Preparation of Trivalent Chromium Coating on 6063 Aluminum Alloy Jian-Zhen HUANG 1,a,* and You-Xiong LUO 1,b

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1 2017 Joint International Conference on Materials Science and Engineering Application (ICMSEA 2017) and International Conference on Mechanics, Civil Engineering and Building Materials (MCEBM 2017) ISBN: Preparation of Trivalent Chromium Coating on 6063 Aluminum Alloy Jian-Zhen HUANG 1,a,* and You-Xiong LUO 1,b 1 Foshan Supervision and Testing Centre of Quality and Metrology, Foshan, Guangdong , China a lyf @163.com, b @qq.com * Corresponding author Keywords: Aluminum alloy, Trivalent chromium, Coating, Corrosion resistance. Abstract. The trivalent chromium coating was deposited on the surface of 6063 aluminum alloy with Cr 2 (SO 4 ) 3, H 3 PO 4 and K 2 ZrF 6. The performances of trivalent chromium conversion coating were analyzed by CuSO4 dropping corrosion test, electrochemical polarization curve, scanning electron microscope (SEM) and energy dispersive X-ray analysis (EDAX). The conversion coating shows gray color and consists of Cr, Zr, K, Al, P, O. The analytical results indicate that the aluminum alloy coated with trivalent chromium exhibits better corrosion resistance than the pure aluminum alloy. Introduction Because of its excellent corrosion resistance, chromate conversion coating is widely used in the surface treatment of aluminum alloys, Mg, Zn and steel [1-3]. However, due to the toxicity of hexavalent chromium in the conversion coating, RoHS directive of European Union (EU) has have imposed severe restrictions on the use of chromate. Thus, many researchers devoted to developing environment friendly chemical conversion coatings, such as Ti-Zr based, trivalent chromium, rare earth salt, chromate and molybdate conversion coating. Among these conversion coatings, trivalent chromium conversion coating is one of the most promising alternatives to chromate conversion coating [4-7]. Sameh et al. investigated the formation mechanism of trivalent chromium coating on aluminum alloy with situ spectroscopic ellipsometry. They found that the formation of trivalent chromium coating included the chemical thinning of the native Al 2 O 3 layer and the rapid formation of trivalent chromium [8]. Yu et al. studied the EIS of trivalent chromium coating on Al 6063 alloy. Their results revealed that the formation and quality of trivalent chromium coating were very sensitive to the ph value in the bath [9]. Qi et al. investigated the behavior of trivalent chromium in the coating. They found trivalent chromium can be oxided to hexavalent chromium in the air [10]. Therefore, many challenges appear in the preparation of trivalent chromium coating with excellent corrosion resistance. In this study, the trivalent chromium coating for aluminum alloy was prepared with Cr 2 (SO 4 ) 3, H 3 PO 4 and K 2 ZrF 6. The corrosion resistance, morphology and electrochemical properties of conversion coating were studied with SEM, EDAX and polarization curve. Experimental Materials 6063 aluminum alloy was used in this study. The major elements of aluminum alloy are listed in Table 1. All chemicals of this work were AR grade. And deionized water was used to prepare all solutions.

2 Table 1. Chemical composition of 6063 aluminum alloy. Element Mg Si Fe Cu Zn Mn Cr Ti Al W [%] Balance Experiment Procedure Before the chemical conversion treatment, the aluminum alloy sheets were washed with alcohol and deionized water. Then, the washed alloy sheets were activated with 10% NaOH aqueous solution for 1 min and washed with deionized water. At last, the alloy sheets were immersed in the bath containing trivalent chromium. A typical surface conversion treatment solution contains 10 g/l Cr 2 (SO 4 ) 3, 2 g/l K 2 ZrF 6, 10 g/l H 3 PO 4. The surface conversion treatment was controlled at 40 o C for 10 min. Examination Techniques Surface morphology of the trivalent chromium conversion coatings was investigated by scanning electron microscopy (SEM) (MIRA3 TESCAN) equipped with energy dispersive X-ray analysis (EDAX). The corrosion resistance of the coating was evaluated by copper sulfate (3g CuSO 4 +1mL HCl+75mL H 2 O) dropping test. The electrochemical properties of the trivalent chromium conversion coatings were chastised by electrochemical workstation (CHI Instruments Cordova). All the measurements were conducted in a three electrodes system 3.5% NaCl aqueous solution. The alloy with the conversion coating was used for work electrode. And the density of coating was calculated as follow: P=(W 2 -W 1 )/S, W 1 is the weight of aluminum alloy sheet, W 2 is the weight of aluminum alloy sheet after conversion treatment, S is the area of aluminum alloy sheet. Results and Discussion Formation Mechanism of Trivalent Chromium Coating During the pretreatment, the aluminum on the surface of aluminum alloy was oxided as follow: Al + 2OH - = AlO H 2 (1) Then, the impurity was rinsed in the reaction and a clean alloy surface was achieved. During the conversion treatment, the formation of trivalent chromium coating was resulted from the increase of ph on the alloy surface: 2Al + 3H 2 O Al 2 O 3 + 6H + + 6e (2) Al Al e (3) 2H + + 2e 2H 2 (4) O 2 + 2H 2 O + 4e 4OH - (5) On the other hand, the consistent in the solution ionize as follow: K 2 ZrF 6 2K + + ZrF 6 Cr 2 (SO 4 ) 3 2Cr SO 4 H 3 PO 4 H + + H 2 PO 4 - (6) (7) (8)

3 H 2 PO 4 - H + + HPO 4 HPO 4 H + + PO 4 3- (9) (10) At last, the conversion coating was formed on the surface of alloy as follow: ZrF OH - ZrO H 2 O + 6F - (11) Cr OH - Cr(OH) 3 (12) Al OH - Al (OH) 3 (13) Cr 3+ + PO 4 3- CrPO 4 (14) Al 3+ + PO 4 3- AlPO 4 (15) Thus, the formation of trivalent chromium coating includes two steps: (1) the chemical thinning of the Al 2 O 3 layer, (2) formation of the trivalent chromium coating. The formation model of trivalent chromium coating on aluminum alloy surface was shown in Fig. 1. Figure 1. Formation model of trivalent chromium coating on aluminum alloy surface. Figure 2. Effect of Cr2(SO4)3 concentration on the density and the corrosion resistance of trivalent chromium coating.

4 Corrosion Resistance The corrosion resistance of trivalent chromium coating was evaluated by copper sulfate dropping test. The effect of Cr 2 (SO 4 ) 3 concentration on the density and the corrosion resistance of conversion coating was studied under the conditions of 2 g/l K 2 ZrF 6, 10 g/l H 3 PO 4 and 40 o C. And the surface conversion reaction was controlled at 10 min. The results are shown in Fig. 2. The density of conversion coating (from 323 g/cm 2 to 430 g/cm 2 ) is increased with the increase of Cr 2 (SO 4 ) 3 concentration. However, the dropping time of CuSO 4 increases with the increase of Cr 2 (SO 4 ) 3 concentration when Cr 2 (SO 4 ) 3 concentration is less than 10 g/l. Then, the CuSO 4 dropping time decrease with with the increase of Cr 2 (SO 4 ) 3 concentration when Cr 2 (SO 4 ) 3 concentration is more than 10 g/l. Because the reaction rate is low at low reactant concentration, it is conducive to the evently deposition of conversion coating on the surface of aluminum alloy sheet. A too high reactant concentration will result in a too high reaction rate. Then, a uneven coating will be obtained, which will has a negative impact on the corrosion resistance of conversion coating. Morphology and Chemical Composition Figure 3. SEM imges of aluminum alloy (a) and aluminum alloy with trivalent chromium coating (b). Fig. 3 presents the SEM images of the aluminum alloy and aluminum alloy with trivalent chromium coating (10 g/l Cr 2 (SO 4 ) 3, 2 g/l K 2 ZrF 6, 10 g/l H 3 PO 4, 40 o C, 10 min). The surface of pure aluminum alloy is very smooth. There is little particles can be seen on the alloy surface. However, the alloy surface becomes rough after the surface conversion treatment. The trivalent chromium conversion coating is charactized by distributed sparsely, 1~2 µm, and spherical particles. In addition, the conversion coating exhibited cracking because of the vacuum during SEM measurement. Similar phenomenon was observed in other reports on the trivalent chromium conversion coating. Figure 4. EDAX patterns of aluminum alloy (a) and aluminum alloy with trivalent chromium coating (b).

5 Fig. 4 presents the EDAX patterns of the aluminum alloy and aluminum alloy with trivalent chromium coating (10 g/l Cr 2 (SO 4 ) 3, 2 g/l K 2 ZrF 6, 10 g/l H 3 PO 4, 40 o C, 10 min). The pure aluminum alloy contains alloy elements Mg and Si, besides the aluminum. It reveals that the alloy is 6063 aluminum alloy. After the surface conversion treatment, the alloy surface contains Cr, P, Zr and K, besides the aluminum. It indicates the conversion coating is trivalent chromium coating. Conclusion (1) The optimized process conditions for conversion treatment are as follows: 10 g/l Cr 2 (SO 4 ) 3, 2 g/l K 2 ZrF 6, 10 g/l H 3 PO 4, temperature 40 o C, and reaction time 10 min. (2) The conversion coating is charactized by distributed sparsely, 1~2 µm, and spherical particles. The coating contains Cr, P, Zr and K. (3) The trivalent chromium coating enhanced the corrosion resistance of aluminum alloy after surface conversion treatment. References [1] N. T. Wen, C. S. Lin, C. Y. Bai, M. D. Ger, Structures and characteristics of Cr(III)-based conversion coatings on electrogalvanized steels, Surf. Coat. Technol. 203 (2008) [2] Y. Guo, G. S. Frankel, Characterization of trivalent chromium process coating on AA2024-T3, Surf. Coat. Technol. 206 (2012) [3] H. A. Ramezani-Varzaneh, S. R. Allahkaram, M. Isakhani-Zakaria, Effects of phosphorus content on corrosion behavior of trivalent chromium coatings in 3.5 wt.% NaCl solution, Surf. Coat. Technol. 244 (2014) [4] F. O. George, P. Skeldon, G. E. Thompson, Formation of zirconium-based conversion coatings on aluminum and Al Cu alloys, Corros. Sci. 65 (2012) [5] A. H. Yi, W. F. Li, J. Du, S. L. Mu, Preparation and properties of chrome-free colored Ti/Zr based conversion coating on aluminum alloy, Appl. Surf. Sci. 258 (2012) [6] O. Lunder, C. Simensen, Y. Yu, K. Nisancioglu, Formation and characterization of Ti Zr based conversion layers on AA6060 aluminium, Surf. Coat. Technol. 184 (2004) [7] X. Zuo, W. F. Li, S. L. Mu, J. Du, Y. Y Yang, P. Tang, Investigation of composition and structure for a novel Ti Zr chemical conversion coating on 6063 aluminum alloy, Prog. Org. Coat. 87 (2015) [8] S. Dardona, M. Jaworowski, In situ spectroscopic ellipsometry studies of trivalent chromium coating on aluminum, Appl. Phys. Lett. 97 (2010) [9] H. C. Yu, B. Z. Chen, X. C. Shi, X. L. Sun, B. Li, Investigation of the trivalent-chrome coating on 6063 aluminum alloy, Mater. Lett. 62 (2008) [10] J. T. Qi, T. Hashimoto, J. R. Walton, X. Zhou, P. Skeldon, G. E. Thompson, Trivalent chromium conversion coating formation on aluminum, Surf. Coat. Technol. 280 (2015)

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