CC BY
41
УДК 621.794, 621.793
Синтез, коррозия и биоактивность гибридного анодированного
покрытия из поликапролактона фумарата и фторапатита, легированного Si и Mg, на подложке из магниевого сплава AZ31
K. Mohemi1, T. Ahmadi1, A. Jafarzadeh1, H.R. Bakhsheshi-Rad2, M. Taghian Dehaghani3, and F. Berto4
1 Исламский университет Азад в Шeхреза, Шехреза, 86145-311, Иран 2 Исследовательский центр перспективных материалов, Исламский университет Азад в Наджафабаде, Наджафабад, Иран
3 Ширазский университет, Абаде, Иран 4 Норвежский университет естественных и технических наук, Тронхейм, 7491, Норвегия
В данной работе изготовлено двухслойное композитное покрытие на подложке из магниевого сплава AZ31. Покрытие состоит из внутреннего анодированного слоя и внешнего нанокомпозитного слоя из поликапролактона фумарата (ПКЛФ) и фторапатита (ФА), легированного кремнием и магнием (Si-Mg-ФА). Толщина нанокомпозитного ПКЛФ/Si-Mg-ФА покрытия составляет 9.72 мкм, при этом наночастицы Si-Mg-ФА равномерно распределены в матрице из ПКЛФ. Электрохимические измерения показали, что сплав AZ31 с анодированным П^Ф^-И^-ФА покрытием имеет низкую плотность тока коррозии (5.137 х 10-6 А/см2) и достаточную коррозионную стойкость (Rp = 5888.72 Ом см2). Испытания в искусственной биологической жидкости показали, что на сплаве AZ31 с анодированным ПКЛФ/Si-Mg-ФА покрытием образуется пористый апатит, обеспечивающий хорошую биоактивность. Полученное покрытие способствует адгезии клеток остеосаркомы. Модификация поверхности сплава AZ31 анодированным ПКЛФ/Si-Mg-ФА покрытием может быть подходящим методом контроля коррозионного разрушения, увеличения биоактивности и прикрепления клеток, что позволяет использовать сплав AZ31 в имплантологии.
Ключевые слова: анодирование, покрытие погружением, поликапролактона фумарат, фторапатит, сплав AZ31, биоактивность, коррозионная стойкость DOI 10.24412/1683-805X-2021-3-82-86
Synthesis, corrosion, and bioactivity evaluation of the hybrid anodized polycaprolactone fumarate/silicon- and magnesium-codoped fluorapatite nanocomposite coating on AZ31 magnesium alloy
K. Mohemi1,2, T. Ahmadi1,2, A. Jafarzadeh1,2, H.R. Bakhsheshi-Rad3, M. Taghian Dehaghani4, and F. Berto5
1 Department of Materials Engineering, Shahreza Branch, Islamic Azad University, Shahreza, 86145-311, Iran 2 Razi Chemistry Research Center (RCRC), Shahreza Branch, Islamic Azad University, Shahreza, Iran 3 Advanced Materials Research Center, Department of Materials Engineering, Najafabad Branch, Islamic Azad University, Najafabad, Iran 4 Shiraz University, Abadeh Center of High Education, Abadeh, Iran 5 Department of Mechanical and Industrial Engineering, Norwegian University of Science and Technology,
Trondheim, 7491, Norway
In the present study, a dual composite coating consisted of an anodized layer as the inner layer and PCLF (polycaprolactone fumarate)/silicon- and magnesium-codoped fluorapatite (Si-Mg-FA) nanocomposite as the outer layer was fabricated on AZ31 Mg alloy. The thickness of the PCLF/(Si-Mg-FA) nanocomposite coating is 9.72 (im, with the Si-Mg-FA nanoparticles being well distributed in the PCLF matrix. Electrochemical measurements showed that AZ31 Mg alloy with the anodized PCLF/Si-Mg-FA coating has a low corrosion current density (5.137 х 10-6 A/cm2), providing a sufficient protection (Rp = 5888.72 Q cm2) for Mg alloys. Immersion tests in a simulated body fluid showed that cauliflower-like/cloudy apatite forms on AZ31 Mg alloy with the anodized PCLF/Si-Mg-FA coating and governs good bioactivity. Osteosarcoma cells adhere well to the surface of the coating. Surface modification by the anodized PCLF/Si-Mg-FA coating can be a suitable method for controlling the corrosion degradation and increasing the bioactivity and cell attachment of AZ31 Mg alloy for implant applications.
Keywords: anodizing, dip coating, polycaprolactone fumarate, fluorapatite, AZ31 alloy, bioactivity, corrosion resistance
© Mohemi K., Ahmadi T., Jafarzade A., Bakhsheshi-Rad H.R., Taghian Dehaghani M., Berto F., 2021
1. Introduction
Magnesium, an essential element for bone metabolism, and its alloys are used for temporary fixing of bones due to degradability and specific mechanical features [1]. Low elastic modulus, high specific strength, and low density of these alloys are of special interest for biomedical application in bone replacement and orthopedic utilizations [1-3]. However, the undesirable property of Mg alloys is that they lose the mechanical integrity before bone healing and also the collection of hydrogen gas around the Mg implants [4, 5]. These crucial problems are due to the highly negative equilibrium potential, leading to a rapid corrosion rate [6]. Thus, many efforts have been made to improve corrosion resistance and slow down Mg alloys' biodegradation rate [7-9]. Surface modification or formation of a coating on the substrate as a solution to these problems can provide a layer to separate the substrate from contacting with corrosion mediums [10]. A bioactive surface can be achieved by using a bioactive coating.
Among different surface modification methods [11-18], micro-arc oxidation is also called microplasma oxidation, is one of the most efficient techniques to fabricate the corrosion protection layer on light metals such as magnesium and its alloy for biomedical applications [19-21]. During this technique, discharge occurs above the dielectric breakdown voltage, and a porous layer consisting of magnesium oxides (ceramic coating) can be in situ formed on the surface [22]. The coating produced by this technique can substantially improve some surface properties of the magnesium substrate, such as resistance to wear, corrosion resistance, and hardness [21]. Nevertheless, as ceramic coating fabricated by this method is usually porous and includes many microcracks, flaws, and defects, the enhanced corrosion resistance of this coating by itself may be insufficient [23-25]. Thus, subsequent coating as a post-treatment for improving corrosion resistance is suggested by researchers [26, 27]. On the other hand, this coating with a special porous structure can act as an intermediate layer to promote next coating adhesion by mechanical interlocking [28]. Dip coating technique possessing some interesting characteristics such as low-temperature processing, simple operation, and low cost can act as a sealing technique for Mg substrate [29, 30]. Polymeric biomaterial layer prepared by the dip-coating technique can increase the corrosion resistance of magnesium alloys substrate by creating a barrier between the metal and corrosion environment [31, 32]. It is worth mentioning that class 0(B), according to
ASTM D3359-09, has been categorized for the adhesion strength of a polymer on the Mg surface, indicating a low bonding strength on the substrate [33].
Polycaprolactone fumarate (PCLF), a synthetic polymer, is a promising material for tissue engineering applications because of its biodegradable, biocompatible, and good mechanical properties [34-36]. Nevertheless, there are some significant drawbacks related to this polymer, including fast degradation, poor cell response, and bioactivity, which makes it desirable to fabricate composite with the incorporation of some bioceramics into the polymer matrix [37-39]. Our previous investigation shows that nano-sized silicon and magnesium co-doped fluorapatite obtained by high energy ball milling possess higher cell response and bioactivity than nanosized fluorapatite [40, 41]. This work aimed to adjust corrosion rate and provide precipitation ability of apatite layer by using a dual composite coating consisting of ano-dized layer as an inner layer and PCLF/Si-Mg-FA nanocomposite as an outer layer on AZ31 Mg alloy. Furthermore, uncoated, anodized, nanocomposite-coated corrosion behavior and anodized-PCLF/Si-Mg-FA coated samples were compared with each other.
2. Materials and methods
2.1. Preparation of PCLF/Si-Mg-FA nanocomposite
Based on previously reported procedure [40], silicon and magnesium co-doped fluorapatite nanopow-der was synthesized by milling of a blend of silicon oxide (SiO2, Sigma-Aldrich), calcium fluoride (CaF2, Merck), magnesium hydroxide (Mg(OH)2, Merck), calcium hydroxide (Ca(OH)2, Merck) and phosphorous pentoxide (P2O5, Merck) in a high energy planetary ball mill (Fretch Pulverisette 5) for 12 h. The details of the experimental procedure are given in our previous study [40]. The obtained powder with Si and Mg co-doped fluorapatite was named Si-Mg-FA. Figure 1 shows the transmission electron microscopy (TEM, CM120, Philips) image of Si-Mg-FA nano-particles, indicating spherical shape morphology with a mean diameter of about 30 nm. In order to prepare PCLF/Si-Mg-FA nanocomposite, firstly, 0.05 g of synthesized Si-Mg-FA nanopowder was mixed with 10 mL of dichloromethane. Then, the slurry was magnetically stirred for 2 h to obtain a homogenous slurry. Finally, 0.5 g of polycaprolactone fumarate (PCLF, Mw = 10000) was added to the slurry, and stirring was further continued for 24 h.
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Received 09.03.2021, revised 18.05.2021, accepted 18.05.2021
This is an excerpt of the article "Synthesis, Corrosion, and Bioactivity Evaluation of the Hybrid Anodized Poly-caprolactone Fumarate/Silicon- and Magnesium-Codoped Fluorapatite Nanocomposite Coating on AZ31 Magnesium Alloy". Full text of the paper is published in Physical Mesomechanics Journal. DOI: 10.1134/ S1029959922010106
Сведения об авторах
Kamran Mohemi, Master's degree, Islamic Azad University, Iran, kamranmohemmi94@gmail.com
Tahmineh Ahmadi, Dr., Islamic Azad University, Iran, tahmadi56@yahoo.com, tahmineh.ahmadi@iaush.ac.ir
Aliakbar Jafarzade, Master's degree, Islamic Azad University, Iran, a.a.jafarzadeh.sh@gmail.com
Hamid Reza Bakhsheshi-Rad, Dr., Najafabad Branch, Islamic Azad University, Iran, rezabakhsheshi@gmail.com
Majid Taghian Dehaghani, PhD degree, Dr., Shiraz University, Iran, majid.taghian@yahoo.com
Filippo Berto, Prof., Norwegian University of Science and Technology, Norway, filippo.berto@ntnu.no
