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Hydroxyapatite-containing PEO-coating design for biodegradable Mg-0.8Ca alloy: Formation and corrosion behaviour

Journal of Magnesium and Alloys 2023年第12期11卷 4468-4484页

作者： a.s.gnedenkov s.L.sinebryukhov V.s.Filonina s.V.gnedenkov Institute of Chemistry of FEB RAs 159 Pr.100-letiya VladivostokaVladivostok690022Russian Federation

In this study, the biocompatible protective coating was formed using plasma electrolytic oxidation(PEO) on bioresorbable Mg-0.8Ca alloy. The composition of the formed coating was studied using XRD, sEM-EDX analysis, and micro-Raman spectroscopy. The uniform distribution of hydroxyapatite over the thickness of protective PEO-layer was established. Using traditional(EIs, PDP, OCP) and local scanning electrochemical methods(sVET, sIET with H^(+)-selective microelectrode), the level of protective properties of PEO-layer in a biological environment(mammalian cell culture medium, MEM) was determined. It was established that modification of Mg-0.8Ca alloy surface by PEO contributes to a significant increase in the corrosion resistance of the surface layer, making it possible to control the process of material‘s biodegradation. The maximum local electrochemical activity was recorded after 72 h of testing, while for the uncoated sample,intense corrosion degradation was recorded in the first 12 min of exposure to the cell culture medium. Formation of the PEO-coating results in a twofold decrease in the corrosion current density(2.8·10^(-6)A cm^(-2)) and an increase in the impedance modulus measured at a low frequency(1.7·10^(4)Ω cm^(2)) in comparison with the uncoated material(9.5·10^(-6)A cm^(-2);8.1·10^(3)Ω cm^(2)). The mechanism of material bioresorption was established and a model for biodegradation process of Mg-0.8Ca alloy with hydroxyapatite-containing PEO-coating in MEM was proposed. Analysis of these results and comparing with others obtained by various scientific groups indicate the prospects for application of biocompatible PEO-coating on Mg-Ca alloy in implant surgery.

关键词： Magnesium-calcium alloy Biodegradation Implant surgery Plasma electrolytic oxidation Electrochemistry Minimum essential medium Hydroxyapatite

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smart composite antibacterial coatings with active corrosion protection of magnesium alloys

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Journal of Magnesium and Alloys 2022年第12期10卷 3589-3611页

作者： a.s.gnedenkov s.L.sinebryukhov V.s.Filonina N.G.Plekhova s.V.gnedenkov Institute of Chemistry of FEB RAs 159 Pr.100-letiya VladivostokaVladivostok690022Russia

A new method of the formation of composite coatings with the function of active corrosion protection of magnesium alloys was developed using the plasma electrolytic oxidation(PEO) method. susceptibility of PEO-layers to pitting formation was evaluated using localized electrochemical methods(sVET/sIET). The morphological features and electrochemical properties of composite coatings were studied using sEM/EDX, XRD, micro-Raman spectroscopy and EIs/PDP measurements, respectively. The effect of surface layers impregnation with corrosion inhibitor on their protective properties in a corrosive environment was established. Additional protection was achieved using controllable coating pore sealing with polymer. It was found that the polymer treatment of the PEO-layer does not reduce the inhibitor’s efficiency. The formed protective composite inhibitor-and-polymer-containing layers decrease the corrosion current density of a magnesium alloy in a 3 wt.% Na Cl solution to three orders of magnitude. This predetermines the prospect of new smart coatings formation that significantly expand the field of application of electrochemically active materials. The mechanism of smart composite coating corrosion degradation was established. The antibacterial activity of the inhibitor-containing coatings against s. aureus methicillin-resistant strain was proved using the in vitro model. These protective layers are promising for reducing the incidence of implant-associated infections.

关键词： Magnesium alloy Plasma electrolytic oxidation Corrosion inhibitor self-healing Protective coatings

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Design of self-healing PEO-based protective layers containing in-situ grown LDH loaded with inhibitor on the MA8 magnesium alloy

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Journal of Magnesium and Alloys 2023年第10期11卷 3688-3709页

作者： a.s.gnedenkov s.L.sinebryukhov A.D.Nomerovskii V.s.Filonina A.Yu.Ustinov s.V.gnedenkov Institute of Chemistry of FEB RAs 159 Pr.100-letiya VladivostokaVladivostok690022Russia

The high corrosion rate of magnesium and its alloys in chloride-containing solution significantly reduces the potential of this material for diverse ***,the formation of a smart protective coating was achieved in this work to prevent degradation of the MA8 magnesium alloy.A porous ceramic-like matrix was obtained on the material by plasma electrolytic oxidation(PEO).Further surface functionalization was performed using layered double hydroxides(LDH) served as nanocontainers for the corrosion *** methods of LDH intercalation with benzotriazole(BTA) were *** composition and morphology of the formed coating were studied using sEM-EDX analysis,XRD,XPs,and Raman *** corrosion behavior of the coated samples was evaluated using electrochemical impedance spectroscopy and potentiodynamic *** corrosion rate was estimated using volumetry and gravimetry *** formed composite coating provides the Mg alloy with the lowest corrosion activity(|Z|_(f)=0.1 Hz)=8.48·10^(5) Ω·cm^(2),I_(c)=1.4·10^(-8)A/cm^(2),P_(H)=0.21 mm/year) and improves the protective properties of the PEO-coated sample(|Z|_(f)=0.1 Hz)=8.37·10^(3) Ω·cm^(2),I_(c)=4.1·10^(-7)A/cm^(2),P_(H)=0.31 mm/year).The realization of the self-healing effect of the inhibitor-containing LDH/PEO-coated system was studied using localized electrochemical methods(sVET and sIET) with two artificial defects on the surface.A mechanism involving three stages for the active corrosion protection of the alloy was *** findings contribute to the follow-up work of developing modified LDH/PEO-based structures that promote the Mg alloy with high corrosion resistance,superior electrochemical performance for applications in various fields of industry and medicine.

关键词： Magnesium alloy Plasma electrolytic oxidation Layered double hydroxides Corrosion inhibitor Electrochemistry Corrosion rate

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The detailed corrosion performance of bioresorbable Mg-0.8Ca alloy in physiological solutions

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Journal of Magnesium and Alloys 2022年第5期10卷 1326-1350页

作者： a.s.gnedenkov s.L.sinebryukhov V.s.Filonina V.s.Egorkin A.Yu.Ustinov V.I.sergienko s.V.gnedenkov Institute of Chemistry of FEB RAs 159 Pr.100-letiya VladivostokaVladivostok690022Russia

The electrochemical behaviour of biodegradable magnesium alloy Mg-0.8Ca was evaluated in a mammalian cell culture medium(MEM)and Na Cl solutions(0.9 wt.%, 0.3 wt.%) using traditional(EIs, PDP, OCP) and local scanning electrochemical(sVET, sIET with p H-selective microelectrode) methods at the micro-and meso-level. Corrosion rates of samples in two different media were determined using weight loss tests. The influence of testing media components, alloy composition and microstructure on the material’s degradation process was *** sVET/sIET test parameters were optimized for in vitro investigation of the bioresorbable material surface. The mechanism of the alloy’s bioresorption was suggested. The effect of microsized phases on the corrosion behaviour of the alloy was proved using complementary in situ monitoring and sKPFM measurements. The rapid degradation rate of the alloy is related to the presence of local microgalvanic cells formed by cathodic α-magnesium matrix and anodic Mg_(2)Ca phase. The highest corrosion activity was revealed in the first 12 min of sample exposure to MEM, followed by stabilization of corrosion process due to the material’s passivation. Using sEM-EDX analysis, micro-Raman spectroscopy and XPs analysis the composition of the corrosion products was determined. Degradation in MEM proceeds with a formation of magnesium-and-carbonate substituted hydroxyapatite-containing film on the sample’s surface. The low possibility of application of Mg-0.8Ca alloy without coating protection in implant surgery was highlighted.

关键词： Magnesium-calcium alloy Biodegradation Corrosion rate Electrochemistry Weight loss Minimum essential medium

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Influence of ZrO_(2)/siO_(2) nanomaterial incorporation on the properties of PEO layers on Mg-Mn-Ce alloy

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Journal of Magnesium and Alloys 2022年第2期10卷 552-566页

作者： D.V.Mashtalyar I.M.Imshinetskiy K.V.Nadaraia a.s.gnedenkov s.L.sinebryukhov A.Yu.Ustinov A.V.samokhin s.V.gnedenkov Institute of Chemistry Far Eastern BranchRussian Academy of SciencesVladivostok 690022Russian Federation Far Eastern Federal University Vladivostok 690922Russian Federation A.A.Baikov Institute of Metallurgy and Materials science Russian Academy of SciencesMoscow 119991Russian Federation

The properties of coatings formed on the MA8 magnesium alloy by the plasma electrolytic oxidation in electrolytes containing mechanical mixture of zirconia and silica nanoparticles in concentrations of 2,4 and 6 g/l have been *** has been established by sEM,EDs,and XPs that ZrO_(2)/siO_(2)nanoparticles successfully were incorporated into the ***-Raman spectroscopy showed the presence of ZrO_(2)in tetragonal and monoclinic forms in the PEO-coating composition as well as Mg_(2)siO_(4) in tetrahedral configuration uniformly distributed in the outer part of *** coatings significantly reduce corrosion current density in comparison with bare Mg alloy and base PEOlayer(from 2.4×10^(–7)A/cm^(2) for base PEO layer to 0.7×10^(–7)A/cm^(2) for coatings with nanoparticles).It has been found that the presence of solid nanoparticles in the composition of coating has a positive effect on their hardness(this parameter was increased from 2.1±0.3 GPa to 3.1±0.4 GPa)and wearproof(the wear was reduced from(4.3±0.4)×10^(–5)mm^(3)/(N×m)to(3.5±0.2)×10^(–5)mm^(3)/(N×m)).

关键词： Plasma electrolytic oxidation Composite coatings Nanoparticles Zirconia silica Protective coatings

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Effect of TiO_(2) nanoparticles on the photocatalytic properties of PEO coatings on Mg alloy

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Journal of Magnesium and Alloys 2023年第2期11卷 735-752页

作者： D.V.Mashtalyar I.M.Imshinetskiy K.V.Nadaraia a.s.gnedenkov s.N.suchkov D.P.Opra E.V.Pustovalov A.Yu Ustinov s.L.sinebryukhov s.V.gnedenkov Institute of Chemistry Far Eastern BranchRussian Academy of SciencesVladivostok690022Russia Far Eastern Federal University Vladivostok690950Russia

A comprehensive study of the properties of coatings formed on a magnesium alloy by plasma electrolytic oxidation(PEO) using the electrolytes with nanosized particles of anatase(titanium dioxide) has been carried out. Formed coatings reduce corrosion current density 2.5-fold and increase hardness by 25% compared to a coating without particles. Confocal micro-Raman spectroscopy revealed the presence of anatase and rutile phases in the composition of PEO coating due to the incorporation of TiO2nanoparticles during plasma electrolytic treatment. The presence of titanium dioxide had a positive effect on the photocatalytic properties of coatings: the constant rate of the methyl orange and methyl blue decomposition is increased in 1.6 and 1.8-fold, respectively, compared to the coating formed in electrolyte without TiO_(2) particles.

关键词： Plasma electrolytic oxidation Nanoparticles Titanium dioxide Photocatalysis Protective coatings

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Effect of Ta_(2)O_(5)nanoparticles on bioactivity,composition,structure,in vitro and in vivo behavior of PEO coatings on Mg-alloy

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Journal of Magnesium and Alloys 2024年第6期12卷 2360-2379页

作者： D.V.Mashtalyar I.M.Imshinetskiy V.V.Kashepa K.V.Nadaraia M.A.Piatkova A.I.Pleshkova K.A.Fomenko A.Yu.Ustinov s.L.sinebryukhov s.V.gnedenkov Institute of Chemistry Far Eastern BranchRussian Academy of SciencesVladivostok690022Russia Far Eastern Federal University Vladivostok690950Russia Regional Clinical Dermatovenerological Dispensary Vladivostok690033Russia

The present study investigates the physical and chemical characteristics,behavior in vitro and in vivo,and biocompatibility of coatings containing Ta_(2)O_(5),which are obtained by plasma electrolytic oxidation(PEO)on MA8 magnesium *** obtained coatings demonstrate in vivo biocompatibility and in vitro *** to the base PEO coating,the layers containing Ta_(2)O_(5)facilitate the development of apatite in simulated body fluid,suggesting that the inclusion of nanoparticles improves bioactivity of the *** was found that incorporation of Ta_(2)O_(5)nanoparticles increases roughness and porosity of the formed layers by increasing particle concentration in electrolytes for the PEO process contributing to sufficient soft tissue ingrowth in *** on in vivo studies,these coatings also provide favorable tissue response and minimal inflammatory reaction in comparison with the bare magnesium alloy due to protection of living tissues from deleterious corrosion events of magnesium implant such as local alkalization and intense hydrogen *** results obtained in the present study concluded biocompatibility,tissue integration of the PEO coatings containing Ta_(2)O_(5)nanoparticles making them a promising protective layer for biodegradable magnesium implants.

关键词： Plasma electrolytic oxidation Bioactive coatings Tantalum pentoxide simulated body fluid(sBF) Apatite formation Histology

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Antibacterial HA-coatings on bioresorbable Mg alloy

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Journal of Magnesium and Alloys 2024年第5期12卷 1965-1985页

作者： K.V.Nadaraia D.V.Mashtalyar M.A.Piatkova A.I.Pleshkova I.M.Imshinetskiy M.s.Gerasimenko E.A.Belov V.V.Kumeiko D.N.Kozyrev K.A.Fomenko V.V.Mostovaya B.R.Torpanov A.R.Biktimirov I.s.Osmushko s.L.sinebryukhov s.V.gnedenkov Institute of Chemistry FEB RAs 159 Pr.100-letiya VladivostokaVladivostok 690022Russia Far Eastern Federal University 10 Ajax BayRussky IslandVladivostok 690922Russia A.V.Zhirmunsky National scientific Center of Marine Biology FEB RAs 17 St.PalchevskogoVladivostok 690041Russia Regional Clinical Dermatovenerological Dispensary 18 V St.GamarnikaVladivostok 690033Russia NMIC“Treatment and Rehabilitation Center” 3 Ivankovskoe highwayMoscow 125367Russia

In this study,a calcium-phosphate coating was formed on a Mg-Mn-Ce alloy by the plasma electrolytic oxidation(PEO).The antibiotic vancomycin,widely used in the treatment of infections caused by staphylococcus aureus(***),was impregnated into the *** with vancomycin showed high bactericidal activity against *** mechanical and electrochemical properties of the formed coatings were studied,as well as in vitro cytotoxicity tests and in vivo tests on mature male rats were *** to sEM,EDs,XRD and XPs data,coatings had a developed morphology and contained hydroxyapatite,which indicates high *** analysis of roughness of coatings without and with vancomycin did not reveal any differences,confirming the high roughness of the *** electrochemical tests,an increase in corrosion resistance by more than two times after the application of PEO coatings was *** to the results of an in vivo study,after 28 days of the implantation of samples with calcium phosphate PEO coating and vancomycin,no signs of inflammation were observed,while an inflammatory reaction developed in the area of implantation of bare alloy,followed by *** release tests from the coatings show a sharp decrease in the concentration of the released antibiotic on day 7 and then a gradual decrease until day *** the experiment,no significant deviations in the condition and behavior of the animals were observed;clinical tests did not reveal a systemic toxic reaction.

关键词： Bioactive coatings Biocompatibility Mg alloy Plasma electrolytic oxidation Hydroxyapatite Vancomycin

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Plasma electrolytic oxidation of the magnesium alloy MA8 in electrolytes containing TiN nanoparticles

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Journal of Materials science & Technology 2017年第5期33卷 461-468页

作者： D.V.Mashtalyar s.V.gnedenkov s.L.sinebryukhov I.M.Imshinetskiy A.V.Puz Institute of Chemistty Far Eastern BranchRussian Academy of Sciences 159Prosp.100-1etya VladivostokaVladivostok 690022Russia Far Eastern Federal University 8 Sukhanova St.Vladivostok690950Russia

The formation of protective multifunctional coatings on magnesium alloy MA8 using plasma electrolyt- ic oxidation （PEO） in an electrolytic system containing nanosized particles of titanium nitride was investigated. Electrochemical and mechanical properties of the obtained layers were examined. It was established that microhardness of the coating with the nanoparticle concentration of 3 gl-1 increased twofold （4.2 ± 0.5 GPa）, while wear resistance decreased （4.97 × 10-6 mm3 N-1 m-1）, as compared to re- spective values for the PEO-coating formed in the electrolyte without nanoparticles （2.1 ± 0.3 GPa, 1.12 × 10.5 mm3 N-1 m-1）.

关键词： Magnesium alloys Protective coatings Plasma electrolytic oxidation Corrosion titanium nitride Nanoparticles

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New approach to formation of coatings on Mg-Mn-Ce alloy using a combination of plasma treatment and spraying of fluoropolymers

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Journal of Magnesium and Alloys 2022年第4期10卷 1033-1050页

作者： D.V.Mashtalyar K.V.Nadaraia I.M.Imshinetskiy s.L.sinebryukhov s.V.gnedenkov Institute of Chemistry FEB RAs 159 Pr.100-letiyaVladivostok 690022Russia Far Eastern Federal University 10 Ajax BayRussky IslandVladivostok 690922Russia

This paper presents a method of the formation of composite polymer-containing coatings on a Mg–Mn–Ce magnesium alloy by forming a ceramic-like layer using plasma electrolytic oxidation(PEO)and subsequent spraying superdispersed polytetrafluoroethylene *** coating composition and their morphological features were studied by sEM,EDs,GDOEs,and *** presented data confirm the embedding of fluoropolymer in the PEO *** evaluation of the corrosion properties of the formed composite polymer-containing coatings indicates a decrease in the corrosion current density by more than 3 orders of magnitude in comparison with the base PEO *** incorporation of a fluoropolymer in a PEO layer by more than 32%increases the load value at which abrasion of the coating to the substrate occurs and reduces the wear of the coating by more than 27 fold in comparison with the PEO *** has been established that composite coatings possess hydrophobic properties:the value of the contact angle attains 152°.

关键词： Plasma electrolytic oxidation Polytetrafluoroethylene Composite coatings Corrosion Wear superhydrophobicity

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