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228 Surface Modification of Magnesium and its Alloys for Biomedical Applications
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Biocompatibility of surface-
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modified magnesium and
7
magnesium alloys
Ke Yang, Xiao Lin
Chinese Academy of Sciences, Shenyang, China
7.1 Introduction
Biocompatibility is a critical factor for successful applications of biom edical materials.
During the years between 1940 and 1980, biomaterials were thought to be bioinert.
Therefore, it was considered that biocompatibility would be achieved by designing
material to be extremely chemically stable. However, with the development of
biomaterials, it is gradually being recognized that it will be better that a biomaterial
can properly react with the surrounding tissues rather than being totally inert. More
recently, it has become widely accepted that, for some purposes, biomaterials that
can finally degrade in the physiological environment are better than those that exist
permanently. In 2008, David F. Williams proposed a concept of biocompatibility as
follows: Biocompatibility refers to the ability of a biomaterial to perform its desired
function with respect to a medical therapy, without eliciting any undesirable local or
systemic effects in the recipient or beneficiary of that therapy, but generating the
most appropriate beneficial cellular or tissue response in that specific situation, and
optimizing the clinically relevant performance of that therapy (Williams, 2008).
Magnesium (Mg)-based metals include pure Mg and Mg alloys. They are degradable in the body environment, which is an advantage compared with permanently
implanted metallic biomaterials. For surface-modified Mg-based metals, not only
the surface should generate “the most appropriate beneficial cellular or tissue
response,” but also the degradation products of the alloys and the surface modification
layers should not elicit “any undesirable local or systemic effects. ” In this chapter, we
will analyze the medical suitability of the materials introduced by the surface modifications on Mg-based metals. Then, we will introduce both the in vitro and in vivo
biocompatibility studies of surface-modified Mg-based metals and discuss the influencing factors on biocompatibility. Lastly, we will give a likely trend of the future
development of the biocompatible surface-modified Mg-based metals.
7.2 Biocompatibility of the materials introduced
by surface modification
Since the surface-modified Mg-based metals are biodegradable in the body environment, the alloying elements in the alloys and the materials introduced onto alloy
Surface Modification of Magnesium and its Alloys for Biomedical Applications. http://dx.doi.org/10.1016/B978-1-78242-077-4.00007-3
Copyright © 2015 Elsevier Ltd. All rights reserved.
232 Surface Modification of Magnesium and its Alloys for Biomedical Applications
surfaces by different surface modifications should be controlled to ensure that the
degradation products from the Mg implants will not elicit any undesirable local or
systemic effects. Information on the biocompatibility of alloying elements can be
found elsewhere (Habibovic & Barralet, 2011; Li & Zheng, 2013; Witte et al.,
2008). Here we give several recommended alloy elements from the biocompatibility
consideration in Table 7.1 . In this section, we mainly focus on the biocompatibility
of the materials introduced by surface modification on Mg-based metals. The
general properties of commonly adopted coati ng materials, which are introduced in
detail in the following sections, are listed in Table 7.2.
7.2.1 Calcium phosphates
Many works have studied calcium phosphate-containing coatings on the biodegradable Mg-based metals (Chang, Tian, Liu, & Duan, 2013; Niu et al., 2013; Shadanbaz
& Dias, 2012; Wang, Guan, Wang, Ren, & Wang, .; Wen et al., 2009). The main inor-
ganic component in bones is exactly a biological apatite (CaP). Thus, CaP has always
been considered to have an excellent biocompatibility, especially for the bone tissues.
There are many kinds of CaPs, including calcium phosphate dehydrate (DCP), octacalcium phosphate (OCP), tricalcium phosphate (TCP), and hydroxyapatite (HA). The
biocompatibilities of CaPs have been clearly revealed, and they are all biodegradable,
although they have different degradation rates (Shadanbaz & Dias, 2012). CaPs are
suggested as the coating materials on biodegradable Mg-based metals.
7.2.2 Magnesium phosphate
Magnesium phosphate-containing coatings are mainly fabricated by the substrateinvolving chemical reactions through either chemical conversion (Ishizaki,
Shigematsu, & Saito, 2009; Zhou, Shan, Han, & Ke, 2008) or microarc oxidation
(MAO) (Bai et al., 2012; Bala Srinivasan, Liang, Blawert, St Rmer, & Dietzel,
2009; Bala Srinivasan, Liang, Blawert, St Rmer, & Dietzel, 2010; Gao, Yerokhin,
& Matthews, 2013; Lin et al., 2014) methods. Recently, magnesium phosphate cement
(MPC) has attracted much attention as a potential biodegradable bone-implant material
(Mestres & Ginebra, 2011; Waselau, Samii, Weisbrode, Litsky, & Bertone, 2007;
Wu et al., 2008; Yu et al., 2010). The in vitro and in vivo studies showed that MPC
has excellent biocompatibility. It is believed that magnesium phosphate can be transformed into CaP in vivo, which has higher chemical stability.
7.2.3 Magnesium silicate
Magnesium silicate-containing coatings on the biodegradable Mg-based metals have
been fabricated through anodization (Wu et al., 2007; Xue, Yun, Schulz, & Shanov,
2011) or MAO (Gu et al., 2011; Lin, Tan, Zhang et al., 2013; Wan et al., 2013; Yao,
Li, & Jiang, 2009) methods. Magnesium silicate was mainly in the form of Mg
which has been widely studied as a biodegradable material for the scaffold in bonetissue engineering and/or load-bearing devices due to its biodegradability and good
SiO4,
2
Biocompatibility of surface-modified magnesium and magnesium alloys 233
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Table 7.1 Recommended alloy elements for biodegradable
magnesium alloy
Elements Biofunctionality References
Calcium Major component in human bone;
essential in chemical signaling
with cells; elevated calcium has
a number of stimulating effects
on osteoblasts
Zinc Plays an important role in various
physiological processes; one of
the constituents of the
antioxidant system; involved in
the synthesis of a large number
of proteins and is required for
their stability; important to the
bone tissues health
Silicon An essential trace element in the
skeletal development;
associated with calcium in an
early stage of calcification;
induce proliferation of
osteoblast-like cells and
angiogenesis during bone
regeneration
Strontium About 98% in the human body is
in the skeleton; strontium
renalate is used clinically in the
treatment of osteoporotic
patients in Europe; positive
effects on ostegenic
differentiation and mineral
formation; inhibitory effects on
osteoclastic differentiation and
resorption; dose-dependent
effect
Copper Osteoporosis associates with
copper deficiency, while a
supplement of copper may
have a potential therapeutic
application in the treatment and
prevention of involutional
osteoporosis; essential for
blood vessel formation
(Adams, Mansfield, Perlot, &
Shapiro, 2001; Dvorak et al.,
2004; Ilich & Kerstetter, 2000)
(Prasad, Bao, Beck, Kucuk, &
Sarkar, 2004; Tapiero & Tew,
2003; Yamaguchi, Oishi, &
Suketa, 1988)
(Carlisle, 1970; Carlisle, 1982;
Shie, Ding, Chang et al., 2011;
Zhai et al., 2012)
(Bonnelye, Chabadel, Saltel, &
Jurdic, 2008; Grynpas &
Marie, 1990; Marie, Ammann,
Boivin, & Rey, 2001;
Skoryna, 1984)
(Rico et al., 2000; Yee, Kubena,
Walker, Champney, &
Sampson, 1995; De Lima
et al., 2008)
234 Surface Modification of Magnesium and its Alloys for Biomedical Applications
Table 7.2 Biocompatibility and biodegradability of coating materials
on biodegradable magnesium alloy
Materials Biocompatibility Biodegradability
Calcium phosphates Excellent biocompatibility Degradable; degradation
rate varies significantly
between different
calcium phosphates
Magnesium phosphate Biocompatible Degradable
Magnesium silicate Biocompatible Degradable; degradation
rate is very low
Magnesium fluoride Dose-dependent
biocompatibility
Titania Questionable; depend on its
size and existing state
Alumina Biocompatible Not degradable
Degradable polymers Biocompatible Degradable; degradation
Degradable
Not degradable
products may elicit
slight inflammatory
reaction
biocompatibility (Kharaziha & Fathi, 2009; Kharaziha & Fathi, 2010; Ni & Chang,
2009; Ni, Chou, & Chang, 2007). It has been reported that silicon (Si) is an essential trace
element in skeletal development (Carlisle, 1982; Jugdaohsingh et al., 2004; Yamada
et al., 2003). It was also found that an appropriate Si concentration was effective in
supporting the proliferation of osteoblast-like cells (Shie et al., 2011). Thus, magnesium
silicate is a biocompatible coating material. However, it should be noted that its degradation rate is very low (Ni & Chang, 2009; Tavangarian & Emadi, 2011).
7.2.4 Magnesium fluoride
Magnesium fluoride (MgF2)-containing coatings were prepared on biodegradable
Mg-based metals through hydrofluoric acid-involving chemical conversion (Chiu,
Wong, Cheng, & Man, 2007; Lin, Tan, Wan et al., 2013; Pereda et al., 2010; Thomann
et al., 2010; Yan et al., 2010) or MAO (Pan, Chen, Wang, & Lin, 2013; Pan, Chen,
Wang, & Zhao, 2013; Seyfoori, Mirdamadi, Khavandi, & Raufi, 2012) methods.
Fluorine (F) is a natural component in human bones and teeth (Zheng, Wu, Ng,
Wang, & Lian, 2002). A proper release of F will not cause harm to the organisms
(Thomann et al., 2010). The bone response to fluoride is dose-dependent: a low-dose
release of F will facilitate the bone formation; however, a high dose of it will cause
the formation of poorly mineralized osteoid (Ellingsen, 1995). Thus, MgF
able coating material, although the degradation rate should be controlled.
is an accept-
2
Biocompatibility of surface-modified magnesium and magnesium alloys 235
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7.2.5 Titania
Some researchers fabricated titania-containing coatings on biodegradable Mg-based
metals through one of the methods of solegel (Hu et al., 2011; Li, Chen, Zhang,
Hu, & Su, 2010), direct current reactive magnetron sputtering (Chen et al., 2011),
and ion implantation (Liu, Xin, Tian, & Chu, 2007; Zhao et al., 2013). The titania coatings have been prepared on the permanently implanted metallic materials, showing
excellent biocompatibility and bioactivity (Chen et al., 2004; Huang et al., 2003;
Jokinen et al., 1998). A porous titania ceramic has been studied as a bone graft substi-
tute, which demonstrated excellent biocompatibility (Sabetrasekh, Tiainen,
Lyngstadaas, Reseland, & Haugen, 2011). However, titania is an inert and poorly
soluble material (Wang et al., 2007). The use of titania as coating material on
biodegradable Mg-based metals is controversial. In addition, the titania particles
from the coating might elicit some undesirable local or systemic effect s (Wang
et al., 2007).
7.2.6 Alumina
Alumina-containing coatings have been prepared on biodegradable Mg-based metals
through plasma immersion ion implantation (Liu et al., 2007; Wong et al., 2013; Zhao,
Wu, Pan, Yeung, & Chu, 2012)orfiltered cathodic arc deposition (Xin et al., 2008)
methods. Alumina is frequently used for medical implants and prostheses because
of its excellent biocompatibility (Fischer et al., 2005; Thomas, Barnstorf, Summer,
Willmann, & Przybilla, 2003). However, alumina is a bioinert ceramic with high
chemical stability, and its degradability could be a concern when applied on biodegradable Mg-based metals.
7.2.7 Organic materials
Many researchers have fabricated organic materials containing coatings on biodegradable Mg-based metals (Abdal-hay, Dewidar, & Lim, 2012; Abdal-hay, Amna, & Lim,
2013a; Abdal-hay, Barakat, & Lim, 2013b; Abdal-hay, Barakat, & Lim, 2013c;
Alabbasi, Liyanaarachchi, & Kannan, 2012; Bai et al., 2012; Cui, Beniash, Gawalt,
Xu, & Sfeir, 2013; Degner, Singer, Cordero, Boccaccini, & Virtanen, 2013; Fekry,
Ghoneim, & Ameer, 2014; Gray-Munro, Seguin, & Strong, 2009; Killian, Wagener,
Schmuki, & Virtanen, 2010; Ko, Choe, Jung, & Kim, 2013; Kunjukunju et al.,
2013; Li, Cao, Zhang, Zhang, & He, 2010b; Liu et al., 2013; Oosterbeek, Seal, Seitz, &
Hyland, 2013; Ostrowski et al., 2013; Shanshan, Lili, Yingxue, Bingchun, & Ke,
2013; Srinivasan, Ranjani, & Rajendran, 2013; Wagener, Killian, Turhan, & Virtanen,
2013; Wang, Zhao, Chen, Li, & Zhang, 2012; Wang et al., 2013; Wong et al., 2010;
Xu & Yamamoto, 2012; Xue et al., 2012; Zomorodian et al., 2013). The coating
materials include the well-known biodegradable polymers, such as poly(
acid) (PLA) (Abdal-hay et al., 2013c; Alabbasi et al., 2012; Gray-Munro et al.,
2009; Xu & Yamamoto, 2012), poly (lactide-co-glycolide) (PLGA) (Li, Cao
et al., 2010; Shanshan et al., 2013), poly (e-caprolactone) (PCL) (Degner et al.,
L-lactic
236 Surface Modification of Magnesium and its Alloys for Biomedical Applications
2013; Wang et al., 2012; Wong et al., 2010), polyether imide (PEI) (Zomorodian
et al., 2013), poly(1,3-trimethylene carbonate) (PTMC) (Wang et al., 2013), and
silane (Ko et al., 2013; Liu et al., 2013; Xue et al., 2012). Protein (Killian et al.,
2010; Wagener et al., 2013) and peptide (Cui et al., 2013) were also used as the
coating materials. The biocompatibility of the above materials has been well
addressed (Francis Suh & Matthew, 2000; Gunatillake & Adhikari, 2003; Mohanty,
Misra, & Hinrichsen, 2000; Rezwan, Chen, Blaker, & Boccaccini, 2006). However,
the degradation of some polymers usually produces a high quantity of acidic degradation products in a short time, which may induce a slight inflammatory response
(Bostman & Pihlajamaki, 2000; Taylor, Daniels, Andriano, & Heller, 1994).
7.3 Biocompatibility of surface-modified
magnesium-based metals e in vitro results
Various surface modifications have been applied to Mg-based metals to control their
degradation rates. The coatings can be divided into three classes according to
their compositions: inorganic coatings, organic coatings, and inorg anic/organic composite coatings. In this section, in vitro biocompatibility studies of these three classes
of coatings are introduced.
7.3.1 Inorganic coating
A number of methods have been used to modify the surfaces of biodegradable Mgbased metals by forming inorganic coatings, as illustrated in Figure 7.1. The coating
mechanisms and formed coating materials are summarized in Table 7.3. Although
the compositions of coatings prepared by the same method could vary from each other,
their physicochemical properties were similar. To a great extent, the surface biocompatibility of the surface-modified Mg-based metals should depend on the physicochemical properties of the surface layers. Thus in the following part, in vitro
biocompatibility of the inorganic coatings is introduced according to the modification
methods.
Methods for fabricating inorganic coatings
Alkaline
treatment
Heat
treatment
Biomimetic
treatment
Hydrofluoric acid
treatment
Acid
treatment
Cathodic
electrodeposition
Phytic acid
treatment
Constant
current mode
Micro-arc
oxidation
voltage mode
Anodization
Constant
Figure 7.1 Main inorganic coating methods for biodegradable magnesium alloy. Sometimes
more than one method is used to fabricate inorganiceinorganic composite coatings.
Ion
implantation
Biocompatibility of surface-modified magnesium and magnesium alloys 237
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Table 7.3 Coating mechanisms and formed coating materials of
several inorganic coating methods for biodegradable magnesium
alloy
Method Coating mechanism Coating materials
Alkaline treatment Substrate-involved
chemical reaction
Biomimetic treatment Substrate-involved
chemical reaction; pH
variation-induced
chemical deposition
Acid treatment Substrate-involved
chemical reaction
Cathodic electrodeposition Chemical reaction;
electrochemical reaction;
pH variation-induced
chemical deposition
Micro-arc oxidation Substrate-involved
chemical reaction;
electrochemical reaction
MgO; Mg(OH)
MgO; calcium phosphates;
magnesium phosphates
Phytic-Mg phytate
complex; MgF
Mg(OH)
Calcium phosphates,
especially HA; bioactive
element doped calcium
phosphates
MgO, calcium phosphates;
magnesium phosphates;
CaO, MgF
silicates
2
; MgO;
2
2
, magnesium
2
7.3.1.1 Alkaline treatment
In this treatment, Mg-based metals were immersed in an alkaline solution. A coating
will be formed through a chemical reaction. A heat treatment is always followed to
densify the coating. Gu et al. (Gu, Zheng, Cheng, & Zheng, 2009) soaked a
Mg1.4 wt% Ca alloy in three different alkaline solutions (Na
NaHCO
) for 24 h and subsequently annealed the alloy at 773 K for 12 h. Magnesium
3
oxide layers were formed on the surface of the Mg-Ca alloy after different alkaline
treatments. All the heat-treated Mg alloy samples showed no cell toxicity to L929 cells
during 7 d of co-culture. Lorenz et al. (Lorenz et al., 2009) passivated a pure Mg
(99.9% purity) by soaking it in 1 M NaOH for 24 h. The formed passive film, which
was mainly composed of MgO/Mg(OH)
, was in the order of nanometers in size. The
2
initial dissolution rate of the pure Mg in the cell culture medium was decreased by
approximately a factor of 20 due to the passivation. The human HeLa cell density
on the treated sample was significantly higher than the polished one, where only single
isolated cells could be found and the cell spreading was poor. For the passivated
sample, however, strong formation of the actin cytoskeleton could be observed, and
the cells were well spread, covering most of the surface.
HPO4,Na2CO3, and
2
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