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Corrosion Behavior of Reactive Sputtered Al_2O_3 and ZrO_2 Thin Films on Mg Disk Immersed in Saline Solution

Journal of Materials Science & Technology 2015年第9期31卷 873-880页

作者： Ruben Kotoka Sergey Yarmolenko Devdas Pai Jag Sankar Engineering Research Center for revolutionizing metallic biomaterials North Carolina A&T State University

Magnesium has attracted a lot of attention over the last few decades due to its light weight and potential use as biomaterial However, the poor corrosion resistance of magnesium restricts its practical use for ap- plication where exposure to aggressive aqueous media is unavoidable. This paper describes the growth, characterization and corrosion analyses of Al2O3 and ZrO2 thin film coatings aimed at slowing down the fast degradation of Mg in saline solution. In this study, different thicknesses of Al2O3 and ZrO2 were de- posited on pure magnesium （99.95%） disk using pulsed-DC reactive sputtering process. The microstructure and phase analyses were performed using scanning electron microscopy （SEM） and X-ray diffraction （XRD）, respectively. The corrosion protection behavior of the Al2O3 and ZrO2 coated magnesium samples im- mersed in 0,9 wt% NaCl solution were evaluated using electrochemical measurement techniques, such as open-circuit potential （OCP）, potentiodynamic polarization （PD） and electrochemical impedance spectros- copy （EIS）. The microstructural analyses showed that the Al2O3 thin film coatings have circular grains between 5 and 25 nm, while the ZrO2 coatings have bigger ellipsoidal grains. The results from the electrochemical corrosion analyses showed that the Al2O3 coated Mg disk had corrosion resistance of approximately 3 times that of ZrO2 coated Mg disk. It was also observed that increasing the thickness of the Al2O3 coating im- proved the corrosion resistance of the Mg disk. These results suggest that Al2O3 and ZrO2 coating can be used to effectively control the fast degradation of magnesium for medical implant applications.

关键词： Magnetron sputteringMagnesiumAluminum oxideZirconium oxidePorosity

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Corrosion Protective Conversion Coatings on Magnesium Disks Using a Hydrothermal Technique

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Journal of Materials Science & Technology 2014年第1期30卷 47-53页

作者： R.K.Gupta K.Mensah-Darkwa D.Kumar Department of Chemistry Pittsburg State University Engineering Research Center for revolutionizing metallic biomaterials(erc-RMB) Department of Mechanical EngineeringNorth Carolina A&T State University

A uniform, compact, and well adherent conversion coating of magnesium hydroxide has been formed on bioresorbable magnesium disks by means of a hydrothermal technique. Electrochemical results indicate that the coating brings about a significant reduction in magnesium corrosion in phosphate buffered saline （PBS） solution. It is also observed that corrosion resistance of the coating increases with an increase in treatment time, which in turn, increases the coating thickness. The protective behavior of magnesium hydroxide coating is attributed to its chemical inertness in PBS solution. The coatings are found to be free from pores that reduce the direct contact between corroding media and underlying magnesium.

关键词： Magnesium Polarization Electrochemical impedance spectroscopy (EIS) Scanning electron microscopy (SEM) Conversioncoating Corrosion

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Effect of Post Heat Treatment on Corrosion Resistance of Phytic Acid Conversion Coated Magnesium

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Journal of Materials Science & Technology 2013年第2期29卷 180-186页

作者： R.K. Gupta K. Mensah-Darkwa D. Kumar Engineering Research Center for revolutionizing metallic biomaterials (erc-RMB) Department of Mechanical Engineering North Carolina A&T State University 1601 East Market Street Greensboro NC 27411 USA

An environment friendly chemical conversion coating for magnesium was obtained by using a phytic acid solution. The effect of post-coating 1heat treatment on the microstructures and corrosion properties of phytic acid conversion coated magnesium was investigated. It was observed that the microstructure and corrosion resistive properties were improved for the heat treated samples. The corrosion current density for bare magnesium, phytic acid conversion coated magnesium, and post-coating heat treated magnesium was calculated to be 2.48 ×10^-5, 1.18×10^-6, and 9.27 × 10^7 A/cm^2, respectively. The lowest corrosion current density for the heat treated sample indicated its highest corrosion resistive effect for the magnesium. The maximum corrosion protective nature of the heat treated sample was further confirmed by the largest value of impedance in electrochemical impedance spectroscopy studies.

关键词： Magnesium Phytic acid Corrosion Impedance spectroscopy Scanning electron microscopy

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Bio-Adaption between Magnesium Alloy Stent and the Blood Vessel:A Review

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Journal of Materials Science & Technology 2016年第9期32卷 815-826页

作者： Jun Ma Department of Chemical Biological and BioengineeringNorth Carolina Agricultural and Technical State UniversityGreensboroNCUSA nsf Engineering Research Center-revolutionizing metallic biomaterials North Carolina Agricultural and Technical State UniversityGreensboroNC USA

Biodegradable magnesium （Mg） alloy stents are the most promising next generation of bio-absorbable stents. In this article, we summarized the progresses on the in vitro studies, animal testing and clinical trials of biodegradable Mg alloy stents in the past decades. These exciting findings led us to propose the importance of the concept ＂bio-adaption＂ between the Mg alloy stent and the local tissue microenvironment after implantation. The healing responses of stented blood vessel can be generally described in three overlapping phases： inflammation, granulation and remodeling. The ideal bio-adaption of the Mg alloy stent, once implanted into the blood vessel, needs to be a reasonable function of the time and the space/dimension. First, a very slow degeneration of mechanical support is expected in the initial four months in order to provide sufficient mechanical support to the injured vessels. Although it is still arguable whether full mechanical support in stented lesions is mandatory during the first four months after implantation, it would certainly be a safety design parameter and a benchmark for regulatory evaluations based on the fact that there is insufficient human in vivo data available, especially the vessel wall mechanical properties during the healing/remodeling phase. Second, once the Mg alloy stent being degraded, the void space will be filled by the regenerated blood vessel tissues. The degradation of the Mg alloy stent should be 100% completed with no residues, and the degradation products （e.g., ions and hydrogen） will be helpful for the tissue reconstruction of the blood vessel. Toward this target, some future research perspectives are also discussed.

关键词： Mg stent Bio-adaptation Vessel Wound healing

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Mechanical and Corrosion Properties of Magnesiume-Hydroxyapatite (MgeHA) Composite Thin Films

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Journal of Materials Science & Technology 2013年第9期29卷 788-794页

作者： K.Mensah-Darkwa R.K.Gupta D.Kumar Engineering Research Center of revolutionizing metallic biomaterials Department of Mechanical Engineering North Carolina A & T State University Department of Chemistry Pittsburg State University

Magnesium(Mg)-hydroxyapatite(Ca10(PO4)6(OH)2,abbreviated as HA) composite films have been grown on Mg plates using a pulsed laser deposition *** property measurements and analysis have indicated that hardness and Young’s modulus of nMge(100e n)HA composite coatings increase with Mg content in the coatings and reach a maximum at a 70Mge 30HA composition.n and 100e n in the nMge(100e n)HA represent the relative number of laser pulses impinging on Mg and HA targets,*** current potentiodynamic polarization studies have shown that the corrosion of Mg plate(control) decreases with an increase in the HA ratio in the composite *** example,the corrosion current density of Mg plate reduces by w350 times after coating the Mg plate with 10Mge 90HA composite *** reduction in corrosion current density of Mg plates was also accompanied by a positive shift in the corrosion potential(w6%) due to this *** mechanism behind the reduction in corrosion behavior of Mg plates due to nMge(100e n) HA composite coatings has been understood by electrochemical impedance spectroscopy.

关键词： Magnesium Hydroxyapatite Scanning electron microscopy Pulsed laser deposition Corrosion Impedance spectroscopy

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Enhanced corrosion resistance of phytic acid coated magnesium by stearic acid treatment

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Transactions of Nonferrous Metals Society of China 2013年第5期23卷 1237-1244页

作者： R.K.GUPTA K.MENSAH-DARKWA J.SANKAR D.KUMAR Engineering Research Center for revolutionizing metallic biomaterials(erc-RMB) North Carolina A&T State University

A green chemical conversion coating for magnesium was obtained with a phytic acid solution. The microstructure and corrosion properties of phytic acid conversion coated magnesium were further improved by soaking in stearic acid solution. The phytic acid conversion coated magnesium after soaking in the stearic acid showed no micro-cracks and the surface became very smooth. The corrosion behavior of the uncoated and coated magnesium samples was studied by electrochemical methods. The corrosion resistance of the stearic acid treated sample was much higher than that of phytic acid conversion coated magnesium or uncoated magnesium. The electrochemical results indicated that the stearic acid treated coating provided effective corrosion protection to the magnesium sample.

关键词： magnesium phytic acid stearic acid corrosion impedance spectroscopy

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Systemic modulation of skeletal mineralization by magnesium implant promoting fracture healing: Radiological exploration enhanced with PCA-based machine learning in a rat femoral model

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Journal of Magnesium and Alloys 2024年第3期12卷 1009-1020页

作者： Yu Sun Heike Helmholz Regine Willumeit-Römer Institute of metallic biomaterials Helmholtz-Zentrum HereonGermany

The clinical application of magnesium(Mg)and its alloys for bone fractures has been well supported by in vitro and in vivo ***,there were studies indicating negative effects of high dose Mg intake and sustained local release of Mg ions on bone metabolism or repair,which should not be ignored when developing Mg-based ***,it remains necessary to assess the biological effects of Mg implants in animal models relevant to clinical treatment *** primary purpose of this study was to validate the beneficial effects of intramedullary Mg implants on the healing outcome of femoral fractures in a modified rat *** addition,the mineralization parameters at multiple anatomical sites were evaluated,to investigate their association with healing outcome and potential clinical *** to the control group without Mg implantation,postoperative imaging at week 12 demonstrated better healing outcomes in the Mg group,with more stable unions in 3D analysis and high-mineralized bridging in 2D *** bone tissue mineral density(TMD)was higher in the Mg group at the non-operated femur and lumbar vertebra,while no differences between groups were identified regarding the bone tissue volume(TV),TMD and bone mineral content(BMC)in *** the surgical femur,the Mg group presented higher TMD,but lower TV and BMC in the distal metaphyseal region,as well as reduced BMC at the osteotomy *** component analysis(PCA)-based machine learning revealed that by selecting clinically relevant parameters,radiological markers could be constructed for differentiation of healing outcomes,with better performance than 2D *** study provides insights and preclinical evidence for the rational investigation of bioactive materials,the identification of potential adverse effects,and the promotion of diagnostic capabilities for fracture healing.

关键词： Magnesium Implants Bone fracture Mineralization Systemic modulation Principal component analysis.

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Peri-implant gas accumulation in response to magnesium-based musculoskeletal biomaterials:Reframing current evidence for preclinical research and clinical evaluation

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Journal of Magnesium and Alloys 2024年第1期12卷 59-71页

作者： Yu Sun Heike Helmholz Regine Willumeit-Römer Institute of metallic biomaterials Helmholtz-Zentrum HereonMax-Planck-Str.1Geesthacht 21502Germany

Historically,the rapid degradation and massive gas release from magnesium(Mg)implants resulted in severe emphysema and mechanical *** the advent of new alloys and surface treatment methods,optimized Mg implants have re-entered clinics since last decade with reliable ***,the optimization aims at slowing down the degradation process,rather than exemption of the gas *** study involved a systematic evaluation of current preclinical and clinical evidence,regarding the physical signs,symptoms,radiological features,pathological findings and complications potentially associated with peri±implant gas accumulation(PIGA)after musculoskeletal Mg *** literature search identified 196 potentially relevant publications,and 51 papers were enrolled for further analysis,including 22 preclinical tests and 29 clinical studies published from 2005 to *** Mg-based materials have been evaluated in animal research,and the application of pure Mg and Mg alloys have been reported in clinical follow-ups involving multiple anatomical sites and musculoskeletal *** tissue and intraosseous PIGA are common in both animal tests and clinical follow-ups,and potentially associated with certain adverse *** examinations especially micro-CT and clinical CT scans provide valuable information for quantitative and longitudinal *** according to simulation tests involving Mg implantation and chemical processing,tissue fixation could lead to an increase in the volume of gas cavity,thus the results obtained from ex vivo imaging or histopathological evaluations should be interpreted with *** still lacks standardized procedures or consensus for both preclinical and clinical evaluation of ***,by providing focused insights into the topic,this evidence-based study will facilitate future animal tests and clinical evaluations,and support developing biocompatible Mg implants for the treatment of musculoskeletal

关键词： Magnesium implant Degradation Hydrogen Gas release Postoperative follow-up

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In silico studies of magnesium-based implants: A review of the current stage and challenges

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Journal of Magnesium and Alloys 2022年第11期10卷 2968-2996页

作者： Tamadur Albaraghtheh Regine Willumeit-Römer Berit Zeller-Plumhoff Helmholtz-Zentrum hereon GmbH Institute of Metallic BiomaterialsMax-Planck-Str.1Geesthacht 21502Germany

In silico methods to study biodegradable implants have recently received increasing attention due to their potential in reducing experimental time and cost. An important application case for in silico methods are magnesium(Mg)-based biodegradable implants, as they represent a powerful alternative to traditional materials used for temporary orthopaedic applications. Controlling Mg alloy degradation is critical to designing an implant that supports the bone healing process. To simulate different aspects of this biodegradation process, several mathematical models have been proposed with the ultimate aim of replacing laboratory experiments with computational modeling. In this review, we provide a comprehensive and critical discussion of the published models and their performance with respect to capturing the complexity of the biodegradation process. This complexity is presented initially. Additionally, the present review discusses the different approaches of optimizing and quantifying the different sources of errors and uncertainties within the proposed models.

关键词： Biodegradable implants Degradation In silico Phenomenological approach Physical approach Validation Verification Uncertainty quantification Mg

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Magnesium incorporated chitosan based scaffolds for tissue engineering applications

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Bioactive Materials 2016年第2期1卷 132-139页

作者： Udhab Adhikari Nava PRijal Shalil Khanal Devdas Pai Jagannathan Sankar Narayan Bhattarai Department of Mechanical Engineering North Carolina A&T State UniversityGreensboroNCUSA Department of Chemical Biological and BioengineeringNorth Carolina A&T State UniversityGreensboroNCUSA Department of Energy and Environmental Systems North Carolina A&T State UniversityGreensboroNCUSA nsf erc for revolutionizing metallic biomaterials North Carolina A&T State UniversityGreensboroNCUSA

Chitosan based porous scaffolds are of great interest in biomedical applications especially in tissue engineering because of their excellent biocompatibility in vivo,controllable degradation rate and tailorable mechanical *** paper presents a study of the fabrication and characterization of bioactive scaffolds made of chitosan(CS),carboxymethyl chitosan(CMC)and magnesium gluconate(MgG).Scaffolds were fabricated by subsequent freezing-induced phase separation and lyophilization of polyelectrolyte complexes of CS,CMC and *** scaffolds possess uniform porosity with highly interconnected pores of 50-250 μm size *** strengths up to 400 kPa,and elastic moduli up to 5 MPa were *** scaffolds were found to remain intact,retaining their original threedimensional frameworks while testing in in-vitro *** scaffolds exhibited no cytotoxicity to 3T3 fibroblast and osteoblast *** observations demonstrate the efficacy of this new approach to preparing scaffold materials suitable for tissue engineering applications.

关键词： Chitosan Magnesium gluconate Carboxymethyl chitosan Tissue engineering Composite scaffolds

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