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A self-healing and bioactive coating based on duplex Plasma electrolytic oxidation/polydopamine on AZ91 alloy for bone implants

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Journal of Magnesium and Alloys 2023年第2期11卷 592-606页

作者： Safoora Farshid Mahshid Kharaziha Masoud Atapour Department of Materials Engineering Isfahan University of TechnologyIsfahan84156-83111Iran

Magnesium(Mg) alloys are well-known in biomedical materials owing to their elastic module near to bone, biocompatibility and biodegradation properties. Nevertheless, poor corrosion resistance hinders their biomedical applications. Besides, it is necessary to endow Mg alloys with bioactive property, which is crucial for temporary bone implants. Here, a self-healing, corrosion resistant and bioactive duplex coating of plasma electrolytic oxidization(PEO)/polydopamine(PDA) is applied on AZ91 substrate using PEO and subsequent electrodeposition process. Moreover, the role of different electrodeposition times(60 s, 120 s) and dopamine concentrations(1 and 1.5 mg/ml) to improve corrosion resistance, bioactivity, biocompatibility and self-healing property and its mechanism are investigated. The results indicate that the PEO coating is efficiently sealed by the PDA, depending on the electrodeposition parameters. Noticeably, electrodeposition for 120 s in dopamine concentration of 1 mg/ml(120T-1C) results in the formation of uniform and crack-free PDA coating. Duplex PEO/PDA coatings reveal high bioactivity compared to PEO coating, owing to electrostatic interaction between PDA top-layer and calcium and phosphate ions as well as high hydrophilicity of coatings. In addition, duplex PEO/PDA coatings also show improved and more stable protective performance than the PEO and bare alloy, depending on the PDA deposition parameters. Noticeably, the corrosion current density of the 120T-1C decreases one orders of magnitude compared to PEO. In addition, the presence of a broad passivation region in the anodic polarization branch shows durable self-healing property via Zipper-like mechanism, demonstrating the duplex coating could preserve promising corrosion resistance.Furthermore, the cytocompatibility of duplex coated samples is also confirmed via interaction with MG63 cells. In summary, the PEO/PDA coating with great corrosion protection, self-healing ability, bioactivity and biocompatibility could be a promising candidate for d

关键词： Magnesium alloy Plasma electrolytic oxidation Polydopamine Self-healing Bioactivity Orthopedic applications

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Electrochemical response of MgO/Co_(3)O_(4) oxide layers produced by Plasma electrolytic oxidation and post treatment using cobalt nitrate

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Journal of Magnesium and Alloys 2023年第3期11卷 1057-1073页

作者： Mosab Kaseem Tehseen Zehra Tassawar Hussain Young Gun Ko Arash Fattah-alhosseini Department of Nanotechnology and Advanced Materials Engineering Sejong UniversitySeoul 05006Republic of Korea Materials Electrochemistry Group School of Materials Science and EngineeringYeungnam UniversityGyeongsan 38541Republic of Korea Department of Materials Engineering Bu-Ali Sina UniversityHamedan 65178-38695Iran

This work looked into the influence of the sealing treatment on the structural feature and electrochemical response of AZ31 Mg alloy coated via Plasma electrolytic oxidation(PEO).Here,the inorganic layers produced by PEO in an alkaline-phosphate electrolyte were subsequently immersed for different periods in cold(60°C)and hot(100°C)aqueous solutions containing either 1 or 3 gr of cobalt nitrate hexahydrate in the presence of hydrogen peroxide as an initiator.The results showed that the sealing treatments in the hot solutions could trigger the hydration reactions of PEO coating which would largely assist the surface incorporation of Co_(3)O_(4)into the coating.In contrast,the sealing in cold solutions led to less compact coatings,which was attributed to the fact the hydration reactions would be restricted at 60°C.A nearly fully sealed coating with a porosity of~0.5%was successfully formed on the sample immersed in the hot solution containing 1 gr of cobalt nitrate hexahydrate.Thus,the electrochemical stability of this fully sealed coating was superior to the other samples as it had the lowest corrosion current density(4.71×10^(-10)A·cm^(-2))and the highest outer layer resistance(3.81×10^(7)Ω·cm^(2)).The composite coatings developed in this study are ideal for applications requiring high electrochemical stability.

关键词： AZ31 Mg alloy Plasma electrolytic oxidation Co_(3)O_(4) Hydration Corrosion

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Incorporation of LDH nanocontainers into Plasma electrolytic oxidation coatings on Mg alloy

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Journal of Magnesium and Alloys 2023年第4期11卷 1236-1246页

作者： Yan Li Xiaopeng Lu Maria Serdechnova Carsten Blawert Mikhail L.Zheludkevich Kun Qian Tao Zhang Fuhui Wang Shenyang National Laboratory for Materials Science Northeastern University3-11 Wenhua RoadShenyang 110819China Institute of Surface Science Helmholtz-Zentrum HereonGeesthacht 21502Germany Institute of Materials Research Faculty of EngineeringUniversity of KielKaiserstraβe 2Kiel 24143Germany School of Materials Science and Engineering Southeastern UniversityNanjing 211189China

In-situ incorporation of layered double hydroxides(LDH)nanocontainers into Plasma electrolytic oxidation(PEO)coatings on AZ91 Mg alloy has been achieved in the present study.Fumarate was selected as Mg corrosion inhibitor for exchange and intercalation into the nanocontainers,which were subsequently incorporated into the coating.It was found that the thickness and compactness of the coatings were increased in the presence of LDH nanocontainers.The corrosion protection performance of the blank PEO,LDH containing PEO and inhibitor loaded coatings was evaluated by means of polarization test and electrochemical impedance spectroscopy(EIS).The degradation process and corrosion resistance of PEO coating were found to be greatly affected by the loaded inhibitor and nanocontainers by means of ion-exchange when corrosion occurs,leading to enhanced and stable corrosion resistance of the substrate.

关键词： Magnesium Layered double hydroxides Inhibitor Plasma electrolytic oxidation Nanocontainer

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Effect of carbonate additive on the microstructure and corrosion resistance of Plasma electrolytic oxidation coating on Mg-9Li-3Al alloy

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International Journal of Minerals,Metallurgy and Materials 2022年第7期29卷 1453-1463页

作者： Siyuan Jin Xiaochun Ma Ruizhi Wu Tingqu Li Jiaxiu Wang Boris L Krit Legan Hou Jinghuai Zhang Guixiang Wang Key Laboratory of Superlight Materials&Surface Technology Ministry of EducationHarbin Engineering UniversityHarbin 150001China College of Materials Science and Engineering Jilin Institute of Chemical TechnologyJilin 132022China College of Science Heihe UniversityHeihe 164300China Moscow Aviation Institute National Research UniversityMoscow 125993Russia

Carbonate was added to the silicate system electrolyte to improve the corrosion resistance of the Plasma electrolytic oxidation coating on Mg-9Li-3Al(wt%,LA93)alloy.The influences of carbonate on the morphology,structure,and phase composition of the coating were investigated by scanning electron microscopy,energy dispersive spectrometry,X-ray diffraction,and X-ray photoelectron spectroscopy.The corrosion resistance of the coating was evaluated by electrochemical experiment,hydrogen evolution,and immersion test.The results showed that the addition of carbonate resulted in a denser coating with increased hardness,and the corrosion-resistant Li_(2)CO_(3) phase was formed.Electrochemical experiments showed that compared with the coating without carbonate,the corrosion potential of the carbonate coating positively shifted(24 mV),and the corrosion current density was reduced by approximately an order of magnitude.The coating with carbonate addition possessed a high corrosion resistance and long-term protection capability.

关键词： Mg-Li alloy Plasma electrolytic oxidation corrosion resistance carbonate

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Effect of Initial Oxide Film on the Formation and Performance of Plasma electrolytic oxidation Coating on 7075 Aluminum Alloy

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Acta Metallurgica Sinica(English Letters) 2022年第9期35卷 1559-1571页

作者： Mingyu Zhu Yingwei Song Kaihui Dong Dayong Shan En-Hou Han Key Laboratory of Nuclear Materials and Safety Assessment Institute of Metal ResearchChinese Academy of SciencesShenyang110016China School of Materials Science and Engineering University of Science and Technology of ChinaHefei230026China

In the early stage of Plasma electrolytic oxidation(PEO),the quick formation of the initial oxide film on the surface of the aluminum substrate is necessary for the subsequent discharge spark process.Furthermore,the compactness of the initial oxide film greatly affects the quality of the PEO coating,but the related mechanisms are not investigated in detail.In this paper,the status of the initial oxide film was adjusted by adding the(NaPO)into the based electrolyte,and then the effect of initial oxide film on the formation of the PEO coating was compared.Microstructure and chemical composition were analyzed by scanning electron microscope,transmission electron microscopy and X-ray photoelectron spectrometer.The compactness of the initial oxide film was characterized by Mott-Schottky plots.The corrosion resistance was measured by electrochemical impedance spectroscopy.The results show that the addition of(NaPO)can promote the co-deposition of phosphide compound into the initial oxide film and improve the film compactness,which is beneficial for the more uniform spark discharge in the later stage.As a result,the addition of(NaPO)is helpful to obtain PEO coating with better performance.

关键词： Aluminum alloys Plasma electrolytic oxidation Initial oxide film Growth process Spark discharge Compactness

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Nucleation and growth behavior of coating film on Mg–Al–Zn alloy with different surface topographies via Plasma electrolytic oxidation

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Journal of Magnesium and Alloys 2022年第8期10卷 2185-2192页

作者： Nisa Nashrah Sung Hun Baek Young Gun Ko Materials Electrochemistry Group School of Materials Science and EngineeringYeungnam UniversityGyeongsan 38541Republic of Korea

This work was made to investigate how nucleation and growth behavior of the coating film were affected by surface topographies of Mg–Al–Zn alloy substrate during the initial stage of Plasma electrolytic oxidation(PEO).To satisfy this end,a single substrate was prepared by mechanical treatment exhibiting rough and smooth regions with an equal area on the surface.The rough region with prominent hills and grooves induced the breakdown of passive film,which was indicated by an early appearance of plasma discharge on the rough region since nucleation of coating film occurred preferentially around the hills.However,the coating film grown on the grooves was somewhat thicker and more porous than the film grown on the hills and smooth regions.This was due to the fact that the growth of the coating film was found to be localized in the presence of rough region,which was in line with the discharge activities.Herein,the nucleation and growth behavior during the initial stage of PEO will be discussed schematically on the basis of microstructural interpretation.

关键词： Mg alloy Surface roughness Plasma electrolytic oxidation Coating film

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Development of anti-corrosive coating on AZ31 Mg alloy subjected to Plasma electrolytic oxidation at sub-zero temperature

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Journal of Magnesium and Alloys 2022年第7期10卷 1915-1929页

作者： S.Fatimah M.P.Kamil D.I.Han W.Al-Zoubi Y.G.Ko Materials Electrochemistry Group School of Materials Science and EngineeringYeungnam UniversityGyeongsan 38541Republic of Korea

Plasma electrolytic oxidation(PEO)is a promising surface treatment to generate adherent and thick anti-corrosive coating on light-weight metals(Al,Mg,Ti,etc.)using an eco-friendly alkaline electrolyte.High energy plasma,however,inevitably generates porous structures that limit their practical performance.The present study proposes a straight-forward simple method by utilizing sub-zero electrolyte(268 K)to alter the plasma characteristics during formation of the protective coating on AZ31 Mg alloy via PEO with a comparison to the electrolyte at room temperature(298 K).In refrigerated electrolyte,the formation of micro-defects is suppressed relatively at the expense of low coating growth,which is measured to be twice lower than that at 298 K due to the temperature-dependent soft plasma discharges contributing to the development of the present coating.As a consequence,corrosion resistance of the sample processed at 268 K is superior to that of 298K,implying that the effect of coating thickness is less dominant than that of compactness.This phenomenon is interpreted in relation to the ionic movement and oxide solidification controlled by soft plasma discharges arising from the temperature gradient between electrolyte and surface of the substrate during PEO.

关键词： AZ31 Mg alloy Plasma electrolytic oxidation Sub-zero electrolyte Anti-corrosive coating Corrosion

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Corrosion and wear resistance of coatings produced on AZ31 Mg alloy by Plasma electrolytic oxidation in silicate-based K2TiF6 containing solution:Effect of waveform

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Journal of Magnesium and Alloys 2022年第9期10卷 2574-2587页

作者： Maryam Rahmati Keyvan Raeissi Mohammad Reza Toroghinejad Amin Hakimizad Monica Santamaria Department of Materials Engineering Isfahan University of TechnologyIsfahan 84156-83111Iran Yekta Mobaddel Pars Co. Science and Technology CampusYazd UniversityYazd 89158-18411Iran Dipartimento di Ingegneria Università di PalermoViale Delle ScienzeEd.690128PalermoItaly

In this research,Plasma electrolytic oxidation coatings were prepared on AZ31 Mg alloy in a silicate-based solution containing K_(2)TiF_(6) using bipolar and soft sparking waveforms with 10,20,and 30%cathodic duty cycles.The coatings displayed a net-like surface morphology consisted of irregular micro-pores,micro-cracks,fused oxide particles,and a sintered structure.Due to the incorporation of TiO_(2) colloidal particles and the cathodic pulse repair effect,most of the micro-pores were sealed.Long-term corrosion performance of the coatings was investigated using electrochemical impedance spectroscopy during immersion in 3.5 wt.%NaCl solution up to 14 days.The coating grown by the soft sparking waveform with a 20%cathodic duty cycle having the lowest porosity(6.2%)and a sharp layer concentrated in F element at the substrate/coating interface shows the highest corrosion resistance.The friction coefficient of this coating has remained stable during the sliding even under 5 N normal load,showing relatively higher wear resistance than other coatings.The coating produced using the equivalent unipolar waveform,as the reference specimen,showed the highest friction coefficient and the lowest wear resistance despite its highest micro-hardness.

关键词： Plasma electrolytic oxidation Pulsed waveforms AZ31 Mg alloy Dipotassium titanium hexafluoride Corrosion resistance Wear resistance

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Difference in formation of Plasma electrolytic oxidation coatings on MgLi alloy in comparison with pure Mg

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Journal of Magnesium and Alloys 2021年第5期9卷 1745-1760页

作者： Ting Wu Carsten Blawert Xiaopeng Lu Maria Serdechnova Mikhail L.Zheludkevich Institute of Surface Science Helmholtz-Zentrum Hereon21502 GeesthachtGermany Shenyang National Laboratory for Materials Science Northeastern University110819 ShenyangChina Institute for Materials Science Faculty of EngineeringKiel UniversityKaiserstrasse 224143 KielGermany

In order to study the substrate lattice structure(Li addition)on the growth of Plasma electrolytic oxidation(PEO)coatings,Mg Li alloy(11.36 wt.%of Li,cubic)and pure Mg(hexagonal)were treated under a pulsed direct PEO mode in a phosphate electrolyte for different periods of time.The results revealed that the presence of Li and Li-rich phases in the cubic Mg alloy seems to be essential for the treatment result rather than the original lattice structure.A modified discharge behavior of Mg Li alloy finally led to a different microstructure of the coating.The unstable coatings of Mg Li alloy tended to dissolve rapidly though shared the similar composition to that of pure Mg.Li was incorporated only in the primary conversion products at the interface of coating/Mg Li.In spite of the advanced efficiency of energy input during processing,the more porous and thinner PEO coatings on the Mg Li alloy were less resistant to abrasion and corrosion.

关键词： Plasma electrolytic oxidation Magnesium lithium alloy Pure magnesium Microstructure

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Characteristics of a multi-component MgO-based bioceramic coating synthesized in-situ by Plasma electrolytic oxidation

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Journal of Magnesium and Alloys 2021年第5期9卷 1611-1625页

作者： Nasrinsadat Azarian Seyed Mohammad Mousavi Khoei Department of Mining and Metallurgical Engineering Amirkabir University of Technology(Tehran Polytechnic)P.O.Box 15875-4413TehranIran

Plasma electrolytic oxidation(PEO)has held great potential for the advancement of biodegradable implants,as it helps in developing porous bioceramic coatings on the surface of magnesium alloys.In this research work,MgO-based bioceramic coatings containing the Si,P,Ca,Na,and F elements have been successfully fabricated on an AZ31 magnesium alloy plate utilizing the PEO method.The characteristic current-voltage behavior of the samples during the process was surveyed in an electrolyte containing Ca(H_(2)PO_(4))_(2),Na_(2)SiO_(3)·9H_(2)O,Na_(3)PO_(4)·12H_(2)O,NaF,and KOH with a pH of 12.5 and electrical conductivity of 20 mS/cm^(-1).The results revealed that applying a voltage of 350-400 V(that is 50-100 V higher than the breakdown limit)could greatly facilitate the synthesis of a PEO ceramic coating with fewer defects and more uniform morphology.The resulting coating was a compositionally graded bioceramic layer with a thickness in the range of 3.5±0.4 to 6.0±0.7µm,comprising the above-mentioned elements as promising bioactive agents.The synthesized ceramic features were investigated in terms of the elemental distribution of components through the thickness,which indicated a gradual rise in the Si and P contents and,conversely,a decline in the F content towards the outer surface.The growth mechanism of the PEO coating has been discussed accordingly.

关键词： Az31 magnesium alloy Plasma electrolytic oxidation Bioceramic Coating MgO-based ceramic

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