Effects of porosity on corrosion resistance of Mg alloy foam produced by
powder metallurgy technology

E. Aghion, Y. Perez

PII: S1044-5803(14)00215-0
DOI: doi: 10.1016/j.matchar.2014.07.012
Reference: MTL 7636

To appear in: Materials Characterization

Received date: 25 April 2014

Revised date: 9 July 2014
Accepted date: 11 July 2014

Please cite this article as: Aghion E, Perez Y, Effects of porosity on corrosion resistance
of Mg alloy foam produced by powder metallurgy technology, Materials Characterization
(2014), doi: 10.1016/j.matchar.2014.07.012

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Effects of porosity on corrosion resistance of Mg alloy foam produced

by powder metallurgy technology

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E. Aghion and Y. Perez

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Department of Materials Engineering, Ben-Gurion University of the Negev,

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Beer-Sheva 84105, Israel
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Corresponding author:
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Prof. Eli Aghion

Department of Materials Engineering

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Ben-Gurion University of the Negev

P.O. Box 653, Beer-Sheva 84105, Israel

Tel: +972-8-647-7498

Fax: +972-8-647-7935

e-mail: egyon@bgu.ac.il

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Abstract

Magnesium alloy foams have the potential to serve as structural material for regular

light-weight applications as well as for biodegradable scaffold implants. However,

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their main disadvantage relates to the high reactivity of magnesium and consequently

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their natural tendency to corrode in regular service conditions and in physiological

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environments. The present study aims at evaluating the effect of porosity on the

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corrosion resistance of MRI 201S magnesium alloy foams in 0.9% NaCl solution and

in phosphate buffer saline solution as a simulated physiological electrolyte. The

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magnesium foams were produced by powder metallurgy technology using space-
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holding particles to control the porosity content. Machined chips were used as raw

material for the production of Mg alloy powder by milling process. The

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microstructure of the foams was examined using optical and scanning electron
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microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy analysis. The

corrosion behavior was evaluated by immersion test and potentiodynamic polarization

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analysis. The results obtained clearly demonstrate that the porosity has a significant
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effect on the corrosion resistance of the tested foams. Foams with 14-19% porosity
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have a corrosion rate of 4-10 mcd and 7-15 mcd in NaCl and phosphate buffer saline

solution, respectively, compared to only 0.10 mcd for the same alloy in as cast

conditions. This increased corrosion degradation of the Mg foams by more than one

order of magnitude compared to the cast alloy may limit their potential application in

regular and physiological environments.

Keywords: magnesium foam, powder metallurgy, porosity, corrosion

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1. Introduction

The attractiveness of Mg foams relates to their high specific strength, high energy

absorbing capacity, and significantly reduced weight [1-2]. Hence, Mg foams are

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considered as structural material for light-weight applications in the transportation

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industry including automotive, aerospace, and rail transport, as well as for household

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equipment. In addition, the excellent biocompatibility of Mg coupled with the fact

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that its mechanical properties are close to that of natural bone [3-4] makes Mg foams

an attractive structural material for biodegradable implants. For example, Mg foams

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are considered as a biomaterial scaffold for degradable orthopedic applications that
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eliminates the need for a second surgery to remove hardware [5-7].

Production technologies of Mg foams currently include a variety of methods [8]. Xia

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et al. [9] have fabricated closed-cell Mg alloy foam (AZ31) by melt foaming using Ca
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and CaCO3 as thickening and blowing agents, respectively. Staiger et al. [10]

introduced a method to prepare open-cell porous Mg with topological-ordered

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architecture. Their process is implemented in six steps: (i) creating a 3D model with a
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desired architecture using computer-aided design (CAD); (ii) 3D printing of a positive

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polymeric template of the CAD model; (iii) infiltration of the polymeric template with

NaCl paste; (iv) burn-out of polymeric materials and sintering of NaCl; (v) pressure-

assisted infiltration of the negative NaCl template with liquid Mg; and (vi) removal of

the NaCl template. Neu et al. [11] have produced Mg foams using Mg and Al

powders and TiH2 as a blowing agent. Wen et al. [12] produced Mg foams by powder

metallurgy using space holder particles. According to their process carbamide –

CO(NH2)2 – used as space holder particles was thoroughly mixed with pure Mg

powder and uniaxially compacted to green density. The green dense material was then

heat-treated to 773 K for 2 hr to obtain porous Mg specimens with 35-55% porosity

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and average pore size of 250 µm, as well as specimens with 45% porosity and average

pore sizes of 73, 168, 251, and 412 µm.

Comparing Mg foams with their natural competitors, Al-based foams, in terms of

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their inherent properties introduced some interesting findings. Dong-Hui et al. [13]

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reported that cellular Mg foams prepared by melt-foaming method exhibit superior

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specific strength. They also found that the specific energy absorption capacities of Mg

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foams retain comparable values with those of Al foams. This also agrees with the

understanding of Hao et al. [14] and Yang et al. [15] in relation to energy absorption

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properties. According to Hao et al., increasing the damping capacity of the cell wall
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materials should enhance the energy absorption capacity of the foams, and hence, Mg

foams can be advantageous over Al foam due to their superior damping properties.
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According to Yang et al. the pore uniformity and properties of Mg foams are superior
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to those of Al alloys. In terms of biocompatibility characteristics Mg foams are much

more attractive than Al foams. In fact, according to Gupta et al. [16] Al is a risk factor
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for Alzheimer's disease, and hence cannot be used as implant material. However, in
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spite of the relatively promising mechanical properties of Mg foams, concerns are

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being raised relating to their corrosion resistance due to the high reactivity of Mg [11,

14, 17]. Unfortunately, there is limited information on the corrosion resistance of Mg

foams and in particular information that relates to the effect of porosity on the

corrosion degradation.

The present study aims at evaluating the effects of porosity on the corrosion resistance

of MRI 201S Mg alloy foam produced by powder metallurgy route using space-

holding particles. The corrosion behavior of the tested foams was evaluated in two

different environments; (i) 0.9% NaCl solution saturated with Mg(OH)2 that

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represents regular corrosion conditions and (ii) PBS solution at 37°C, which

represents simulated physiological conditions of biodegradable implants.

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2. Experimental

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Foams with various amounts of porosity were produced from MRI 201S Mg alloy [18]

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by powder metallurgy technology using space-holding particles (spacer). Owing to the

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excellent machining characteristics of Mg, machined chips were used as raw material

for the production of Mg alloy powder. The machined chips were milled by blade

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milling apparatus D3V-10 for 10 hr using a milling velocity of 14,000 rpm in a
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stainless steel milling chamber. In order to eliminate the natural tendency of Mg

powder to oxidize during the milling process, high purity argon atmosphere was used
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as a protective gas in the milling chamber. In addition, the excessive heat produced
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during the milling process was removed by an external heat exchanger attached to the

milling chamber. The space-holding particles were made from Ammonium Hydrogen
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Carbonate salt (50-200 micron diameter) that can be evaporated at relatively low
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temperature of 150°C according to the following reaction [19].

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NH4HCO3 → NH3 + H2O +CO2.

Green density foams were produced by compressing a mixture of magnesium powder

with up to 10% spacer using a uniaxial CARVER 2702 pneumatic press with a

pressing force of up to 25 tons. The dimensions of the obtained specimens were 10

mm diameter and 3 mm length. The sintering process was carried out in a MIT-

GSL1300X vacuum furnace under a protective gas atmosphere after reaching a

vacuum of 10-5 torr. The space-holding particles were evacuated during the initial

sintering phase at a temperature of 150°C. The final sintering temperatures were

between 500°C and 640°C; the sintering time was constant and equal to 3.5 hr. The

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use of different sintering temperatures aims at controlling the porosity content of the

foams as an additional measure to the porosity control obtained by the space-holding

particles. The amount of porosity in the Mg foams was evaluated by the following

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equation after calculating the geometric volume and measuring their weight.

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% Porosity = (1-ρ/ρth) × 100

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where: ρ – foam density after sintering (ρ = M/V, where M = weight of sintered foam

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and V = volume calculated as V = πr2h), ρth – theoretical density equal to 1.81 gr/cm3.

The microstructure of the foams was examined by optical microscopy using a Nikon-

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Epiphot with computerized CCD camera and by Scanning Electron Microscopy
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(SEM) JEOL JSM-5600. Phase identification was obtained by X-ray diffraction

analysis using a RIGAKU-2100H X-ray diffractometer with CuKα, 40 KV/30 mA,

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and a scanning rate of 2º/min. The external surface characteristics were evaluated by
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an ESCALAB 250 X-ray photoelectron spectroscopy (XPS) equipped with an Ar-

sputtering depth profile EX05 ion gun with sputtering rate of 0.1 nm min-1.
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The corrosion performance was evaluated by immersion test and potentiodynamic

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polarization analysis. The immersion test was carried out according to ASTM G31-72
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standard in terms of hydrogen evolution that is indicative of the corrosion rate of Mg

[20]. The potentiodynamic polarization analysis was performed according to ASTM

G5-G94 standard using an SP-200 BioLogic three-electrode electrochemical cell

potentiostat and a scanning rate of 0.5 mv/sec. The reference electrode was a saturated

calomel electrode (SCE) and the counter electrode was platinum. The corrosion rate

(CR) in terms of [mcd] was determined by Tafel extrapolation according to the

following equation:

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where: icorr = corrosion density obtained by Tafel extrapolation in terms of µA, ρ –

density, EW – equivalent weight, k – constant equal to 3.27×10-3 mm gr/µA cm year.

All the corrosion tests were carried out in two different environments: 0.9% NaCl

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solution saturated with Mg(OH)2 and in phosphate buffer saline (PBS) solution at

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37°C. The use of NaCl solution aims at simulating the environmental conditions of

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regular Mg components while the use of PBS solution simulates the physiological

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electrolytic conditions of biodegradable magnesium implants. The use of saturated

Mg(OH)2 in 0.9% NaCl solution aims at eliminating the side effects of the corrosion

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products that are produced during the corrosion process [21,22].
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3. Results and Discussion
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3.1 Microstructure and porosity characteristics

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The characteristic morphology of MRI 201S magnesium alloy powder particles after

10 hr milling of machined chips is shown in Figure 1. The particles exhibit spherical

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shape with an average diameter of about 150 µm. It should be pointed out that
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increasing the milling time beyond 10 hr did not have any significant effect on the
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shape or average size of the obtained particles. In order to evaluate the extent of

oxidation at the external surface of the particles, after the milling process XPS depth

profiling measurements were carried out as shown in Figure 2. According to the

decrease in the oxygen profile after sputtering time of 200 sec the thickness of the

oxide layer was about 20 nm. This oxide layer was relatively thicker than the natural

oxide layer obtained on cast magnesium, which is about 6 nm [21].

The amount of porosity in Mg foams with and without spacer versus the sintering

temperature is shown in Table 1. This indicates that the degree of porosity was

reduced at higher sintering temperatures in both foams. In addition, foams with 10%

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spacer have a greater porosity level compared to foams without spacer, as expected.

The microstructure of Mg foams with and without spacer has revealed that the necking

phenomena in foams with 10% spacer were relatively reduced compared to the foams

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without spacer, as expected. The inter-particle necking characteristics that demonstrate

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adequate sintering process [23,24] were also evident by the fractography analysis as

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shown for foams without spacer (Figure 3a) and foams with 10% spacer (Figure 3b

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and c). XPS depth profiling measurements of sintered Mg foam with 10% spacer are

shown in Figure 4. This revealed an oxide layer with a thickness of about 20-25 nm

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according to the decrease in the oxygen profile line. Compared to the oxide layer
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obtained on the powder particles, it is clearly evident that the sintering process under

protective argon atmosphere did not have any significant contribution to the degree of
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oxidation. This was attributed to the effectiveness of Ar as a protective gas atmosphere

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at the sintering temperature. The XPS examination also included Mg2p high-resolution

XPS spectra analysis at different sputtering times as shown in Figure 5. The wide-
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ranging higher binding energy peak centered between 50.5 and 51.7 eV may
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correspond to the presence of magnesium oxide, while the lower binding peak
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centered at 49.6 eV is indicative of metallic Mg [21].

X-ray diffraction analysis of Mg alloy powder before and after sintering is shown in

Figure 6. This revealed that in both cases the matrix was made of α-Mg and both

powders included oxides of Nd and Y in the form of (Nd,Y)2O3. Combining the results

of the X-ray analysis and XPS examination it is believed that the external oxide layer

in both systems, Mg powder particles and Mg foam, was from a mixture of oxides:

MgO and (Nd,Y)2O3. In principle, the enrichment of the natural magnesium oxide film

with oxide of Rare Earth elements should have a beneficial effect on the corrosion

resistance [25].

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3.2 Corrosion behavior

The corrosion resistance of Mg alloy foams with and without spacing, in 0.9% NaCl

solution saturated with Mg(OH)2 and in PBS solution, in terms of immersion test are

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shown in Figure 7. In both cases the corrosion rate was measured by hydrogen

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evolution due the problematic disintegration characteristics of the foams that limit the

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ability to accurately evaluate their corrosion rate by weight loss. The results of the

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immersion tests clearly demonstrate that in both tested solutions the highest corrosion

rate levels were obtained in Mg foam with 10% spacer sintered at relatively lower

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temperature. Contrarily, the lowest corrosion rates were obtained with Mg foams
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without spacer that were sintered at relatively higher temperature. The range of

corrosion rate of Mg foams with and without spacer in 0.9% NaCl solution saturated

with Mg(OH)2 was 4-10 mcd (mg/cm2/day) compared to 7-15 mcd in PBS solution.
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The relatively reduced corrosiveness of the NaCl solution mainly relates to the

addition of saturated Mg(OH)2 that increased the pH and consequently created more
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passive conditions for magnesium corrosion. The results of the potentiodynamic

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polarization analysis in 0.9% NaCl solution saturated with Mg(OH)2 and in PBS
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solution are shown in Figures 8 and 9 and in Tables 2 and 3, respectively. Basically,

those results are in line with the results of the immersion tests, although the magnitude

of the corrosion rates of the various foams in 0.9% NaCl solution saturated with

Mg(OH)2 and in PBS solution was reduced to the range of about 1.5-4 and 3-6 mcd,

respectively.

3.3 Summary of results

Based on the above results it is quite clear that the corrosion resistance of MRI 201S

Mg alloy foams was significantly affected by their porosity content. Increasing the

porosity content of the tested foams by using reduced sintering temperatures or by

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adding spacer significantly reduces their corrosion resistance. The detrimental effect of

porosity on the corrosion resistance in 0.9% NaCl solution can be also demonstrated

by the fact that the corrosion rate of 201S Mg alloy in as cast condition is only 0.10

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mcd [18] compared to 4-10 mcd for Mg foams with about 14-19% porosity (Figure 7a

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and Table 1). This means that the porosity in the tested foams increased the corrosion

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rate of the as cast alloy by more than one order of magnitude, which may limit its

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ability to serve as an adequate structural material in regular atmospheric conditions

[26]. Relating to the effect of porosity on the corrosion resistance of Mg foams in

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simulated physiological electrolyte (PBS solution), the results of the present study are
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in good agreement with the results of Zhuang et al. [27] and Lietaert et al. [28].

According to Zhuang et al., degradation of the pure Mg foams in physiological

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solution occurs at a rate that is too rapid to allow sufficient time for healing as it is
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desirable to have the implant fixture present for at least 12 weeks. This conclusion was

also shared by Lietaert et al. who reported that the dissolution rate of 4 open cellular
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Mg alloys (AZ63, M2, ZM21, and MZX211) tested as biodegradable orthopedic

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implants was too high for direct use in the human body due to excessive hydrogen
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evolution and overly rapid degradation of mechanical properties. Hence it is believed

that practical applications of Mg alloy foams in regular conditions as well as in a

physiological environment may require the use of coating or other surface treatments

that can restrain the corrosion degradation of the foams.

Conclusion

The results of the present study clearly demonstrate the significant detrimental effect

of porosity on the corrosion resistance of MRI 201S Mg alloy foam. Porosity in the

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range of 14-19% can increase the corrosion rate of this alloy by more than one order of

magnitude compared to its corrosion rate in as cast conditions.

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8. Banhart J. Light-metal foams – History of innovation and technological

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Stein R, Shanmugavelu P, Jagannatha Rao KS. Aluminum in Alzheimer's

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Tables
Table 1: Porosity of Mg foams with and without spacer vs. sintering temperature.
Table 2: Corrosion rates calculated from potentiodynamic polarization curves in 0.9%
NaCl solution saturated with Mg(OH)2 using Tafel extrapolation.

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Table 3: Corrosion rates calculated by Tafel extrapolation from potentiodynamic

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polarization curves in PBS solution.

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Figure Legends

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Figure 1: Typical morphology of Mg powder particles obtained from chips milling (a)
×50, (b) ×200.

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Figure 2: XPS Sputtering depth profiles of Mg powder particles after milling.
Figure 3: Typical fractography of Mg foams after sintering at 640 C for 3 h (a),
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without spacer (b), and (c) with 10% spacer.
Figure 4: XPS Sputtering depth profiles of sintered Mg foam with 10% spacer.
Figure 5: XPS Mg2p-spectra obtained from sintered Mg foam with 10% spacer at
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different sputtering time.

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Figure 6: X-ray diffraction analysis of sintered Mg foam (top) and Mg powder after
milling (bottom).
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Figure 7: Corrosion rates of Mg foams produced at different sintering temperatures

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after immersion tests in (a) 0.9% NaCl solution saturated with Mg(OH)2, (b) PBS
solution.
Figure 8: Potentiodynamic polarization curves obtained in 0.9% NaCl solution
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saturated with Mg(OH)2 (a) Mg foam without spacer sintered at 640°C (b) Mg foams
with 10% spacer sintered at 570-640°C.
Figure 9: Potentiodynamic polarization curves obtained in PBS solution (a) Mg foam
without spacer sintered at 640°C (b) Mg foams with 10% spacer sintered at 570-
640°C.

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Sputtering
time [sec]

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0
1.0
60

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120
External surface
0.8
240

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360
540
0.6
Counts/s

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Internal region

0.4
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0.2

0.0
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54 53 52 51 50 49
Binding Energy [eV]
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Figure 5
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Table 1: Porosity of Mg foams with and without spacer vs. sintering temperature.
Mg foam Mg foam
without spacer with 10% spacer
Sintering 500 640 570 620 640
0
temp. ( C)

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Porosity 15.21±0.35 14.60±0.60 19.33±0.61 18.43±0.67 17.00±1.85

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(Vol. %)

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Table 2: Corrosion rates calculated from potentiodynamic polarization curves in
0.9% NaCl solution saturated with Mg(OH)2 using Tafel extrapolation.
Mg foam Mg foam

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without spacer with 10% spacer
Sintering 640 570 600 640
0
temp. ( C)
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Corrosion 1.55±0.07 3.89±0.25 3.29±0.30 1.69±0.14
rate (mcd)
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Table 3: Corrosion rates calculated by Tafel extrapolation from potentiodynamic

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polarization curves in PBS solution.

Mg foam Mg foam
without spacer with 10% spacer
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Sintering 640 570 600 640

temp. (0C)
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Corrosion 2.89±0.08 5.89±0.83 5.44±0.52 3.54±0.18

rate (mcd)
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Graphical abstract
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Highlights
 Porosity has a detrimental effect on corrosion resistance of MRI201S Mg foams.
 14-19% porosity increases the corrosion rate by more than one order of magnitude.
 Accelerated corrosion limits the use of foams in regular/physiological environments.

T
R IP
SC
NU
MA
D
P TE
CE
AC

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