Antimicrobial and Cytocompatible Bovine Hydroxyapatite-Alumina-Zeolite Composite Coatings Synthesized by Pulsed Laser Deposition from Low-Cost Sustainable Natural Resources

Bovine hydroxyapatite (BHA) and BHA blended with clinoptilolite (CLIN) and alumina (Al2O3) coatings were synthesized using pulsed laser deposition (PLD) with a KrF* excimer laser source (lambda = 248 nm, tau(FWHM) <= 25 ns). Physical-chemical characteristics and the potential use of coatings for preventing bacteria adhesion and biofilm formation were investigated. Optimized PLD conditions were selected for coatings with rough morphologies, suitable for good cell adhesion and implant anchorage and good replication of the source target composition. The crystallinity of composite coatings was progressively decreasing with the augment of the Al2O3 and CLIN contents, which in turn can facilitate an efficacious release of active components. Al2O3- and CLIN-containing coatings exhibited high cytocompatibility and specific antibiofilm profiles, preventing the initiation and maturation of bacterial biofilms. Optimum biological activity profiles associated with the use of sustainable and/or inexpensive materials are, in our opinion, of key importance for the future development of performant implant coatings, which should he perfectly compatible with the surrounding tissue while preventing postsurgical endogenous or nosocomial infections

Hydroxyapatite nano-powders produced hydrothermally from nacreous material

Nano-powders of pure AB-type carbonated hydroxyapatite (HA) sized of similar to 100 nm were successfully produced via hydrothermal transformation (HT) of milled oyster shell powders at 200 degrees C. Low production cost, worldwide availability and natural-biological origin of raw materials are important features of the investigated process. When fine shell powders were used, the transformation reaction from aragonite to hydroxyapatite was accomplished within about 24 h. Calcite, concentrated at the outer surface of the shells, was less prone to transform into hydroxyapatite under the investigated hydrothermal conditions, even after prolonged reaction time (72 h) or in highly concentrated phosphate solutions. (c) 2006 Elsevier Ltd. All rights reserved

Microstructure and mechanical properties of sintered enamel hydroxyapatite

The influence of sintering temperature on the microstructure and the mechanical properties (i.e. compressive strength and microhardness) of samples of calcinated human enamel was investigated. The experimental results indicate a low densification regime after sintering at low temperatures (1000 degrees C, 1100 degrees C) and a high densification regime after sintering at higher temperatures (1200 degrees C, 1300 degrees C). With respect to earlier studies, high mechanical properties were achieved. The enhancement of mechanical properties was attributed to the presence of fluorine traces in enamel. (c) 2006 Elsevier Ltd and Techna Group S.r.l. All rights reserved

Tropical Sea Snail Shells: Possible Exotic Sources for Ceramic Biomaterial Synthesis

In this study, chemical and structural properties of sea snail shell based bioceramic materials (i.e. hydroxyapatite, whitlockite and other phases) are produced by using mechano-chemical (ultrasonic) conversion method. For this purpose, differential thermal and gravimetric analysis (DTA/TG), X-ray diffraction, infra-red (IR) and scanning electron microscope (SEM) studies are performed

Characterization of calcium phosphate powders originating from Phyllacanthus imperialis and Trochidae Infundibulum concavus marine shells

The study reports the preparation and characterization of powders consisting of the different phases of calcium phosphates that were obtained from the naturally derived raw materials of sea-shell origins reacted with H3PO4. Species of sea origin, such as corals and nacres, attracted a special interest in bone tissue engineering area. Nacre shells are built up of calcium carbonate in aragonite form crystallized in an organic matrix. In this work two natural marine origin materials (shells of echinoderm Sputnik sea urchin - Phyllacanthus imperialis and Trochidae Infundibulum concavus mollusk) were involved in the developing powders of calcium phosphate based biomaterials (as raw materials for bone-scaffolds) by hotplate and ultrasound methods. Thermal analyses of the as-prepared materials were made for an assessment of the thermal behavior and heat treatment temperatures. Samples from both sea shells each of them prepared by the above mentioned methods were subjected to thermal treatments at 450 degrees C and 850 degrees C in order to evaluate the crystalline transformations of the calcium phosphate structures in the heating process. By X-ray diffraction analyses various calcium phosphate phases were identified. In Sputnik sea urchins originated samples were found predominantly brushite and calcite as a small secondary phase, while in Trochidae L concavus samples mainly monetite and HA phases were identified. Thermal treatment at 850 degrees C resulted flat-plate whitlockite crystals - beta-MgTCP [(Ca, Mg)(3) (PO4)(2)] for both samples regardless the preparation method (ultrasound or hotplate) or the targeted Ca/P molar ratio according with XRD patterns. Scanning electron microscopy and Fourier transformed infrared spectroscopy were involved more in the characterization of these materials and the good correlations of the results of these methods were made. (C) 2013 Elsevier B.V. All rights reserved

Sol-gel derived alumina-hydroxyapatite-tricalcium phosphate porous composite powders

In this study, alumina-hydroxyapatite-tricalcium phosphate (alpha-Al2O3-HA-TCP) porous composite powders were produced and characterized. At first, boehmite sol (AlOOH) was obtained via sol gel process by using aluminium isopropoxide (Al(OC3H7)(3)) as the starting material. Bovine hydroxyapatite (BHA) powders derived from deproteinized bovine bones were added as 10, 20, 30 and 50% weight of the starting material to each boehmite sol. Also Na-alginate was added to the boehmite sol as the dispersive agent. Subsequently, gelation for 3 h at 110 degrees C was applied to each sol mixture. Finally, gelated samples were heat treated for 2 h at 500, 800, 1000 and 1300 degrees C. DTA-TGA, XRD, FTIR and SEM-EDS analyses were used to characterize the obtained composite powders composed of alpha-Al2O3-HA-TCP phases. In order to investigate porosity properties, powders were pressed with hydraulic manual press and formed into pellets. Later these pellets were sintered for 2 h at 1300 degrees C. Apparent porosity and bulk density tests were applied to the pellets. The evaluation of these tests results indicate that a novel alpha-Al2O3-HA-TCP composite material with similar to 38-44% apparent porosity has been produced. Crown Copyright (C) 2011 Published by Elsevier Ltd and Techna Group S.r.l. All rights reserved

Novel doped hydroxyapatite thin films obtained by pulsed laser deposition

We report on the synthesis of novel ovine and bovine derived hydroxyapatite thin films on titanium substrates by pulsed laser deposition for a new generation of implants. The calcination treatment applied to produce the hydroxyapatite powders from ovine/bovine bones was intended to induce crystallization and to prohibit the transmission of diseases. The deposited films were characterized by scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, and energy dispersive X-ray spectroscopy. Pull-off adherence and profilometry measurements were also carried out. X-ray diffraction ascertained the polycrystalline hydroxyapatite nature of the powders and films. Fourier transform infrared spectroscopy evidenced the vibrational bands characteristic to a hydroxyapatite material slightly carbonated. The micrographs of the films showed a uniform distribution of spheroidal particulates with a mean diameter of similar to 2 mu m. Pull-off measurements demonstrated excellent bonding strength values between the hydroxyapatite films and the titanium substrates. Because of their physical-chemical properties and low cost fabrication from renewable resources, we think that these new coating materials could be considered as a prospective competitor to synthetic hydroxyapatite used for implantology applications. (C) 2012 Elsevier B.V. All rights reserved

Physical-chemical characterization and biological assessment of simple and lithium-doped biological-derived hydroxyapatite thin films for a new generation of metallic implants

We report on the synthesis by PLD of simple and lithium-doped biological-origin hydroxyapatite (HA) films. The role of doping reagents (Li2CO3, Li3PO4) on the morphology, structure, chemical composition, bonding strength and cytocompatibility of the films was investigated. SEM investigations of the films evidenced a surface morphology consisting of particles with mean diameters of (5-7) mu m. GIXRD analyses demonstrated that the synthesized structures consisted of HA phase only, with different degrees of crystallinity, mainly influenced by the doping reagent type. After only three days of immersion in simulated body fluid, FTIR spectra showed a remarkable growth of a biomimetic apatitic film, indicative of a high biomineralization capacity of the coatings. EDS analyses revealed a quasi-stoichiometric target-to-substrate transfer, the values inferred for the Ca/P ratio corresponding to a biological apatite. All synthesized structures displayed a hydrophilic behavior, suitable for attachment of osteoblast cells. In vitro cell viability tests showed that the presence of Li2CO3 and Li3PO4 as doping reagents promoted the hMSC growth on film surfaces. Taking into consideration these enhanced characteristics, corroborated with a low fabrication cost generated by sustainable resources, one should consider the lithium-doped biological-derived materials as promising prospective solutions for a next generation of coated implants with rapid osteointegration. (C) 2018 Elsevier B.V. All rights reserved

Bond-coating in plasma-sprayed calcium-phosphate coatings

The influence of bond-coating on the mechanical properties of plasma-spray coatings of hydroxyatite on Ti was investigated. Plasma-spray powder was produced from human teeth enamel and dentine. Before processing the main apatite coating, a very thin layer of Al2O3/TiO2 was applied on super clean and roughened, by Al2O3 blasting, Ti surface as bond-coating. The experimental results showed that bond-coating caused significant increase of the mechanical properties of the coating layer: In the case of the enamel powder from 6.66 MPa of the simple coating to 9.71 MPa for the bond-coating and in the case of the dentine powder from 6.27 MPa to 7.84 MPa, respectively. Both tooth derived powders feature high thermal stability likely due to their relatively high content of fluorine. Therefore, F-rich apatites, such those investigated in this study, emerge themselves as superior candidate materials for calcium phosphate coatings of producing medical devices. The methods of apatite powder production and shaping optimization of powder particles are both key factors of a successful coating. The methods used in this study can be adopted as handy, inexpensive and reliable ways to produce high quality of powders for plasma spray purposes

In Vivo Assessment of Bone Enhancement in the Case of 3D-Printed Implants Functionalized with Lithium-Doped Biological-Derived Hydroxyapatite Coatings: A Preliminary Study on Rabbits

We report on biological-derived hydroxyapatite (HA, of animal bone origin) doped with lithium carbonate (Li-C) and phosphate (Li-P) coatings synthesized by pulsed laser deposition (PLD) onto Ti6Al4V implants, fabricated by the additive manufacturing (AM) technique. After being previously validated by in vitro cytotoxicity tests, the Li-C and Li-P coatings synthesized onto 3D Ti implants were preliminarily investigated in vivo, by insertion into rabbits' femoral condyles. The in vivo experimental model for testing the extraction force of 3D metallic implants was used for this study. After four and nine weeks of implantation, all structures were mechanically removed from bones, by tensile pull-out tests, and coatings' surfaces were investigated by scanning electron microscopy. The inferred values of the extraction force corresponding to functionalized 3D implants were compared with controls. The obtained results demonstrated significant and highly significant improvement of functionalized implants' attachment to bone (p-values <= 0.05 and <= 0.00001), with respect to controls. The correct placement and a good integration of all 3D-printed Ti implants into the surrounding bone was demonstrated by performing computed tomography scans. This is the first report in the dedicated literature on the in vivo assessment of Li-C and Li-P coatings synthesized by PLD onto Ti implants fabricated by the AM technique. Their improved mechanical characteristics, along with a low fabrication cost from natural, sustainable resources, should recommend lithium-doped biological-derived materials as viable substitutes of synthetic HA for the fabrication of a new generation of metallic implant coatings