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In the present study, amorphous tricalcium phosphate (TCP) has been synthetized by a wet route to obtain low temperature a-TCP at 650 °C (LT-aTCP) and compare its structural, physical–chemical and thermal properties with those of a-TCP obtained by the conventional solid-state reaction method at 1400 °C (HT-aTCP). Even if no significant differences were observed concerning the values of lattice parameters measured by Rietveld refinement, LT-aTCP presented lower crystallinity and higher crystal strains than HT-aTCP. The reactivity in water of the a-TCP obtained by the two different routes was assessed. Both raw samples appeared relatively inert in solution and did not favour the nucleation of calcium deficient apatite (CDA); the LT-aTCP and HT-aTCP were converted into apatite only after milling. The mechanical process leads to a decrease in crystallinity and the formation of an amorphous phase, which is supported in this work by Raman spectroscopy. The faster rate of conversion of milled LT-aTCP compared to HT-aTCP can be assigned to its higher specific surface area, lower crystallinity and higher residual crystal strain; these favour the dissolution of the a-TCP phase. Finally, the setting properties of a-TCP-based bone cements were compared regarding their synthesis route. Although the synthesis route does not significantly affect the setting times, the kinetic of conversion into CDA was faster for LT-aTCP than for HT-aTCP. Thus, the modulation of the dissolution rate of a-TCP-based cement determined by the preparation route and the grinding process allows control of the overall setting reaction., Peer Reviewed, Postprint (author's final draft)

Peri-implantitis is an infectious disease that affects the supporting soft and hard tissues around dental implants and its prevalence is increasing considerably. The development of antibacterial strategies, such as titanium antibacterial-coated surfaces, may be a promising strategy to prevent the onset and progression of peri-implantitis. The aim of this study was to quantify the biofilm adhesion and bacterial cell viability over titanium disc with or without antibacterial surface treatment. Five bacterial strains were used to develop a multispecies oral biofilm. The selected species represent initial (Streptococcus oralis and Actinomyces viscosus), early (Veillonella parvula), secondary (Fusobacterium nucleatum) and late (Porphyromonas gingivalis) colonizers. Bacteria were sequentially inoculated over seven different types of titanium surfaces, combining different roughness level and antibacterial coatings: silver nanoparticles and TESPSA silanization. Biofilm formation, cellular viability and bacterial quantification over each surface were analyzed using scanning electron microscopy, confocal microscopy and real time PCR. Biofilm formation over titanium surfaces with different bacterial morphologies could be observed. TESPSA was able to significantly reduce the cellular viability when compared to all the surfaces (p¿<¿0.05). Silver deposition on titanium surface did not show improved results in terms of biofilm adhesion and cellular viability when compared to its corresponding non-coated surface. The total amount of bacterial biofilm did not significantly differ between groups (p¿>¿0.05). TESPSA was able to reduce biofilm adhesion and cellular viability. However, silver deposition on titanium surface seemed not to confer these antibacterial properties., Peer Reviewed, Postprint (published version)

The conventional tissue engineering is based on seeding of macroporous scaffold on its surface (“top–down” approach). The main limitation is poor cell viability in the middle of the scaffold due to poor diffusion of oxygen and nutrients and insufficient vascularization. Layer-by-Layer (LBL) bioassembly is based on “bottom–up” approach, which considers assembly of small cellularized blocks. The aim of this work was to evaluate proliferation and differentiation of human bone marrow stromal cells (HBMSCs) and endothelial progenitor cells (EPCs) in two and three dimensions (2D, 3D) using a LBL assembly of polylactic acid (PLA) scaffolds fabricated by 3D printing. 2D experiments have shown maintain of cell viability on PLA, especially when a co-cuture system was used, as well as adequate morphology of seeded cells. Early osteoblastic and endothelial differentiations were observed and cell proliferation was increased after 7 days of culture. In 3D, cell migration was observed between layers of LBL constructs, as well as an osteoblastic differentiation. These results indicate that LBL assembly of PLA layers could be suitable for BTE, in order to promote homogenous cell distribution inside the scaffold and gene expression specific to the cells implanted in the case of co-culture system., Postprint (author's final draft)

Intervertebral implants should be designed with low load requirements, high friction coefficient and low elastic modulus in order to avoid the stress shielding effect on bone. Furthermore, the presence of a highly interconnected porous structure allows stimulating bone in-growth and enhancing implant-bone fixation. The aim of this study was to obtain bioactive porous titanium implants with highly interconnected pores with a total porosity of approximately 57¿%. Porous Titanium implants were produced by powder sintering route using the space holder technique with a binder phase and were then evaluated in an in vivo study. The size of the interconnection diameter between the macropores was about 210¿µm in order to guarantee bone in-growth through osteblastic cell penetration. Surface roughness and mechanical properties were analyzed. Stiffness was reduced as a result of the powder sintering technique which allowed the formation of a porous network. Compression and fatigue tests exhibited suitable properties in order to guarantee a proper compromise between mechanical properties and pore interconnectivity. Bioactivity treatment effect in novel sintered porous titanium materials was studied by thermo-chemical treatments and were compared with the same material that had undergone different bioactive treatments. Bioactive thermo-chemical treatment was confirmed by the presence of sodium titanates on the surface of the implants as well as inside the porous network. Raman spectroscopy results suggested that the identified titanate structures would enhance in vivo apatite formation by promoting ion exchange for the apatite formation process. In vivo results demonstrated that the bioactive titanium achieved over 75¿% tissue colonization compared to the 40¿% value for the untreated titanium., Peer Reviewed, Postprint (published version)

The aim of this study was to increase understanding of the mechanism and dominant drivers influencing phase separation during ram extrusion of calcium phosphate (CaP) paste for orthopaedic applications. The liquid content of extrudate was determined, and the flow of liquid and powder phases within the syringe barrel during extrusion were observed, subject to various extrusion parameters. Increasing the initial liquid-to-powder mass ratio, LPR, (0.4–0.45), plunger rate (5–20 mm/min), and tapering the barrel exit (45°–90°) significantly reduced the extent of phase separation. Phase separation values ranged from (6.22 ± 0.69 to 18.94 ± 0.69 %). However altering needle geometry had no significant effect on phase separation. From powder tracing and liquid content determination, static zones of powder and a non-uniform liquid distribution was observed within the barrel. Measurements of extrudate and paste LPR within the barrel indicated that extrudate LPR remained constant during extrusion, while LPR of paste within the barrel decreased steadily. These observations indicate the mechanism of phase separation was located within the syringe barrel. Therefore phase separation can be attributed to either; (1) the liquid being forced downstream by an increase in pore pressure as a result of powder consolidation due to the pressure exerted by the plunger or (2) the liquid being drawn from paste within the barrel, due to suction, driven by dilation of the solids matrix at the barrel exit. Differentiating between these two mechanisms is difficult; however results obtained suggest that suction is the dominant phase separation mechanism occurring during extrusion of CaP paste., Peer Reviewed, Postprint (author's final draft)

The aim of this paper is to analyze the influence of the nature of the orthodontic archwires on the friction coefficient and wear rate against materials used commonly as brackets (Ti–6Al–4V and 316L Stainless Steel). The mate- rials selected as orthodontic archwires were ASI304 stainless steel, NiTi, Ti, TiMo and NiTiCu. The array archwire’s materials selected presented very similar roughness but different hardness. Materials were chosen from lower and higher hardness degrees than that of the brackets. Wear tests were carried out at in artificial saliva at 37 C. Results show a linear relationship between the hardness of the materials and the friction coefficients. The material that showed lower wear rate was the ASI304 stainless steel. To prevent wear, the wire and the brackets have high hardness values and in the same order of magnitude., Peer Reviewed, Postprint (published version)

The aim of this work was to study the effect of UHMWPE crosslinking on wear performance. Differently treated UHMWPEs were studied by means of unidirectional and multidirectional wear tests. Unidirectional tests simulate total knee replacement and multidirectional tests simulate total hip replacement movements. The samples tested were observed by optical and scanning electron microscopy in order to determine wear mechanisms that explain the dif-ferent results obtained in the uni- and multidirectional wear tests performed., Postprint (published version)

Different manufacturing processes of Ni–Ti archwires respond differently to corrosion due to the surface conditions involved. In this study, several topographical features and their influence upon fluoride corrosion were studied. Four topographies (smooth, dimple, scratch, and crack) according to the main surface defect were characterized (n = 40). Static corrosion tests were performed in artificial saliva with fluorated prophylactic gel (12500 ppm) for 28 days. The surface was characterized by SEM and laser confocal microscopy. Standard electrochemical corrosion (open circuit potential, corrosion potential and corrosion current density) was performed. Statistical analysis was carried out using the ANOVA test (a B 0.05). An increase was observed in the surface defects and/or roughness of the cracked and scratched surfaces. These defects produced an important increase in corrosion behavior. The best surfaces for the orthodontic archwires were the smooth and dimpled surfaces, respectively. The increase in defects was independent of roughness. Manufacturing processes that produce surface cracks should be avoided in orthodontic applications., Peer Reviewed, Postprint (published version)

Dental implant failure is commonly associated to dental plaque formation. This problem starts with bacterial colonization on implant surface upon implantation. Early colonizers (such as Streptococcus sanguinis) play a key role on that process, because they attach directly to the surface and facilitate adhesion of later colonizers. Surface treatments have been focused to improve osseointegration, where shot-blasting is one of the most used. However the effects on bacterial adhesion on that sort of surfaces have not been elucidated at all. A methodological procedure to test bacterial adherence to titanium shot-blasted surfaces (alumina and silicon carbide) by quantifying bacterial detached cells per area unit, was performed. In parallel, the surface properties of samples (i.e., roughness and surface energy), were analyzed in order to assess the relationship between surface treatment and bacterial adhesion. Rather than roughness, surface energy correlated to physicochemical properties of shot-blasted particles appears as critical factors for S. sanguinis adherence to titanium surfaces., Peer Reviewed, Postprint (published version)

Wear tests were carried out to study the effect of various counterface materials in the wear behaviour of Ultra High Molecular Weight Polyethylene (UHMWPE). The materials used as counterfaces were based on varieties of CoCrMo: 1) forged (hand-polished) CoCrMo, 2) forged (mass-finished) CoCrMo, and 3) cast (mass-finished) CoCrMo. Addi-tionally, two coatings were proposed: 1) a CoCrMo coating applied to the forged CoCrMo alloy by means of physical vapour deposition (PVD), and 2) a ZrO2 coating applied to the forged CoCrMo alloy by means of plasma-assisted chemical vapour deposition (PACVD). The reciprocating pin-on-flat (RPOF) de-vice for pin-on-disk wear testing was used for this study. The worn surfaces were observed using optical, atomic force and scanning electron microscopes., Peer Reviewed, Postprint (published version)

Wear tests were carried out to study the effect of the hardness and roughness with various counterface materials on UHMWPE wear behaviour. The materials used as counterfaces were based on varieties of CoCrMo: 1) forged (hand-polished) CoCrMo, 2) forged (mass-finished) CoCrMo, and 3) cast (mass-finished) CoCrMo. Additionally, two coatings were proposed: 1) a CoCrMo coating applied to the forged CoCrMo alloy by means of physical vapour deposition (PVD), and 2) a ZrO2 coating applied to the forged CoCrMo alloy by means of plasma-assisted chemical vapour deposition (PACVD). The reciprocating pin-on-flat (RPOF) device for pin-on-disk wear testing was used for this study. The worn surfaces were observed using optical, atomic force and scanning electron microscopes., Peer Reviewed, Postprint (published version)

In oral orthodontic treatments, achievement of a good adhesion between brackets and teeth surfaces is essential. One way to increase adhesion is to apply a surface treatment of teeth facing surfaces through the projection of abrasive particles to produce a surface roughness which improves adhesion of the bracket to the tooth, because of the significantly increased contact between the two surfaces. The effect on adhesion through the use of this technique in different types of brackets, as well as through the use of different blasting particles, however, is yet not well described. In this study we have included three types of brackets which are commonly used in orthodontic therapies (two of them a mesh-type and the third one a micro-milled type) with a contact surface area of 11.16, 8.85 and 6.89 mm2 respectively. These brackets were used combined with a sandblasting treatment with two different types of abrasive particles, alumina (Al2O3) and silicon carbide (SiC) and applied to natural teeth in vitro. The abrasive particles used are bio-compatible and usually used in achieving increased roughness for improved adherence in biomedical materials. Sandblasting was performed at 2 bars for 2 s; three particle sizes were used: 80, 200 and 600 lm. Non-blasted samples were used as control. Each of the pieces were cemented to natural teeth with a selfcuring composite. Samples were stored in physiologic serum at 5 C temperature. Tensile tests were performed with a universal testing machine. Brackets treated with sandblasted particles were measured to have an increased adhesion as compared to the control sample. The highest bond strength was measured for samples sandblasted with alumina particles of 80 and 200 lm combined with micromilled brackets. The recorded stresses did not exceed the tensile strength of tooth enamel., Peer Reviewed, Postprint (published version)

In this work, we analysed 56 clinically failed and retrieved implants by means of scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and histological studies. The surface contamination was compared to that of unused control implants and with that of the same implants after cleaning in a basic medium. The surfaces of the unused implants presented considerable contamination. In particular, high levels of carbon were detected. The nature of this C was elucidated by XPS analysis of the lubricant used in the machining process. The same contamination was observed in the retrieved implants. Histological studies were carried out by means of light microscopy. Fibrosis and granulomatous lesions were detected in the tissues. XPS analysis indicated the presence of traces of other elements (Na, Ca, Zn, S, F, etc.) that were not related to impurities in cpTi. We examined a cleaning process in a basic medium that eliminates the organic components of the implant surfaces. The cleaned implants were implanted in the patients and the results were excellent. None of the implants failed in following 7 months., Postprint (published version)