Comparison of Corrosion Resistance of Phenylalanine, Methionine, and Asparagine-Induced Ca-P Coatings on AZ31 Magnesium Alloys

doi:10.11900/0412.1961.2021.00058

Acta Metall Sin

2021, Vol. 57

Issue (10): 1258-1271 DOI: 10.11900/0412.1961.2021.00058

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Comparison of Corrosion Resistance of Phenylalanine, Methionine, and Asparagine-Induced Ca-P Coatings on AZ31 Magnesium Alloys

WANG Xuemei¹, YIN Zhengzheng¹, YU Xiaotong¹, ZOU Yuhong², ZENG Rongchang¹^,³^,⁴(

)

^1.School of Materials Science and Engineering, Shandong University of Science and Technology, Qingdao 266590, China
^2.School of Chemical and Biological Engineering, Shandong University of Science and Technology, Qingdao 266590, China
^3.School of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450002, China
^4.Hubei Key Laboratory of Advanced Technology for Automotive Components, Wuhan University of Technology, Wuhan 430070, China

Cite this article:

WANG Xuemei, YIN Zhengzheng, YU Xiaotong, ZOU Yuhong, ZENG Rongchang. Comparison of Corrosion Resistance of Phenylalanine, Methionine, and Asparagine-Induced Ca-P Coatings on AZ31 Magnesium Alloys. Acta Metall Sin, 2021, 57(10): 1258-1271.

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Abstract

Ca-P coating not only enhances the corrosion resistance of biodegradable magnesium alloys but also contributes to the formation of new bones and promotes bone integration around implants. However, the Ca-P coatings may have defects like porosity, low adhesion, and coarse grains, which lead to prefailure in the early stage and then the coatings cannot meet the requirements of long-term clinical service. Amino acids can induce the formation of calcium-bearing phosphates on biodegradable magnesium alloy. To clarify the influence of amino acid groups on film formation, Phenylalanine (Phe), Methionine (Met), and Asparagine (Asn) were used to regulate the degradation rate of magnesium alloy. Three amino acid-induced Ca-P (Ca-P_Phe, Ca-P_Met, and Ca-P_Asn) coatings were prepared on AZ31 magnesium alloy via a constant temperature water bath method at a temperature of 60^oC. Additionally, the morphology of the coatings, composition distributions, and phase structures were observed and analyzed via SEM, EDS, XRD, FTIR, and XPS. The corrosion resistance of the coating in simulated body fluid (Hank's solution) was investigated through electrochemical polarization, AC impedance, and hydrogen evolution tests. The formation mechanisms of amino acid additive-induced Ca-P (Ca-P_Phe, Ca-P_Met, and Ca-P_Asn) coatings on AZ31 magnesium alloy were probed. Results showed that the thicknesses of Ca-P, Ca-P_Phe, Ca-P_Met, and Ca-P_Asn coatings were about (3.47 ± 0.47), (6.06 ± 0.77), (7.63 ± 1.70), and (8.23 ± 1.37) μm, respectively. The main constituents of the amino acid-induced Ca-P coatings were CaHPO₄ and Ca₁₀(PO₄)₆(OH)₂ (HA). The results of electrochemical polarization curves, EIS, and hydrogen evolution tests demonstrated that the addition of amino acids enhanced the corrosion resistance of the Ca-P coatings, which was ascribed to the inhibition and adsorption of amino acid molecules on AZ31 magnesium alloy. The adsorption of the amino group was mainly achieved through the coupling of the lone pair electrons of nitrogen atoms with the surface, whereas the carboxyl group combined with Mg²⁺ via their oxygen atoms. Additionally, heteroatoms in amino acids could share their lone pair electrons with the vacant molecular orbitals of the magnesium alloy. A formation mechanism of amino acid-induced Ca-P coating was proposed.

Key words: AZ31 magnesium alloy coating amino acid adsorption corrosion resistance

Received: 01 February 2021

ZTFLH:

TG174

Fund: National Natural Science Foundation of China(52071191);Natural Science Foundation of Shandong Province(ZR2020ME011);Open Foundation of Hubei Key Laboratory of Advanced Technology for Automotive Components(XDQCKF2021006)

About author: ZENG Rongchang, professor, Tel: (0532)80681226, E-mail: rczeng@foxmail.com

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https://www.ams.org.cn/EN/10.11900/0412.1961.2021.00058 OR https://www.ams.org.cn/EN/Y2021/V57/I10/1258

Fig.1 Preparation diagram of Ca-P coating and its amino acids (Phenylalanine (Phe), Methionine (Met), and Asparagine (Asn)) modified coatings (Ca-P_Phe, Ca-P_Met,_{and Ca-P_Asn, respectively) on AZ31 Mg alloy}

Fig.2 SEM images of Ca-P coating (a-c), Ca-P_Phe coating (d-f), Ca-P_Met coating (g-i), and Ca-P_Asn coating (j-l) on AZ31 magnesium alloy surface

Table 1 EDS analysis results of points 1-12 in Fig.2

Fig.3 Cross-sectional SEM images and corresponding Ca and P mapping images of Ca-P coating (a), Ca-P_Phe coating (b), Ca-P_Met coating (c), and Ca-P_Asn coating (d) on AZ31 magnesium alloy surface

Fig.4 XPS survey plots (a, d, g) and high-resolution spectra (b, c, e, f, h, i) of Ca-P_Phe coating (a-c), Ca-P_Met coating (d-f), and Ca-P_Asn coating (g-i)

Fig.5 FTIR of Ca-P coating (a), Ca-P_Phe coating (b), Ca-P_Met coating (c), and Ca-P_Asn coating (d) on AZ31 magnesium alloy surface

Fig.6 XRD spectra of AZ31 Mg alloy (a), Ca-P coating (b), Ca-P_Phe coating (c), Ca-P_Met coating (d), and Ca-P_Asn coating (e) (HA—Ca₁₀(PO₄)₆(OH)₂)

Fig.7 Polarization curves of AZ31Mg alloy, Ca-P coating, Ca-P_Phe coating, Ca-P_Metcoating, and Ca-P_Asn coating (E_b—broken shield potential)

Table 2 Tafel analysis results of AZ31Mg alloy, Ca-P coating, Ca-P_Phecoating, Ca-P_Metcoating, and Ca-P_Asn coating

Fig.8 Nyquist (a) and Bode (b) curves of AZ31 Mg alloy, Ca-P coating, Ca-P_Phe coating, Ca-P_Met coating, and Ca-P_Asn coating (Z_im—imaginary part of impedance, Z_re—real part of impedance, |Z|—impedance modulus)

Fig.9 Equivalent circuits of AZ31 Mg alloy (a), Ca-P coating (b), and Ca-P_Phe/Met/Asn coating (c) (R_s—solution resistance, CPE—constant phase element, R_ct—charge transfer resistance, L—equivalent inductance, R_L—inductive resistance, R₁—coating resistance)

Sample	R_s	CPE₁	n₁	R₁	CPE₂	n₂	R_ct	L	R_L
	Ω·cm²	10^-5 Ω^-1·s $n 1$ ·cm^-2		kΩ·cm²	10^-5 Ω^-1·s $n 2$ ·cm^-2		Ω·cm²	H·cm²	Ω·cm²
AZ31	85.88	1.278	0.9056	-	-	-	578.5	439.7	231.5
Ca-P	57.25	0.136	0.6946	-	2.616	0.6438	593.8	3.7	6856.0
Ca-P_Phe	70.00	0.875	0.6515	289.6	1.582	0.7757	7266.0	-	-
Ca-P_Met	84.64	1.859	0.6809	226.3	1.693	0.8297	7465.0	-	-
Ca-P_Asn	80.93	0.742	0.6782	157.8	1.873	0.8144	8552.0	-	-

Table 3 EIS analysis results of AZ31 Mg alloy, Ca-P coating, Ca-P_Phe coating, Ca-P_Met coating, and Ca-P_Asn coating

Fig.10 Hydrogen evolution rate (HER) curves of AZ31Mg alloy, Ca-P coating, Ca-P_Phe coating, Ca-P_Metcoating, and Ca-P_Asn coating

Fig.11 Digital camera photographs (a, d, g, j, m) and SEM images (b, c, e, f, h, i, k, l, n, o) after 160 h immersion for AZ31 Mg alloy (a-c), Ca-P coating (d-f), Ca-P_Phe coating (g-i), Ca-P_Met coating (j-l), and Ca-P_Asn coating (m-o)

Table 4 EDS analysis results of points 1-15 in Fig.11

Fig.12 FTIR of AZ31 Mg alloy (a), Ca-P coating (b), Ca-P_Phe coating (c), Ca-P_Met coating (d), and Ca-P_Asn coating (e) immersed in Hank's solution after 160 h

Fig.13 XRD spectra of AZ31 Mg alloy (a), Ca-P coating (b), Ca-P_Phe coating (c), Ca-P_Metcoating (d), and Ca-P_Asn coating (e) immersed in Hank's solution after 160 h

Fig.14 Schematics of the formation mechanisms of Ca-P_Phe (a, b), Ca-P_Met (c, d), and Ca-P_Asn (e, f) coatings

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