明内容Contents of the invention
本发明的目的是针对适合野外作战的军用产品既要耐磨、耐腐蚀还要便于伪装的特性，而提供一种表面具有军绿色微弧氧化陶瓷膜的铝合金及其制备方法。The purpose of the present invention is to provide an aluminum alloy with a military green micro-arc oxidation ceramic film on the surface and a preparation method thereof for military products suitable for field operations that are not only wear-resistant, corrosion-resistant, but also easy to camouflage.
实现本发明目的的技术方案是：The technical scheme that realizes the object of the present invention is:
一种表面具有军绿色微弧氧化陶瓷膜的铝合金的制备方法，包括电解液的配制，采用交流脉冲电源进行微弧氧化处理的步骤，具体是：A method for preparing an aluminum alloy with a military-green micro-arc oxidation ceramic film on its surface, comprising the steps of preparing an electrolyte and performing micro-arc oxidation treatment with an AC pulse power supply, specifically:
（1）在PVC塑料槽内注入按特定组分、浓度兑好的碱性电解液，在10~20℃下搅拌均匀，静置1~2小时后使用；(1) Inject the alkaline electrolyte mixed according to the specific composition and concentration into the PVC plastic tank, stir evenly at 10~20°C, and use it after standing for 1~2 hours;
所述的碱性电解液各成分重量与总体积比为：磷酸钠15 ~45g/L、硅酸钠20 ~40g/L、六偏磷酸钠15 ~20g/L、氢氧化钠2 ~5g/L、乙二胺四乙酸二钠3 ~10g/L、重铬酸钾1 ~4g/L、碳酸钠2 ~10g/L、十二烷基硫酸钠1 ~5g/L、过氧化氢2 ~8g/L，电解液的pH值为12～14；The weight and total volume ratio of each component of the alkaline electrolyte is: sodium phosphate 15 ~ 45g/L, sodium silicate 20 ~ 40g/L, sodium hexametaphosphate 15 ~ 20g/L, sodium hydroxide 2 ~ 5g/L L, disodium edetate 3 ~10g/L, potassium dichromate 1 ~4g/L, sodium carbonate 2 ~10g/L, sodium lauryl sulfate 1 ~5g/L, hydrogen peroxide 2 ~ 8g/L, the pH value of the electrolyte is 12-14;
（2）对铝合金基体表面进行打磨，打磨后在丙酮和氢氧化钠溶液中进行超声波清洗、再用去离子水清洗、吹干；(2) Grinding the surface of the aluminum alloy substrate, ultrasonic cleaning in acetone and sodium hydroxide solution after grinding, cleaning with deionized water, and drying;
（3）将铝合金基体作为阳极，取2个不锈钢片作为阴极，用夹具将铝合金基体固定在2个不锈钢片中间，并完全浸没在步骤(1)中的碱性电解液中，采用交流脉冲电源进行微弧氧化处理，处理时正向电压为270~600V、负向电压为10~100V、电流密度为10~20A/dm2、频率为550～850Hz、占空比为15%～45%、氧化时间为5～60min；(3) Use the aluminum alloy substrate as the anode, take 2 stainless steel sheets as the cathode, fix the aluminum alloy substrate in the middle of the 2 stainless steel sheets with a clamp, and completely immerse in the alkaline electrolyte in step (1). Pulse power supply for micro-arc oxidation treatment, the forward voltage is 270~600V, the negative voltage is 10~100V, the current density is 10~20A/dm2, the frequency is 550~850Hz, and the duty cycle is 15%~45%. , Oxidation time is 5~60min;
（4）将经微弧氧化处理后的铝合金基体，在pH值为5.5～6.5，90～100℃的去离子水中放置40~50min，取出铝合金基体，清洗，吹干，即可制得表面具有军绿色微弧氧化陶瓷膜的铝合金。(4) Place the aluminum alloy substrate after micro-arc oxidation treatment in deionized water with a pH value of 5.5 to 6.5 and 90 to 100°C for 40 to 50 minutes, take out the aluminum alloy substrate, wash it, and dry it to obtain Aluminum alloy with army green micro-arc oxidation ceramic film on the surface.
本发明另一目的是提供一种用上述方法制得的表面具有军绿色微弧氧化陶瓷膜的铝合金。Another object of the present invention is to provide an aluminum alloy with army green micro-arc oxidation ceramic film on the surface prepared by the above method.
所述的军绿色陶瓷膜的厚度为20μm～35μm，表层硬度为1700～1800HV。The thickness of the army green ceramic membrane is 20 μm-35 μm, and the hardness of the surface layer is 1700-1800 HV.
本发明的有益效果是：制备方法简单、成本低、对环境污染小，适用面广，对轻金属都适用，如在铝、镁、钛及其合金表面都可以微弧氧化制得军绿色陶瓷膜。制备的军绿色陶瓷膜具有耐磨性高、耐蚀性好、色泽均匀、致密、稳定性好、不易褪色等优点，特别适于军用产品的伪装需要。The beneficial effect of the present invention is: the preparation method is simple, the cost is low, the pollution to the environment is small, the application range is wide, and it is suitable for light metals. . The prepared military green ceramic film has the advantages of high wear resistance, good corrosion resistance, uniform color, compactness, good stability, and not easy to fade, and is especially suitable for the camouflage needs of military products.
附图说明Description of drawings
图1为本发明表面具有军绿色微弧氧化陶瓷膜的铝合金断面结构示意图；Fig. 1 is the cross-sectional structure schematic diagram of the aluminum alloy with military green micro-arc oxidation ceramic film on the surface of the present invention;
图中：1.铝合金基体 2. 军绿色陶瓷膜；In the picture: 1. Aluminum alloy substrate 2. Army green ceramic film;
图2为实施例1表面形貌扫描电镜图；Fig. 2 is the scanning electron micrograph of embodiment 1 surface topography;
图3为实施例1截面形貌扫描电镜图。3 is a scanning electron microscope image of the cross-sectional morphology of Example 1.
具体实施方式detailed description
下面结合附图和实施例对本发明的内容作进一步的阐述，但不是对本发明的限定。The content of the present invention will be further described below in conjunction with the accompanying drawings and embodiments, but the present invention is not limited.
实施例1Example 1
参照图1，本发明一种表面具有军绿色微弧氧化陶瓷膜的铝合金，由铝合金基体1和覆合在铝合金基体1表面的军绿色陶瓷膜2组成。Referring to FIG. 1 , an aluminum alloy with a military green micro-arc oxidation ceramic film on the surface of the present invention is composed of an aluminum alloy substrate 1 and a military green ceramic film 2 coated on the surface of the aluminum alloy substrate 1 .
铝合金基体：采用6061型铝合金，尺寸：30mm×20mm×3mm。Aluminum alloy substrate: 6061 aluminum alloy, size: 30mm×20mm×3mm.
本发明的制备方法是：The preparation method of the present invention is:
（1）在PVC塑料槽内注入按特定组分、浓度兑好的碱性电解液，在10~20℃下搅拌均匀，静置1~2小时后使用；(1) Inject the alkaline electrolyte mixed according to the specific composition and concentration into the PVC plastic tank, stir evenly at 10~20°C, and use it after standing for 1~2 hours;
所述的碱性电解液各成分重量与电解液总体积比为：磷酸钠25g/L、六偏磷酸钠15g/L、氢氧化钠4g/L、乙二胺四乙酸二钠3g/L、重铬酸钾3g/L、碳酸钠4g/L、十二烷基硫酸钠2g/L、过氧化氢2g/L， pH值为12～14；The weight of each component of the alkaline electrolyte and the total volume ratio of the electrolyte are: sodium phosphate 25g/L, sodium hexametaphosphate 15g/L, sodium hydroxide 4g/L, disodium edetate 3g/L, Potassium dichromate 3g/L, sodium carbonate 4g/L, sodium lauryl sulfate 2g/L, hydrogen peroxide 2g/L, pH value 12-14;
（2）依次用400#、600#、800#、1000#的耐水砂纸将铝合金基体表面打磨光滑至表面划痕方向一致，打磨后在丙酮和氢氧化钠溶液中进行超声波清洗15min，再用去离子水清洗、吹干，去除表面的氧化物；(2) Use 400#, 600#, 800#, and 1000# water-resistant sandpaper to polish the surface of the aluminum alloy substrate until the surface scratches are in the same direction. After polishing, perform ultrasonic cleaning in acetone and sodium hydroxide solution for 15 minutes, and then use Wash with deionized water and dry to remove oxides on the surface;
（3）将铝合金基体作为阳极，取2个不锈钢片作为阴极，用夹具将铝合金基体固定在2个不锈钢片中间，并完全浸没在步骤(1)的碱性电解液中，采用交流脉冲电源进行微弧氧化处理，处理时正向电压为358~400V、负向电压为25V、电流密度为20A/dm2、脉冲频率为550Hz、占空比为15%、正脉冲数为15、负脉冲数为3、氧化时间为60min；(3) Use the aluminum alloy substrate as the anode, take 2 stainless steel sheets as the cathode, fix the aluminum alloy substrate between the 2 stainless steel sheets with a clamp, and completely immerse in the alkaline electrolyte in step (1), and use AC pulse The power supply is subjected to micro-arc oxidation treatment. During the treatment, the forward voltage is 358~400V, the negative voltage is 25V, the current density is 20A/dm2 , the pulse frequency is 550Hz, the duty cycle is 15%, the number of positive pulses is 15, and the negative pulse number is 15. The number of pulses is 3, and the oxidation time is 60 minutes;
（4）将经微弧氧化处理后的铝合金基体，在pH值为5.5～6.5，90～100℃的去离子水中放置40~50min，取出铝合金基体，用去离子水清洗，在蒸馏水中浸泡10min ，吹干，即可制得表面具有军绿色微弧氧化陶瓷膜的铝合金。(4) Place the aluminum alloy substrate after micro-arc oxidation treatment in deionized water with a pH value of 5.5-6.5 and 90-100°C for 40-50 minutes, take out the aluminum alloy substrate, wash it with deionized water, and place it in distilled water. After soaking for 10 minutes and blowing dry, an aluminum alloy with a military green micro-arc oxidation ceramic film on the surface can be prepared.
利用扫描电子显微镜观察到军绿色陶瓷膜表面形貌扫描电镜图2、截面形貌扫描电镜图3，显微硬度为1800HV，用膜层测厚仪检测陶瓷膜的厚度为33.9μm。Using a scanning electron microscope to observe the surface morphology of the army green ceramic membrane scanning electron microscope Figure 2, and the cross-sectional morphology scanning electron microscope Figure 3, the microhardness is 1800HV, and the thickness of the ceramic membrane is 33.9 μm measured by a film thickness gauge.
实施例2Example 2
一种表面具有军绿色微弧氧化陶瓷膜的铝合金的制备，铝合金基体：采用 6061型铝合金，尺寸：30mm×20mm×3mm。Preparation of an aluminum alloy with a military green micro-arc oxidation ceramic film on the surface, the aluminum alloy substrate: 6061 aluminum alloy, size: 30mm×20mm×3mm.
所述的碱性电解液各成分重量与电解液总体积比为：磷酸钠30g/L、硅酸钠30g/L、六偏磷酸钠20g/L、氢氧化钠3g/L、乙二胺四乙酸二钠4g/L、重铬酸钾3.5g/L、碳酸钠4g/L、十二烷基硫酸钠3g/L、过氧化氢2g/L；微弧氧化时间为20min，电流密度为10 A/dm2，其余制备方法与实施例1相同，制得的陶瓷膜厚度为20.2μm，显微硬度为1700HV。The weight of each component of the alkaline electrolyte and the total volume ratio of the electrolyte are: sodium phosphate 30g/L, sodium silicate 30g/L, sodium hexametaphosphate 20g/L, sodium hydroxide 3g/L, ethylenediaminetetra Disodium acetate 4g/L, potassium dichromate 3.5g/L, sodium carbonate 4g/L, sodium lauryl sulfate 3g/L, hydrogen peroxide 2g/L; micro-arc oxidation time is 20min, current density is 10 A/dm2 , the rest of the preparation method is the same as in Example 1, the thickness of the prepared ceramic film is 20.2 μm, and the microhardness is 1700HV.
实施例3Example 3
一种表面具有军绿色微弧氧化陶瓷膜的铝合金的制备，铝合金基体：采用 6061型铝合金，尺寸：20mm×15mm×1mm。Preparation of an aluminum alloy with a military green micro-arc oxidation ceramic film on the surface, the aluminum alloy substrate: 6061 aluminum alloy, size: 20mm×15mm×1mm.
所述的碱性电解液各成分重量与电解液总体积比为：硅酸钠40g/L、六偏磷酸钠18g/L、氢氧化钠4g/L、乙二胺四乙酸二钠2g/L、重铬酸钾4g/L、碳酸钠10g/L、十二烷基硫酸钠5g/L、过氧化氢2g/L；微弧氧化时间为45min，电流密度为10 A/dm2，其余制备方法与实施例1相同，制得的陶瓷膜厚度为21.4μm，显微硬度为1700HV。The ratio of the weight of each component of the alkaline electrolyte to the total volume of the electrolyte is: sodium silicate 40g/L, sodium hexametaphosphate 18g/L, sodium hydroxide 4g/L, disodium edetate 2g/L , potassium dichromate 4g/L, sodium carbonate 10g/L, sodium lauryl sulfate 5g/L, hydrogen peroxide 2g/L; the micro-arc oxidation time is 45min, the current density is 10 A/dm2 , and the rest are prepared The method is the same as in Example 1, and the thickness of the prepared ceramic film is 21.4 μm, and the microhardness is 1700 HV.
实施例4Example 4
一种表面具有军绿色微弧氧化陶瓷膜的铝合金的制备，铝合金基体：采用LY型铝合金，尺寸：直径35mm，厚度2mm。Preparation of an aluminum alloy with a military green micro-arc oxidation ceramic film on the surface, the aluminum alloy substrate: LY-type aluminum alloy, size: diameter 35mm, thickness 2mm.
所述的碱性电解液各成分重量与总体积比为：硅酸钠35g/L、六偏磷酸钠16g/L、氢氧化钠2g/L、乙二胺四乙酸二钠8g/L、重铬酸钾都为2.7g/L、碳酸钠10g/L、十二烷基硫酸钠3.5g/L、过氧化氢5.5g/L；微弧氧化时间为30min，电流密度为15 A/dm2，其余制备方法与实施例1相同，制得的陶瓷膜厚度为25.7μm，显微硬度为1750HV。The weight and total volume ratio of each component of the alkaline electrolyte is: sodium silicate 35g/L, sodium hexametaphosphate 16g/L, sodium hydroxide 2g/L, disodium edetate 8g/L, weight Potassium chromate is 2.7g/L, sodium carbonate is 10g/L, sodium lauryl sulfate is 3.5g/L, hydrogen peroxide is 5.5g/L; the micro-arc oxidation time is 30min, and the current density is 15A /dm2 , the rest of the preparation method is the same as in Example 1, the thickness of the prepared ceramic film is 25.7 μm, and the microhardness is 1750HV.
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