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Frontiers of Materials Science

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Front. Mater. Sci.    2016, Vol. 10 Issue (2) : 134-146    https://doi.org/10.1007/s11706-016-0332-1
RESEARCH ARTICLE
Corrosion resistance of biodegradable polymeric layer-by-layer coatings on magnesium alloy AZ31
Lan-Yue CUI1,2,Rong-Chang ZENG1,2,*(),Xiao-Xiao ZHU1,Ting-Ting PANG1,Shuo-Qi LI1,2,*(),Fen ZHANG1,2
1. College of Materials Science and Engineering, Shandong University of Science and Technology, Qingdao 266590, China
2. State Key Laboratory of Mining Disaster Prevention and Control Co-founded by Shandong Province and the Ministry of Science and Technology, Shandong University of Science and Technology, Qingdao 266590, China
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Abstract

Biocompatible polyelectrolyte multilayers (PEMs) and polysiloxane hybrid coatings were prepared to improve the corrosion resistance of biodegradable Mg alloy AZ31. The PEMs, which contained alternating poly(sodium 4-styrenesulfonate) (PSS) and poly(allylamine hydrochloride) (PAH), were first self-assembled on the surface of the AZ31 alloy substrate via electrostatic interactions, designated as (PAH/PSS)5/AZ31. Then, the (PAH/PSS)5/AZ31 samples were dipped into a methyltrimethoxysilane (MTMS) solution to fabricate the PMTMS films, designated as PMTMS/(PAH/PSS)5/AZ31. The surface morphologies, microstructures and chemical compositions of the films were investigated by FE-SEM, FTIR, XRD and XPS. Potentiodynamic polarization, electrochemical impedance spectroscopy and hydrogen evolution measurements demonstrated that the PMTMS/(PAH/PSS)5/AZ31 composite film significantly enhanced the corrosion resistance of the AZ31 alloy in Hank’s balanced salt solution (HBSS). The PAH and PSS films effectively improved the deposition of Ca–P compounds including Ca3(PO4)2 and hydroxyapatite (HA). Moreover, the corrosion mechanism of the composite coating was discussed. These coatings could be an alternative candidate coating for biodegradable Mg alloys.
Keywords magnesium alloy      polyelectrolyte      polysiloxane      corrosion      layer-by-layer     
Corresponding Author(s): Rong-Chang ZENG,Shuo-Qi LI   
Online First Date: 16 March 2016    Issue Date: 11 May 2016
 Cite this article:   
Lan-Yue CUI,Rong-Chang ZENG,Xiao-Xiao ZHU, et al. Corrosion resistance of biodegradable polymeric layer-by-layer coatings on magnesium alloy AZ31[J]. Front. Mater. Sci., 2016, 10(2): 134-146.
 URL:  
https://academic.hep.com.cn/foms/EN/10.1007/s11706-016-0332-1
https://academic.hep.com.cn/foms/EN/Y2016/V10/I2/134
Fig.1  Schematic representation of the preparation of the PMTMS/(PAH/PSS)5/AZ31 films and corresponding chemical structures of PEI, PAH, PSS and MTMS.
Fig.2  Macro-photographs and FE-SEM images of (a)(d) the bare AZ31 substrate, (b)(e) the (PAH/PSS)5/AZ31 film and (c)(f) the PMTMS/(PAH/PSS)5/AZ31 film.
Fig.3  Cross-sectional SEM images of (a) the PMTMS/(PAH/PSS)5/AZ31 films and its corresponding (b) EDS mapping of elemental Si, (c)(d) the EDS spectra of points 1 and 4 and (e)(f)(g)(h)(i) the linear scanning images.
EDS spectrum Mass content /wt.%
C O Mg Si S
Spectrum 1 69.28 19.98 5.34 4.79 0.61
Spectrum 2 68.89 19.21 5.30 5.06 0.55
Spectrum 3 69.28 21.06 4.74 4.46 0.46
Spectrum 4 – 15.89 84.11 – –
Tab.1  The mass contents of C, O, Mg, Si and S elements for different EDS spectra
Fig.4  FTIR spectrum of the PMTMS/(PAH/PSS)5/AZ31 films.
Fig.5  XPS survey scan of (a) the (PAH/PSS)5/AZ31 and the PMTMS/(PAH/PSS)5/AZ31 films, and high resolutions of (b) the Si2p peak and (c) the C1s peak of the PMTMS/(PAH/PSS)5/AZ31 films.
Fig.6  Polarization curves of the bare AZ31 substrate (a), (PAH/PSS)5/AZ31 film (b) and PMTMS/(PAH/PSS)5/AZ31 film (c) in HBSS.
Sample Ecorr /(mV, SCE) icorr /(A·cm-2) Eb /(mV, SCE)
AZ31 substrate -1492 2.65×10-5 –
(PAH/PSS)5/AZ31 film -1432 8.45×10-7 -1336
PMTMS/(PAH/PSS)5/AZ31 film -1358 6.65×10-8 -1328
Tab.2  Electrochemical parameters of the polarization curves
Fig.7  (a) Nyquist plots and fitting curves, (b) Bode plots and (c) Bode plots of phase angle vs. frequency for the bare AZ31 substrate (i), the (PAH/PSS)5/AZ31 film (ii) and the PMTMS/(PAH/PSS)5/AZ31 film (iii) in HBSS.
Fig.8  HER as a function of immersion time for the bare AZ31 substrate (a), (PAH/PSS)5/AZ31 film (b) and PMTMS/(PAH/PSS)5/AZ31 film (c) in HBSS for 150 h.
Fig.9  Nyquist plots and Bode plots of (a)(b) the (PAH/PSS)5/AZ31 and (c)(d) the PMTMS/(PAH/PSS)5/AZ31 films in HBSS after immersions of 1 min, 1 h, 12 h, 24 h, 36 h and 48 h, its corresponding equivalent circuits for fitting the impedance data for (e) the bare AZ31, the (PAH/PSS)5/AZ31 and (PAH/PSS)5/AZ31 in HBSS at the initial 1 h of immersion, (f) the (PAH/PSS)5/AZ31 after 1 h of immersion and the PMTMS/(PAH/PSS)5/AZ31 during 48 h of immersion.
Sample RS/(Ω?cm2) Rf1/(Ω?cm2) CPE1/(Ω-1?sn?cm-2) n1 C/(Ω-1?sn?cm-2) Rf2/(Ω?cm2) C/(Ω-1?sn?cm-2) Rct/(Ω?cm2)
AZ31 substrate 77.73 1179 1.923E-5 0.8654 – – 1.479E-3 451.8
(PAH/PSS)5/AZ31 film 82.31 4332 9.994E-6 0.799 – – 1.752E-3 2142
PMTMS/(PAH/PSS)5/AZ31 film 60.01 1.923E4 1.197E-6 0.6473 2.984E-7 3.709E5 2.668E-6 7.854E4
(PAH/PSS)5/AZ31 film, 1 min 67.05 2360 1.094E-5 0.7674 – – 1.627E-4 3661
(PAH/PSS)5/AZ31 film, 1 h 59.16 4157 1.545E-5 0.6315 – – 1.91E-6 7988
(PAH/PSS)5/AZ31 film, 12 h 56.21 1736 1.001E-5 0.6797 7.613E-7 1.291E4 1.09E-9 1.776E4
(PAH/PSS)5/AZ31 film, 24 h 68.39 2828 7.581E-6 0.6841 2.372E-6 1.563E4 3.123E-6 1.015E4
(PAH/PSS)5/AZ31 film, 36 h 64.73 2979 9.628E-6 0.728 3.991E-7 1.775E4 4.695E-6 1.147E5
(PAH/PSS)5/AZ31 film, 48 h 61.08 1832 1.06E-5 0.7199 6.434E-7 1.094E4 9.132E-5 1.095E4
PMTMS/(PAH/PSS)5/AZ31 film, 1 min 53.28 1.008E4 3.449E-6 0.6708 3.243E-7 2.661E4 1.538E-6 6.397E4
PMTMS/(PAH/PSS)5/AZ31 film, 1 h 66.75 6167 3.552E-6 0.738 8.588E-7 1.65E4 8.022E-4 5.162E4
PMTMS/(PAH/PSS)5/AZ31 film, 12 h 63.84 1.525E4 1.052E-6 0.7559 2.766E-6 1.593E4 7.763E-6 3.245E4
PMTMS/(PAH/PSS)5/AZ31 film, 24 h 58 9220 7.166E-6 0.6863 1.299E-6 5.298E4 4.929E-4 1.118E4
PMTMS/(PAH/PSS)5/AZ31 film, 36 h 49.92 6714 5.563E-6 0.6411 2.762E-7 2.377E4 2.413E-6 2.43E4
PMTMS/(PAH/PSS)5/AZ31 film, 48 h 50.81 3739 5.402E-6 0.6311 4.593E-8 1.925E4 5.711E-8 3.883E4
Tab.3  Electrochemical data obtained by equivalent circuit fitting of EIS curves
Fig.10  FE-SEM images and the corresponding EDS spectra of (a)(d) the bare AZ31 substrate, (b)(e) the (PAH/PSS)5/AZ31 film and (c)(f) the PMTMS/(PAH/PSS)5/AZ31 film in HBSS after a 150-h immersion.
Fig.11  XRD patterns of the bare AZ31 substrate, the (PAH/PSS)5/AZ31 film and the PMTMS/(PAH/PSS)5/AZ31 film in HBSS after 150 h.
Fig.12  A comparison of the corrosion resistances of various PEM films on Mg alloys [20,23,45].
Fig.13  Schematic representation of the corrosion mechanism of the PMTMS/(PAH/PSS)5/AZ31 films on the AZ31 substrate in HBSS.
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