Application of novel organic–inorganic hybrid sol–gel coatings containing dispersed hydroxyapatite particles improved the biocompatibility and corrosion protection properties of the Ti6Al4V alloy used in medical implants.
The aim of this work was to prepare hydroxyapatite coatings (HAp) by a sol-gel method on Ti6Al4V alloy and to study the bioactivity, biocompatibility and corrosion protection behaviour of these coatings in presence of simulated body fluids (SBFs). Thermogravimetric/Differential Thermal Analyses (TG/DTA) and X-ray Diffraction (XRD) have been applied to obtain information about the phase transformations, mass loss, identification of the phases developed, crystallite size and degree of crystallinity of the obtained HAp powders. Fourier Transformer Infrared Spectroscopy (FTIR) has been utilized for studying the functional groups of the prepared structures. The surface morphology of the resulting HAp coatings was studied by Scanning Electron Microscopy (SEM). The bioactivity was evaluated by soaking the HAp-coatings/Ti6Al4V system in Kokubo’s Simulated Body Fluid (SBF) applying Inductively Coupled Plasma (ICP) spectrometry. 3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyl tetrazolium bromide (MTT) and Alamar blue cell viability assays were used to study the biocompatibility. Finally, the corrosion behaviour of HAp-coatings/Ti6Al4V system was researched by means of Electrochemical Impedance Spectroscopy (EIS). The obtained results showed that the prepared powders were nanocrystalline HAp with little deviations from that present in the human bone. All the prepared HAp coatings deposited on Ti6Al4V showed well-behaved biocompatibility, good bioactivity and corrosion protection properties.
Ti6Al4V samples, obtained by selective laser melting (SLM), were subjected to successive treatments: acid etching, chemical oxidation in hydrogen peroxide solution and thermochemical processing. The effect of temperature and time of acid etching on the surface roughness, morphology, topography and chemical and phase composition after the thermochemical treatment was studied. The surfaces were characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction and contact profilometry. The temperature used in the acid etching had a greater influence on the surface features of the samples than the time. Acid etching provided the original SLM surface with a new topography prior to oxidation and thermochemical treatments. A nanostructure was observed on the surfaces after the full process, both on their protrusions and pores previously formed during the acid etching. After the thermochemical treatment, the samples etched at 40 °C showed macrostructures with additional submicro and nanoscale topographies. When a temperature of 80 °C was used, the presence of micropores and a thicker anatase layer, detectable by X-ray diffraction, were also observed. These surfaces are expected to generate greater levels of bioactivity and high biomechanics fixation of implants as well as better resistance to fatigue.
The aim of this work was to prepare bioactive hydroxyapatite coatings by sol-gel method and to study the effect of thermal treatment temperature upon the bioactivity and corrosion protection of these coatings on Ti6Al4V alloy. The application of (DTA/TGA) and (XRD) has provided valuable information about the phase transformation, mass loss, identification of the phases developed, crystallite size and degree of crystallinity. (SEM/EDX) has been applied to study the surface morphology of coated samples before and after immersion in simulated body fluid (SBF) to detect the biomimetic precipitation of the bonelike apatite. The obtained results show that all the prepared samples are ceramic nanocrystalline with crystal structure and composition like hydroxyapatite, with little deviations from that present in the human bone. The bioactivity of the studied samples is found to be closely related to the thermal treatments applied. That is, the bioactivity decreases as the temperature of the thermal treatment increase. Coatings from such prepared hydroxyapatite sol have been accomplished by dip-coating technique on non-toxic Ti6Al4V alloy for biomedical applications. The corrosion behaviour of the resulting hydroxyapatite coatings in a (SBF) has been studied by electrochemical impedance spectroscopy (EIS). The hydroxyapatite coated Ti6Al4V alloy displayed excellent bioactivity when soaked in the (SBF) and acceptable corrosion protection behaviour.
Resumen Se han preparado nuevos recubrimientos de hidroxiapatita (HAp) obtenidos a partir de precursores de tipo sol-gel, depositados sobre sustratos metálicos de una aleación de base hierro denominada MA956, previamente oxidados a elevadas temperaturas, para mejorar la adherencia con los recubrimientos de hidroxiapatita. El recubrimiento sol-gel se obtuvo aplicando una ruta acuosa, utilizando como precursores del fósforo y del calcio trietilfosfito y nitrato calcico tetrahidratado, respectivamente. Sobre los geles resultantes se aplicaron distintos tratamientos térmicos de sinterización, hasta la obtención de recubrimientos de hidroxiapatita homogéneos, adhérentes y cristalinos. Las técnicas de caracterización utilizadas para realizar este estudio han sido microscopía óptica, MBE/EDX, DRX y FTIR. Así mismo, se ha determinado la adherencia entre el substrato y el recubrimiento de hidroxiapatita según la norma ASTM D 3359-02. Los resultados obtenidos han mostrado que el tratamiento térmico óptimo se consigue cuando se aplica una temperatura de sinterización de 550 °C durante un tiempo igual a 72 h. Palabras clave Hidroxiapatita. Recubrimientos sol-geL Biomateriales. Aleación MA956. Hydroxyapatite coatings prepared by a sol-gel process Abstract Hydroxyapatite coatings (HAp) have been obtained starting from precursors of sol-gel type. The coatings previously oxidized were deposited on metal surfaces of a based on iron alloy so-called MA956. The alloys were at high temperatures, in order to improve the adhesion with the hydroxyapatite coatings. The sol-gel coating was obtained applying an aqueous route, using triethyl phosphite and aqueous calcium nitrate, as precursors of phosphorous and calcium, respectively. Different sintering thermal treatments were applied on the resulting gels in order to obtain a homogeneous, adherent and crystalline hydroxyapatite coating. The characterization techniques used for this study were optical microscopy, SEM/EDX, XDR and FTIR. Moreover, the adhesion between the hydroxylapatite coating and the substrate was assessed according to the ASTM D 3359-02 standard test method. The results of this study showed that the best thermal treatment is obtained for a sintering temperature of 550 °C during a time of 72 h.
The control of the texture in synthetic hydroxyapatite ceramics had limited their application in the ield of the materials for bone implantation, even more when it is used as a illing in cements and other formulations in orthopedic surgery. The present article shows preliminary results demonstrating the efectiveness of a modiication of the controlled rate thermal analysis (CRTA), developed by J. Rouquerol, used for the preparation of ceramic materials with controlled textural characteristics, during the formation of ceramic powders of synthetic hydroxyapatite at low temperatures. The thermal treatments of the hydroxyapatite were carried out in a device connected to a computer, to control temperature and pressure system, keeping the decomposition speed constant. Results, reported when preparing ceramic powders of hydroxyapatite at 300 and 850°C under controlled pressure, using synthetic hydroxyapatite with a Ca/P molar ratio equal to 1.64, were checked using IR spectroscopy and X-ray difraction, showed that the formed phase corresponds to that of crystalline hydroxyapatite, even at 300°C of maximum temperature. Values of speciic surface (BET) between 17 and 66 m 2 /g, with pore size in the range of 50-300 Å in both cases are obtained by N 2 absorption isotherms, when analyzing the isotherms of nitrogen absorption.
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