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292 Surface Modification of Magnesium and its Alloys for Biomedical Applications
reported cases, the combination of chemical etching to produce micro/nanoscale hierarchical structures and surface modificati on resulted in coatings that exhibited
superhydrophobicity.
Hydrothermal treatments have also been successfully used to generate oxide/hydroxide barrier layers with micronanoscale hierarchical topography. These layers are formed
by dissolution and reprecipitation reactions that occur upon exposure of the alloy to
aqueous solution at high temperatures for periods of several hours or more. Several
authors have used hydrothermal treatment of magnesium alloys in pure water, producing
surfaces covered with magnesium hydroxide nanosheets with typical thicknesses of
approximately 100 nm (Ishizaki & Sakamoto, 2011; Ou et al., 2013). One interesting
advantage of this method is that the hydroxide layer can be color tuned depending on
the immersion time. A paper demonstrated that these coatings exhibit colors ranging
from metallic silver to orange, green, or orchid as a function of hydrothermal treatment
time (Ishizaki & Sakamoto, 2011). The hydrothermal method has also been used to
create a hydrotalcite/hydromagnesite conversion coating on the AZ31 alloy (J. Wang
et al., 2010). This conversion coating consisted of nanoscale flake-like structures that
completely covered the surface. Randomly distributed microscale papillae were also
observed.
The deposition of structured prelayers has also been explored as a way of producing
hierarchical topography on magnesium alloy surfaces. Microarc oxidation followed by
coating with hydrophobic nanoscale silica particles fabricated via the solegel method
has showed promise as an adherent, corrosion-resistant superhydrophobic coating
(S. Wang et al., 2012). Another promising method is the deposition of crystalline nanosheets of cerium oxide as a coating via a simple immersion process (Ishizaki et al.,
2011; Ishizaki & Saito, 2010; Liu et al., 2013). In each case, the superhydrophobic
films prepared by this method exhibited bett er corrosion resistance in sodium chloride
solutions than the unmodified magnesium alloy; however, due to the presence of
cracks in the coating, they did not have adequate long-term corrosion resistance.
The deposition of metallic layers by electroless plating and/or electrochemical deposition has also been shown to be an effective surface roughening strategy (She et al.,
2012; Z. Wang et al., 2012) leading to the desired micronanoscale hierarchical topog-
raphy. Wang et al. (2013) used a combination of selective chemical etching followed
by electroless zinc deposition for this purpose. The selective chemical etching resulted
in preferential etching of the magnesium-rich phase of the alloy, the a phase. Upon
exposure to the electroless zinc-plating solution, zinc deposited on both phases of
the alloy but preferentially on the Mg
, b phase, leading to a micronanoscale hi-
17Al12
erarchical topography.
In each of the articles discussed, the roughened surface is subsequently modified
with a hydrophobic molecule. The use of two classes of hydrophobic molecules has
been reported, including organosilanes and long- chain fatty acids. Modification with
organosilanes is by far the most widely used method. Organosilanes have the structure
(RO)
-Si-X, where R is a methoxy or ethoxy group and the nature of X depends on the
3
desired application. These molecules undergo a series of hydrolysis and condensation
reactions, resulting in the formation of covalent bonds between the organosilane molecules and magnesium surface hydroxyl groups. When the roughening procedure
Biomimetic surface modifications of magnesium and magnesium alloys for biomedical applications 293
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involves deposition of a surface layer that does not contain a significant number of surface hydroxyl groups, a catalyst is added to the coating bath to promote hydrolysis and
condensation (Ishizaki & Saito, 2010). In the case of superhydrophobic coatings, the X
group of the organosilane is typically a long-chain hydrocarbon or a long-chain hydrocarbon containing low surface energy eCF
- and -CF3- functional groups. Surface
2
modification with fluoroalkylsilanes has been shown to result in superhydrophobic
coatings that have long-term stability in air and high chemical stability in acidic, basic,
and salt solutions, as well as improved corrosion resistance compared to untreated
magnesium alloys (Ishizaki et al., 2011; Ishizaki & Saito, 2010; Liu et al., 2008;
Ou et al., 2013; Xu et al., 2011). Improved corrosion resistance has also been observ ed
with alkylsilane surface treatments (Ishizaki & Sakamoto, 2011; Liu et al., 2013;
Yin et al., 2010).
The long-chain fatty acids, stearic acid and lauric acid, have also been used to
impart hydrophobicity to the surface of magnesium alloys (She et al., 2012; Song
et al., 2013; Y. Wang et al., 2010; Z. Wang et al., 2012; Wang et al., 2013). When these
molecules are adsorbed to the magnesium alloy surface by a simple immersion process, an acid/base interaction is established between the magnesium hydroxide surface
and the carboxylic acid functional group of the molecule. The films produced by this
method are stable in air (Song et al., 2013; Y. Wang et al., 2010) but have been shown
to have poor corrosion resistance in sodium chloride solutions (Y. Wang et al., 2010).
However, the use of long- chain fatty acids is desirable due to their decreased cost and
increased environmental friendliness compared to organosilanes. Therefore, several
researchers have employed electrodeposition (Z. Wang et al., 2012; Wang et al.,
2013) or electrostatic adsorption (She et al., 2012) methods to improve the stability
of these hydrophobic coatings. The electrodeposition method has been shown to result
in the deposition of zinc stearate (Wang et al., 2013) and copper laurate (Z. Wang et al.,
2012) compounds on the magnesium alloy surface. In each case significantly improved
corrosion resistance was observed. However, it was reported that the copper laurate
films were unstable in basic solution.
Biomimetic superhydrophobic coatings mimic nature through a combination of
hierarchical topography at the micro and nanoscale coupled with the presence of hydrophobic molecules. These coatings have shown promise as a surfa ce modification
strategy for engineering surface treatments on magnesium alloys with optimum corrosion resistance.
10.4 Conclusions
In comparison to other materials, relatively little research has been done on biomimetic
surface modifications of magnesium and its alloys. As this field develops, the ability to
mimic nature through surface modifications that combine hierarchical topographies
with specific surface chemistries will provide us with biodegradable implants that
have controlled degradation rates. These biomimetically modi fied surfaces will also
be designed to elicit desired cell responses for implants that readily integrate into
the host tissue. Furthermore, the development of superhydrophobic coatings with
294 Surface Modification of Magnesium and its Alloys for Biomedical Applications
optimized corrosion resistance will lead to increased use of magnesium alloys in applications where high strength- to-weight ratios are advantageous.
Acknowledgements
I would like to acknowledge the contribution of Ms Katherine Bissonnette, Mr Sahejmeet
Guraya, and Mr Jean-Paul Rank, who collected some of the data presented from our research
groups. Your hard work and dedication to your projects is very much appreciated.
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Surface modification by natural
biopolymer coatings on
11
magnesium alloys for biomedical
applications
Z. Zhen, T.F. Xi, Y.F. Zheng
Peking University, Beijing, China
11.1 Introduction
As a lightweight metal, magnesium possesses mechanical properties similar to natural
bone. It is an essential element for human beings, with significant functional roles in
biological systems. In addition, it easily degrades via corrosion in the electrolytic environment of the body. Therefore, magnesium and its alloys show promise as biocompatible, osteoconductive, cardiovascular, and degradable implants for load-bearing
applications (Staiger, Pietak, Huadmai, & Dias, 2006). However, the high corrosion
rate and accumulation of hydrogen gas upon degradation hinder its clinical application.
Many surface modifications have been adopted to improve the biodegradation resistance of magnesium, such as ion implantation (Liu, Xin, Tian, & Chu, 2007a; Wan
et al., 2008; Wang, Zeng, Wu, Yao, & Lai, 2007; Wu, Zeng, Yao, & Han, 2007),
micro-arc oxidation (Gu et al., 2011; Zhang, Zhao, Wu, Wang, & Wu, 2007), and
hydrothermal treatment (Gu, Zheng, Cheng, & Zheng, 2009a; Tomozawa &
Hiromoto, 2011).
A great deal of polymers have been successfully adopted as surface coating modifications on magnesium alloys, including commonly used biodegradable synthetic
polymers such as polylactic-co-glycolic acid (PLGA) (Li, Cao, Zhang, Zhang, &
He, 2010), polycaprolactone (PCL) (Wong et al., 2010), and polylactic acid (PLA)
(Chen et al., 2011). Some natural biopolymers, such as chitosan (Gu et al., 2009b),
phytic acid (Ye, Zheng, Wang, Xi, & Li, 2012), and stearic acid (Ng, Wong, & Cheng,
2010) have been reported to be coated on the surface of magnesium alloys.
Natural biomaterial-based coatings are attractive for biomedical applications
because they offer protection against corrosion and other functions, such as drug
delivery and the ability to be functionalized with organic biomolecules (Hornberger,
Virtanen, & Boccaccini, 2012). Compared to synthetic polymers, natural biomaterials
exhibit excellent biocompatibility and bioactivity due to their extracellular cell
matrix (ECM) components, which contain cell-specific domains such as the RGD
(Arg-Gly-Asp) sequence (Tan & Marra, 2010). In addition, they are abundant in the
biomass and are easily accessible from a range of sources, such as forest products,
grasses, tunicates, crustacea, and stalks.
Surface Modification of Magnesium and its Alloys for Biomedical Applications. http://dx.doi.org/10.1016/B978-1-78242-078-1.00011-6
Copyright © 2015 Elsevier Ltd. All rights reserved.
302 Surface Modification of Magnesium and its Alloys for Biomedical Applications
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These natural materials have been shown to promote better healing at a faster rate
and are expected to exhibit greater compatibility with humans. However, new concepts
in implantable medical devices, especially tissue engineering derived from a combination of biomaterials, require temporal features that ensure the biomaterial biodegrades
into nontoxic byproducts (Khor & Lim, 2003).
In this chapter, we review the surface modification of magnesium alloys by natural
biopolymer coatings to improve the biocompatibility or corrosion properties of biodegradable magnesium and its alloys.
11.2 Phytic acid modification
11.2.1 Introduction to phytic acid
Phytic acid (myo-inositol hexaphosphoric acid C6H18O24P6) is a constituent of plants,
which is composed of 1e5% by weight of edible legumes, cereals, oil seeds, pollens,
and nut (Graf, Empson, & Eaton, 1987). Phytic acid (PA) has a strong ability to chelate
multivalent metal ions, especially zinc, calcium, and iron, and, to a lesser extent, magnesium (Cheryan & Rackis, 1980). Figure 11.1 shows the structure of PA. Studies
have shown its abilities to alter signal transduction, stimulate genes toward greater
cell differentiation, act as an antioxidant as a food additive, and demonstrate anticancer
properties (Ye et al., 2012).
11.2.2 Phytic acid coated on WE43 alloys
Ye et al. (2012) studied the in vitro corrosion and biocompatibility of PA-modified
WE43 alloys as biomaterials. The conversion coatings were prepared by immersing
the WE43 alloy into the phytic acid solutions with different pH values (pH 3, 5, 8
and 10) at 40
In different pH conditions, one phytic acid can chelate with different numbers of
magnesium ions using its 12 hydroxyl groups, resulting in different modification effects.
As shown in Figure 11.2, when the pH of the coating solution increased from 3 to 5,
8, and 10, the content of element P (at%) changed from 11.47% to 11.67%, 7.22%, and
OH
HO
O
O
HO
P
O
HO
Figure 11.1 Structure of phytic acid.
Adapted from Ye et al. (2012).
C, with untreated WE43 alloy samples as controls.
OH
HO
P
OO
OP
O
O
P
OHHO
OH
O
P
O
HO
O
O
P
OH
OH
R
RR
R
R
R ==OPOH
R
O
OH
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