Boosting Titanium Surfaces with Positive Charges: Newly Developed Cationic Coating Combines Anticorrosive and Bactericidal Properties for Implant Application.

Along with poor implant-bone integration, peri-implant diseases are the major causes of implant failure. Although such diseases are primarily triggered by biofilm accumulation, a complex inflammatory process in response to corrosive-related metallic ions/debris has also been recognized as a risk factor. In this regard, by boosting the titanium (Ti) surface with silane-based positive charges, cationic coatings have gained increasing attention due to their ability to kill pathogens and may be favorable for corrosion resistance. Nevertheless, the development of a cationic coating that combines such properties in addition to having a favorable topography for implant osseointegration is lacking. Because introducing hydroxyl (-OH) groups to Ti is essential to increase chemical bonds with silane, Ti pretreatment is of utmost importance to achieve such polarization. In this study, plasma electrolytic oxidation (PEO) was investigated as a new route to pretreat Ti with OH groups while providing favorable properties for implant application compared with traditional hydrothermal treatment (HT). To produce bactericidal and corrosion-resistant cationic coatings, after pretreatment with PEO or HT (Step 1), surface silanization was subsequently performed via immersion-based functionalization with 3-aminopropyltriethoxysilane (APTES) (Step 2). In the end, five groups were assessed: untreated Ti (Ti), HT, PEO, HT+APTES, and PEO+APTES. PEO created a porous surface with increased roughness and better mechanical and tribological properties compared with HT and Ti. The introduction of -OH groups by HT and PEO was confirmed by Fourier transform infrared spectroscopy and the increase in wettability producing superhydrophilic surfaces. After silanization, the surfaces were polarized to hydrophobic ones, and an increase in the amine functional group was observed by X-ray photoelectron spectroscopy, demonstrating a considerable amount of positive ions. Such protonation may explain the enhanced corrosion resistance and dead bacteria (Streptococcus aureus and Escherichia coli) found for PEO+APTES. All groups presented noncytotoxic properties with similar blood plasma protein adsorption capacity vs the Ti control. Our findings provide new insights into developing next-generation cationic coatings by suggesting that a tailorable porous and oxide coating produced by PEO has promise in designing enhanced cationic surfaces targeting biomedical and dental implant applications.

Effect of Plasma Excitation Power on the SiOxCyHz/TiOx Nanocomposite.

Titanium dioxide has attracted a great deal of attention in the field of environmental purification due to its photocatalytic activity under ultraviolet light. Photocatalytic efficiency and the energy required to initiate the process remain the drawbacks that hinder the widespread adoption of the process. Consistently with this, it is proposed here the polymerization of hexamethyldisiloxane fragments simultaneously to TiO2 sputtering for the production of thin films in low-pressure plasma. The effect of plasma excitation power on the molecular structure and chemical composition of the films was evaluated by infrared spectroscopy. Wettability and surface energy were assessed by a sessile drop technique, using deionized water and diiodomethane. The morphology and elemental composition of the films were determined using scanning electron microscopy and energy dispersive spectroscopy, respectively. The thickness and roughness of the resulting films were measured using profilometry. Organosilicon-to-silica films, with different properties, were deposited by combining both deposition processes. Titanium was detected from the structures fabricated by the hybrid method. It has been observed that the proportion of titanium and particles incorporated into silicon-based matrices depends on the plasma excitation power. In general, a decrease in film thickness with increasing power has been observed. The presence of Ti in the plasma atmosphere alters the plasma deposition mechanism, affecting film deposition rate, roughness, and wettability. An interpretation of the excitation power dependence on the plasma activation level and sputtering yield is proposed. The methodology developed here will encourage researchers to create TiO2 films on a range of substrates for their prospective use as sensor electrodes, water and air purification systems, and biocompatible materials.

The race for the optimal antimicrobial surface: perspectives and challenges related to plasma electrolytic oxidation coating for titanium-based implants.

Plasma electrolytic oxidation (PEO) is a low-cost, structurally reliable, and environmentally friendly surface modification method for orthopedic and dental implants. This technique is successful for the formation of porous, corrosion-resistant, and bioactive coatings, besides introducing antimicrobial compounds easily. Given the increase in implant-related infections, antimicrobial PEO-treated surfaces have been widely proposed to surmount this public health concern. This review comprehensively discusses antimicrobial implant surfaces currently produced by PEO in terms of their in vitro and in vivo microbiological and biological properties. We present a critical [part I] and evidence-based [part II] review about the plethora of antimicrobial PEO-treated surfaces. The mechanism of microbial accumulation on implanted devices and the principles of PEO technology to ensure antimicrobial functionalization by one- or multi-step processes are outlined. Our systematic literature search showed that particular focus has been placed on the metallic and semi-metallic elements incorporated into PEO surfaces to facilitate antimicrobial properties, which are often dose-dependent, without leading to cytotoxicity in vitro. Meanwhile, there are concerns over the biocompatibility of PEO and its long-term antimicrobial effects in animal models. We clearly highlight the importance of using clinically relevant infection models and in vivo long-term assessments to guarantee the rational design of antimicrobial PEO-treated surfaces to identify the 'finish line' in the race for antimicrobial implant surfaces.

Copper source determines chemistry and topography of implant coatings to optimally couple cellular responses and antibacterial activity.

Implant-related infections at the early healing period are considered one of the main risk factors in implant failure. Designing coatings that control bacterial adhesion and have cell stimulatory behavior remains a challenging strategy for dental implants. Here, we used plasma electrolytic oxidation (PEO) to produce antimicrobial coatings on commercially pure titanium (cpTi) using bioactive elements (calcium and phosphorus) and different copper (Cu) sources: copper acetate (CuAc), copper sulfate (CuS), and copper oxide (CuO); coatings containing only Ca and P (CaP) served as controls. Cu sources drove differential physical and chemical surface features of PEO coatings, resulting in tailorable release kinetics with a sustained Cu ion release over 10 weeks. The antibacterial effects of Cu-containing coatings were roughness-dependent. CuAc coating exhibited optimal properties in terms of its hydrophilicity, pores density, and limited surface roughness, which provided the most robust antibacterial activity combined with appropriate responses of human primary stem cells and angiogenic cells. Our data indicate that Cu source selection largely determines the functionality of Cu-containing PEO coatings regarding their antibacterial efficacy and cytocompatibility.

Surface characterization of different surface treatments associations with plasma and bonding analysis of Y-TZP and the veneering ceramic.

OBJECTIVES: To characterize the surface of zirconia (Y-TZP) submitted to different surface treatments (with and without plasma associations) and to evaluate the shear bond strength (SBS) between veneering ceramic (VC) and Y-TZP after different aging methods. METHODS: 301 Y-TZP specimens were fabricated and distributed into 7 groups: C (control): no treatment; Al: airborne abrasion with 27 µm Al2O3 particle; L: liner; P: plasma; Al + L: airborne + liner; Al + P: airborne + plasma; P + L: plasma + liner. The Y-TZP surface was characterized by SEM, EDS, AFM, surface profilometry, surface-free energy (SFE), and XRD. SBS between Y-TZP and VC was verified after three aging protocols: initial, after hydrothermal aging (autoclave for 5 h), or thermal fatigue (30,000 baths - 5-55 °C). One- (profilometry, SFE) and two-way ANOVA (SBS), and Tukey's HSD test were used. RESULTS: For the plasma groups, a full globular surface coverage was observed (SEM, AFM). Si was found for Al, L, Al + L, and P + L. Roughness was lower for C, P, and Al + P. For SFE, the highest values were found when the liner was applied (>74.59 nm/Nm). The highest monoclinic content was observed for Al + L (6.96%) and Al + P (5.86%). For the initial period, Al and P + L presented the lowest SBS values (<5.85 MPa; P > 0.331). The highest SBS values were found for L, P, and P + L (hydrothermal aging) and for P, L, Al + L, and Al + P (thermal fatigue). SIGNIFICANCE: Changes in Y-TZP topography and the SBS with the VC were found, according to treatments performed. Plasma treatment improved SBS and did not cause phase transformation.

Is an anodizing coating associated to the photobiomodulation able to optimize bone healing in ovariectomized animal model?

This in vivo study investigated whether the bioactivity of anodizing coating, produced by plasma electrolytic oxidation (PEO), on mini-plate in femur fracture could be improved with the association of photobiomodulation (PBM) therapy. From the 20 ovariectomized Wistar female rats, 8 were used for model characterization, and the remaining 12 were divided into four groups according to the use of PBM therapy by diode laser (808 nm; power: 100 mW; energy: 6.0 J; energy density: 212 J/cm2; power density: 3.5 W/cm2) and the type of mini-plate surface (commercially pure titanium mini-plate -cpTi- and PEO-treated mini-plate) as follow: cpTi; PEO; cpTi/PBM; and PEO/PBM. After 60 days of surgery, fracture healing underwent microstructural, bone turnover, histometric, and histologic adjacent muscle analysis. Animals of groups with PEO and PBM showed greater fracture healing than cpTi control group under histometric and microstructural analysis (P < 0.05); however, bone turnover was just improved in PBM's groups (P < 0.05). there was no difference between cpTi and PEO without PBM (P > 0.05). Adjacent muscle analysis showed no metallic particles or muscle alterations in all groups. PEO and PBM are effective strategies for bone repair in fractures, however their association does not provide additional advantages.

Miniplates coated by plasma electrolytic oxidation improve bone healing of simulated femoral fractures on low bone mineral density rats.

The treatment of polytrauma patients represents a great challenge in the maxillofacial and orthopedic surgery fields. Therefore, this study tested the hypothesis that the use of a bioactive coating (by plasma electrolytic oxidation, PEO) on titanium microplates could improve the fracture healing of low bone mineral density (BMD) rats. Thirty female rats underwent bilateral ovariectomy surgery (OVX), and 35 rats underwent fake surgery (SHAM). Three months later, animals were subjected to femoral fracture simulation and were fixed with either non-coated (CONV) or coated (PEO) titanium miniplates. Eight weeks postoperatively, microplate/bone complexes were analyzed through computed microtomography, histometric, confocal microscopy, molecular, and biomechanical analysis. Bioactive elements (Ca and P) were incorporated on the PEO microplate and the surface was modified in a volcano-like structure. In the microCT analysis the OVX/PEO group had greater values for Tb.Th (bone trabecular thickness), Tb.Sp (separation of bone trabeculae) and Tb.N (number of trabeculae) parameters compared to the OVX/CONV group. According to histometric analysis, the OVX/PEO group showed significantly higher new bone formation than the OVX/CONV group (P < 0.05). For the fluorochrome area, the OVX groups (PEO and CONV) showed greater values for calcein precipitation (old bone) than alizarin red (new bone). Molecular results showed greater values for proteins related to the final phase of bone formation (P < 0.05) in the OVX/PEO group. The OVX/PEO group showed higher bone/miniplate system resilience compared to the others (P < 0.05). It was concluded that PEO coating optimizes bone healing on simulated femoral fractures in low bone mineral density rats. This sheds new light in the treatment of osteoporotic patients with bone fractures.

Thin Film Deposition by Atmospheric Pressure Dielectric Barrier Discharges Containing Eugenol: Discharge and Coating Characterizations.

Eugenol (4-Allyl-2-methoxyphenol) is the main constituent of clove oil. In addition to being widely used as a condiment, it has been recognized as a powerful bactericide. Owing to that, Eugenol has been used in several applications including odontology and as a conservative for food products. Aiming at the development of natural bactericide coatings, in this work, using an atmospheric pressure plasma in a dielectric barrier discharge (DBD) reactor Eugenol was deposited on stainless steel substrate, with argon as a carrier gas. The discharge power supply was a transformer at 14.4 kV peak-to-peak voltage and 60 Hz frequency. Operating with a gas flow rate at 4 L/min, the active power was around 1.2 W. The maximum plasma electron temperature of the plasma with monomers was about 1.5 eV, estimated by visible emission spectroscopy using a local thermodynamic equilibrium approach. The study also comprehended the analysis of the film structure, aging, and thermal stability using infrared reflectance spectroscopy, and its thicknesses and roughness by profilometry. The thickness of the films was in the range of 1000 to 2400 nm with a roughness of up to 800 nm with good adhesion on the substrate. The FTIR result shows a stable coating with a chemical structure similar to that of the monomer. Aging analysis showed that the film does not degrade, even after exposing the film for 120 days in ambient air and for 1.0 h under a high thermal UV-lamp.

Author Correction: Plasma Electrolytic Oxidation as a Feasible Surface Treatment for Biomedical Applications: an in vivo study.

An amendment to this paper has been published and can be accessed via a link at the top of the paper.

Synthesis of bioactive glass-based coating by plasma electrolytic oxidation: Untangling a new deposition pathway toward titanium implant surfaces.

HYPOTHESIS: Although bioactive glass (BG) particle coatings were previously developed by different methods, poor particle adhesion to surfaces and reduced biological effects because of glass crystallization have limited their biomedical applications. To overcome this problem, we have untangled, for the first time, plasma electrolytic oxidation (PEO) as a new pathway for the synthesis of bioactive glass-based coating (PEO-BG) on titanium (Ti) materials. EXPERIMENTS: Electrolyte solution with bioactive elements (Na2SiO3-5H2O, C4H6O4Ca, NaNO3, and C3H7Na2O6P) was used as a precursor source to obtain a 45S5 bioglass-like composition on a Ti surface by PEO. Subsequently, the PEO-BG coating was investigated with respect to its surface, mechanical, tribological, electrochemical, microbiological, and biological properties, compared with those of machined and sandblasted/acid-etched control surfaces. FINDINGS: PEO treatment produced a coating with complex surface topography, Ti crystalline phases, superhydrophilic status, chemical composition, and oxide layer similar to that of 45S5-BG (~45.0Si, 24.5 Ca, 24.5Na, 6.0P w/v%). PEO-BG enhanced Ti mechanical and tribological properties with higher corrosion resistance. Furthermore, PEO-BG had a positive influence in polymicrobial biofilms, by reducing pathogenic bacterial associated with biofilm-related infections. PEO-BG also showed higher adsorption of blood plasma proteins without cytotoxic effects on human cells, and thus may be considered a promising biocompatible approach for biomedical implants.

Atmospheric Pressure Plasma Chemical Vapor Deposition of Carvacrol Thin Films on Stainless Steel to Reduce the Formation of E. Coli and S. Aureus Biofilms.

In this paper, we have investigated the deposition of thin films from natural carvacrol extract using dielectric barrier discharge (DBD) plasma polymerization, aiming at the inhibition of bacteria adhesion and proliferation. The films deposited on stainless steel samples have been characterized by scanning electron microscopy, infrared reflectance-absorbance spectroscopy, profilometry, and contact angle measurements. Films with thicknesses ranging from 1.5 µm to 3.5 µm presented a chemical structure similar to that of carvacrol. While the formation of biofilm was observed on untreated samples, the coating completely inhibited the adhesion of E. coli and reduced the adhesion of S. aureus biofilm in more than 90%.

Plasma Electrolytic Oxidation as a Feasible Surface Treatment for Biomedical Applications: an in vivo study.

OBJECTIVES: In this in vivo animal study, we evaluated the effect of plasma electrolytic oxidation (PEO) coating on the topographic and biological parameters of implants installed in rats with induced osteoporosis and low-quality bones. MATERIALS AND METHODS: In total 44 Wistar rats (Rattus novergicus), 6 months old, were submitted to ovariectomy (OXV group) and dummy surgery (SHAM group). After 90 days, the ELISA test was performed and the ovariectomy effectiveness was confirmed. In each tibial metaphysis, an implant with PEO coating containing Ca2+ and P5+ molecules were installed, and the other tibia received an implant with SLA acid etching and blasting (AC) (control surface). After 42 days, 16 rats from each group were euthanized, their tibias were removed for histological and immunohistochemical analysis (OPG, RANKL, OC and TRAP), as well as reverse torque biomechanics. Data were submitted to One-way ANOVA or Kruskal-Wallis tests, followed by a Tukey post-test; P < 0.05. Histological analyses showed higher bone neoformation values among the members of the PEO group, SHAM and OVX groups. Immunohistochemical analysis demonstrated equilibrium in all groups when comparing surfaces for TRAP, OC and RANKL (P > 0.05), whereas OPG showed higher PEO labeling in the OVX group (P < 0.05). Biomechanical analysis showed higher reverse torque values (N.cm) for PEO, irrespective of whether they were OVX or SHAM groups (P < 0.05). CONCLUSION: The results indicated that the PEO texturing method favored bone formation and showed higher bone maturation levels during later periods in osteoporotic rats.

Comparison between Plasma Electrolytic Oxidation Coating and Sandblasted Acid-Etched Surface Treatment: Histometric, Tomographic, and Expression Levels of Osteoclastogenic Factors in Osteoporotic Rats.

Plasma electrolytic oxidation (PEO) has been a promising surface coating with better mechanical and antimicrobial parameters comparing to conventional treatment surfaces. This study evaluated the peri-implant bone repair using (PEO) surface coatings compared with sandblasted acid (SLA) treatment. For this purpose, 44 Wistar rats were ovariectomized (OVX-22 animals) or underwent simulated surgery (SS-22 animals) and received implants in the tibia with each of the surface coatings. The peri-implant bone subsequently underwent molecular, microstructural, bone turnover, and histometric analysis. Real-time PCR showed a higher expression of osteoprotegerin (OPG), receptor activator of nuclear kappa-B ligand (RANKL), and osteocalcin (OC) proteins in the SLA/OVX and PEO/SS groups (p < 0.05). Computed microtomography, confocal microscopy, and histometry showed similarity between the PEO and SLA surfaces, with a trend toward the superiority of PEO in OVX animals. Thus, PEO surfaces were shown to be promising for enhancing peri-implant bone repair in ovariectomized rats.

UV-photofunctionalization of a biomimetic coating for dental implants application.

Photofunctionalization mediated by ultraviolet (UV) rays changes the physico-chemical characteristics of titanium (Ti) and improves the biological activity of dental implants. However, the role of UV-mediated photofunctionalization of biofunctional Ti surfaces on the antimicrobial and photocatalytic activity remains unknown and was investigated in this study. Commercially pure titanium (cpTi) discs were divided into four groups: (1) machined samples without UV light application [cpTi UV-]; (2) plasma electrolytic oxidation (PEO) treated samples without UV light application [PEO UV-]; (3) machined samples with UV light application [cpTi UV+]; and (4) PEO-treated samples with UV light application [PEO UV+]. The surfaces were characterized according to their morphology, roughness, crystalline phase, chemical composition and wettability. The photocatalytic activity and proteins adsorption were measured. For the microbiological assay, Streptococcus sanguinis was grown on the disc surfaces for 1 h and 6 h, and the colony forming units and bacterial organization were evaluated. In addition, to confirm the non-cytotoxic effect of PEO UV +, human gingival fibroblast (HGF) cells were cultured in a monolayer onto each material surface and the cells viability and proliferation evaluated by a fluorescent cell staining method. PEO treatment increased the Ti surface roughness and wettability (p < 0.05). Photofunctionalization reduced the hydrocarbon concentration and enhanced human blood plasma proteins and albumin adsorption mainly for the PEO-treated surface (p < 0.05). PEO UV+ also maintained higher wettability values for a longer period and provided microbial reduction at 1 h of bacterial adhesion (p = 0.012 vs. PEO UV-). Photofunctionalization did not increase the photocatalytic activity of Ti (p > 0.05). Confocal microscopy analyses demonstrated that PEO UV+ had no cell damage effect on HGF cells growth even after 24 h of incubation. The photofunctionalization of a biofunctional PEO coating seems to be a promising alternative for dental implants as it increases blood plasma proteins adsorption, reduces initial bacterial adhesion and presents no cytotoxicity effect.

Role of the Plasma Activation Degree on Densification of Organosilicon Films.

The possibility of controlling the density of organosilicon films was investigated by tuning the plasma activation degree without providing extra energy to the structure, as usually reported in the literature. For this purpose, thin films were deposited in plasmas fed with hexamethyldisiloxane/Ar mixtures at a total pressure of 9.5 Pa. The power of the radiofrequency excitation signal, P, ranged from 50 to 300 W to alter the average energy of the plasma species while the electrical configuration was chosen to avoid direct ion bombardment of the growing films. In this way, it was possible to evaluate the effect of P on the film properties. Thickness and deposition rate were derived from profilometry data. X-ray energy dispersive and infrared spectroscopies were, respectively, applied to analyze the chemical composition and molecular structure of the layers. Surface topography and roughness were determined by atomic force microscopy while nanoindentation was used to evaluate the mechanical properties of the films. From electrochemical impedance spectroscopy the total resistance to the flow of electrolyte species was derived. The main alteration observed in the structure with changing P is related to the proportion of the methyl functional which remains connected to the Si backbone. Chain crosslinking and film density are affected by this structural modification induced by homogeneous and heterogeneous plasma reactions. The density increase resulted in a film with hardness comparable to that of the silica and more resistant to the permeation of oxidative species, but preserving the organosilicon nature of the structure.

Visible-Light-Induced Photocatalytic and Antibacterial Activity of TiO2 Codoped with Nitrogen and Bismuth: New Perspectives to Control Implant-Biofilm-Related Diseases.

Biofilm-associated diseases are one of the main causes of implant failure. Currently, the development of implant surface treatment goes beyond the osseointegration process and focuses on the creation of surfaces with antimicrobial action and with the possibility to be re-activated (i.e., light source activation). Titanium dioxide (TiO2), an excellent photocatalyst used for photocatalytic antibacterial applications, could be a great alternative, but its efficiency is limited to the ultraviolet (UV) range of the electromagnetic spectrum. Since UV radiation has carcinogenic potential, we created a functional TiO2 coating codoped with nitrogen and bismuth via the plasma electrolytic oxidation (PEO) of titanium to achieve an antibacterial effect under visible light with re-activation potential. A complex surface topography was demonstrated by scanning electron microscopy and three-dimensional confocal laser scanning microscopy. Additionally, PEO-treated surfaces showed greater hydrophilicity and albumin adsorption compared to control, untreated titanium. Bismuth incorporation shifted the band gap of TiO2 to the visible region and facilitated higher degradation of methyl orange (MO) in the dark, with a greater reduction in the concentration of MO after visible-light irradiation even after 72 h of aging. These results were consistent with the in vitro antibacterial effect, where samples with nitrogen and bismuth in their composition showed the greatest bacterial reduction after 24 h of dual-species biofilm formation ( Streptococcus sanguinis and Actinomyces naeslundii) in darkness with a superior effect at 30 min of visible-light irradiation. In addition, such a coating presents reusable photocatalytic potential and good biocompatibility by presenting a noncytotoxicity effect on human gingival fibroblast cells. Therefore, nitrogen and bismuth incorporation into TiO2 via PEO can be considered a promising alternative for dental implant application with antibacterial properties in darkness, with a stronger effect after visible-light application.

Can Nonthermal Plasma Improve the Adhesion between Acrylic Resin for Ocular Prostheses and Silicone-Based Relining Material?

PURPOSE: To investigate the influence of nonthermal plasma (NTP) treatment on the tensile bond strength between heat-polymerized acrylic resin for ocular prostheses and silicone reliner, with and without the use of an adhesive primer. MATERIALS AND METHODS: One-hundred and sixty-four acrylic resin specimens were fabricated and randomly distributed into four groups according to the type of surface treatment: Sofreliner Primer, NTP, Sofreliner Primer + NTP, and NTP + Sofreliner Primer. Two specimens interposed with relining material (Sofreliner) formed one test sample to perform the tensile bond strength tests, before (initial) and after storage (final) in saline solution (37°C, 90 days, n = 10). Surface characterization was performed by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The failure type was classified as cohesive, adhesive, or mixed. The data were analyzed statistically using the two-way ANOVA and Tukey test, as well as the chi-squared test (α = 0.05), Bonferroni correction (α = 0.005), and Spearman correlation coefficient (α = 0.05). RESULTS: The SEM and EDS analyses showed the presence of a thin, homogenous organic film in the groups treated with NTP. The NTP + Sofreliner Primer group presented the largest bond strength mean values in the initial period (p < 0.05). Sofreliner Primer and NTP + Sofreliner Primer groups presented the first and second largest tensile bond strength mean values in the final period (p < 0.05), respectively. NTP + Sofreliner Primer group also had the largest number of cohesive (70%, initial) and mixed (90%, final) failures. CONCLUSIONS: The NTP treatment performed before the primer application enhanced the bond between the acrylic resin ocular prosthesis and the Sofreliner silicone-based reliner, even after 90 days of immersion in saline solution.

Characterization of chemically treated Ti-Zr system alloys for dental implant application.

Materials and surfaces developed for dental implants need to withstand degradation processes that take place in the oral cavity. Therefore, the aim of the study was to develop and evaluate the topographical, mechanical, chemical, electrochemical and biological properties of Ti-xZr alloys (x = 5, 10, and 15 wt%) with two surface features (machined and double acid etched). Commercially pure titanium (cpTi) and Ti-6Al-4V alloy were used as controls. Surface characterization was performed using dispersive energy spectroscopy, X-ray diffraction, scanning electron microscopy, atomic force microscopy, profilometry and surface energy. The mechanical properties were assessed using Vickers microhardness, elastic modulus and stiffness. The electrochemical behavior analysis was conducted in a body fluid solution (pH 7.4). In addition, MC3T3-E1 cells were used to determine the impact of material and surface treatment on cell morphology by SEM analysis. Data were analyzed by two-way ANOVA and Bonferroni test (α = 0.05). Ti-Zr alloys showed lower surface roughness, elastic modulus and stiffness, as well as higher hardness and surface energy when compared to cpTi. Ti-Zr system increased the polarization resistance values and significantly decreased the capacitance, corrosion current density (icorr), and passivation current density (ipass) values. The acid treatment increased the resistance and corrosion potential of the oxide layer. SEM data analysis demonstrated that Ti-Zr alloys displayed normal cell attachment/spreading and slightly changed cell morphology in the double etched surface. In conclusion, Zr addition and surface treatment altered surface, mechanical, biological and electrochemical properties of Ti material.

Characterisation of a new plasma-enhanced film to improve shear bond strength between zirconia and veneering ceramic.

The aim of this study was to develop and characterise a new plasma-enhanced chemical vapor deposition (PECVD) film for improving shear bond strength (SBS) between yttria-stabilised tetragonal zirconia (Y-TZP) and veneering ceramic. In total, 192 Y-TZP samples (13 × 5.4 × 5 mm) were divided into 6 groups: control - no treatment (C), airborne-particle abrasion with 27 µm aluminum oxide particles (Al27), 110 µm aluminum oxide particles (Al110), and 250 µm aluminum oxide particles (Al250), application of liner for zirconia (L) and the PECVD film application (P). The Y-TZP surface was characterised by means of Scanning Electronic Microscopy (SEM), Energy-dispersive Spectroscopy (EDS), atomic force microscopy (AFM), surface profilometry and surface-free energy (SFE). SBS between Y-TZP and veneering ceramic was tested before and after thermocycling (20,000 cycles of 5 and 55 °C), and failure mode was also evaluated. Data were analysed by ANOVA and Tukey's HSD test (α = 0.05). Data analysis showed that PECVD film had no effect on surface roughness of Y-TZP (p > 0.05 vs control), whilst the other groups presented higher roughness values (p < 0.05). All treatments increased SFE, except the Al27 group. The highest SBS was presented by the P group (p < 0.05), and values were similar to those of the Al27 group (p = 0.107). Mixed failures were prevalent in all groups, and premature failures were found only in Al groups after thermocycling. Whilst PECVD treatment did not affect Y-TZP surface roughness, high SBS between Y-TZP and the veneering layer was observed. Therefore, PECVD treatment is a promising alternative to improve the performance of bi-layer zirconia-based restorations.

Effect of nonthermal plasma on the properties of a resinous liner submitted to aging.

STATEMENT OF PROBLEM: The properties, such as softness and viscoelasticity, of a resinous reliner can deteriorate and extrinsic elements can become incorporated, making surface protection of the reliner material essential. PURPOSE: The purpose of this in vitro study was to evaluate the effect of low temperature plasma on Coe-Soft resinous reliner, submitted to aging in artificial saliva for up to 180 days. Sorption, solubility, Shore A hardness, surface energy, and topographic characteristics were analyzed by scanning electronic microscopy (SEM) and energy-dispersive spectroscopy (EDS). MATERIAL AND METHODS: Forty-four specimens were fabricated and distributed in 2 groups: nonplasma reliner (control group) and reliner with plasma (plasma group). The plasma was applied with a mixture of 70% hexamethyldisiloxane, 20% O, and 10% Ar. Total work pressure was maintained at a constant 20 Pa for 30 minutes of deposition. The specimens were analyzed before and after aging in an incubator with immersion in artificial saliva for 30, 90, and 180 days. The quantitative data were submitted to 2-way ANOVA and the Tukey test (α=.05), while qualitative data were compared visually. RESULTS: The control group presented lower Shore A hardness values only in the initial period, and surface energy increased with aging for both groups until 90 days. Greater sorption percentage values were encountered at 180 days in the plasma group. Greater solubility values were encountered in the control group in all periods. CONCLUSIONS: Plasma is an option for the protection of the material studied because the deposited film remained on the surface of the reliner material after aging.