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.

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.

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.

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.

Effects of negatively and positively charged Ti metal surfaces on ceramic coating adhesion and cell response.

This manuscript reports an evaluation of the effects of simple chemical-heat treatments on the deposition of different ceramic coatings, i.e., TiO2, CaTiO3 and CaP, on commercially pure titanium (cp-Ti) and Ti6Al4V and the influence of the coatings on cells interaction with the surfaces. The ceramic materials were prepared by the sol-gel method and the coating adhesion was analyzed by pull-off bending tests. The wettability of positively or negatively charged surfaces was characterized by contact angle measurements, which also enabled the calculation of the surface free energy through the polar-apolar liquids approach. Both acid and alkaline treatments activated the cp-Ti, whereas Ti6Al4V was only activated by the alkaline treatment. Such treatment led to increased hydrophilicity with inhibition of the fibroblastic response on Ti6Al4V. On the other hand, osteoblastic cells adhered to and proliferated on the positively and negatively charged surfaces. The maximum adhesion strength (~ 3400 N) was obtained with a negative Ti6Al4V-CaTiO3-CaP multilayer surface.

Achieving surface chemical and morphologic alterations on tantalum by plasma electrolytic oxidation.

BACKGROUND: Search for materials that may either replace titanium dental implants or constitute an alternative as a new dental implant material has been widely studied. As well, the search for optimum biocompatible metal surfaces remains crucial. So, the aim of this work is to develop an oxidized surface layer on tantalum using plasma electrolytic oxidation (PEO) similar to those existing on oral implants been marketed today. METHODS: Cleaned tantalum samples were divided into group 1 (control) and groups 2, 3, and 4 (treated by PEO for 1, 3, and 5 min, respectively). An electrolytic solution diluted in 1-L deionized water was used for the anodizing process. Then, samples were washed with anhydrous ethyl alcohol and dried in the open air. For complete anodic treatment disposal, the samples were immersed in acetone altogether, taken to the ultrasonic tank for 10 min, washed again in distilled water, and finally air-dried. For the scanning electron microscopy (SEM) analysis, all samples were previously coated with gold; the salt deposition analysis was conducted with an energy-dispersive X-ray spectroscopy (EDS) system integrated with the SEM unit. RESULTS: SEM images confirmed the changes on tantalum strips surface according to different exposure times while EDS analysis confirmed increased salt deposition as exposure time to the anodizing process also increased. CONCLUSIONS: PEO was able to produce both surface alteration and salt deposition on tantalum strips similar to those existing on oral implants been marketed today.

Biomimetic coatings enhance tribocorrosion behavior and cell responses of commercially pure titanium surfaces.

Biofunctionalized surfaces for implants are currently receiving much attention in the health care sector. Our aims were (1) to create bioactive Ti-coatings doped with Ca, P, Si, and Ag produced by microarc oxidation (MAO) to improve the surface properties of biomedical implants, (2) to investigate the TiO2 layer stability under wear and corrosion, and (3) to evaluate human mesenchymal stem cells (hMSCs) responses cultured on the modified surfaces. Tribocorrosion and cell experiments were performed following the MAO treatment. Samples were divided as a function of different Ca/P concentrations and treatment duration. Higher Ca concentration produced larger porous and harder coatings compared to the untreated group (p < 0.001), due to the presence of rutile structure. Free potentials experiments showed lower drops (-0.6 V) and higher coating lifetime during sliding for higher Ca concentration, whereas lower concentrations presented similar drops (-0.8 V) compared to an untreated group wherein the drop occurred immediately after the sliding started. MAO-treated surfaces improved the matrix formation and osteogenic gene expression levels of hMSCs. Higher Ca/P ratios and the addition of Ag nanoparticles into the oxide layer presented better surface properties, tribocorrosive behavior, and cell responses. MAO is a promising technique to enhance the biological, chemical, and mechanical properties of dental implant surfaces.

Layer-by-layer assembly of functionalized reduced graphene oxide for direct electrochemistry and glucose detection.

We report an electrochemical glucose biosensor made with layer-by-layer (LbL) films of functionalized reduced graphene oxide (rGO) and glucose oxidase (GOx). The LbL assembly using positively and negatively charged rGO multilayers represents a simple approach to develop enzymatic biosensors. The electron transport properties of graphene were combined with the specificity provided by the enzyme. rGO was obtained and functionalized using chemical methods, being positively charged with poly(diallyldimethylammonium chloride) to form GPDDA, and negatively charged with poly(styrene sulfonate) to form GPSS. Stable aqueous dispersions of GPDDA and GPSS are easily obtained, enabling the growth of LbL films on various solid supports. The use of graphene in the immobilization of GOx promoted Direct Electron Transfer, which was evaluated by Cyclic Voltammetry. Amperometric measurements indicated a detection limit of 13.4µmol·L(-1) and sensitivity of 2.47µA·cm(-2)·mmol(-1)·L for glucose with the (GPDDA/GPSS)1/(GPDDA/GOx)2 architecture, whose thickness was 19.80±0.28nm, as determined by Surface Plasmon Resonance (SPR). The sensor may be useful for clinical analysis since glucose could be detected even in the presence of typical interfering agents and in real samples of a lactose-free milk and an electrolyte solution to prevent dehydration.

Production of a biofunctional titanium surface using plasma electrolytic oxidation and glow-discharge plasma for biomedical applications.

In this study, the authors tested the hypotheses that plasma electrolytic oxidation (PEO) and glow-discharge plasma (GDP) would improve the electrochemical, physical, chemical, and mechanical properties of commercially pure titanium (cpTi), and that blood protein adsorption on plasma-treated surfaces would increase. Machined and sandblasted surfaces were used as controls. Standard electrochemical tests were conducted in artificial saliva (pHs of 3.0, 6.5, and 9.0) and simulated body fluid. Surfaces were characterized by scanning electron microscopy, energy-dispersive spectroscopy, x-ray photoelectron spectroscopy, atomic force microscopy, x-ray diffraction, profilometry, Vickers microhardness, and surface energy. For biological assay, the adsorption of blood serum proteins (i.e., albumin, fibrinogen, and fibronectin) was tested. Higher values of polarization resistance and lower values of capacitance were noted for the PEO and GDP groups (p < 0.05). Acidic artificial saliva reduced the corrosion resistance of cpTi (p < 0.05). PEO and GDP treatments improved the surface properties by enrichment of the surface chemistry with bioactive elements and increased surface energy. PEO produced a porous oxide layer (5-µm thickness), while GDP created a very thin oxide layer (0.76-µm thickness). For the PEO group, the authors noted rutile and anatase crystalline structures that may be responsible for the corrosion barrier improvement and increased microhardness values. Plasma treatments were able to enhance the surface properties and electrochemical stability of titanium, while increasing protein adsorption levels.

Incorporation of Ca, P, and Si on bioactive coatings produced by plasma electrolytic oxidation: The role of electrolyte concentration and treatment duration.

The objectives of the present study were to produce bioactive coatings in solutions containing Ca, P, and Si by plasma electrolytic oxidation (PEO) on commercially pure titanium, to investigate the influence of different electrolytes concentration and treatment duration on the produced anodic films and to evaluate biocompatibility properties. The anodic films were characterized using scanning electron microscopy, energy-dispersive spectroscopy, atomic force microscopy, and x-ray diffraction and x-ray photoelectron spectroscopies. The surface energy and roughness were also evaluated. PEO process parameters influenced the crystalline structure formation and surface topography of the anodic films. Higher Ca content produced larger porous (volcanolike appearance) and thicker oxide layers when compared to the lower content. Treatment duration did not produce any topography difference. The treatment modified the surface chemistry, producing an enriched oxide layer with bioactive elements in the form of phosphate compounds, which may be responsible for mimicking bone surface. In addition, a rough surface with increased surface energy was generated. Optimal spreading and proliferation of human mesenchymal stem cells was achieved by PEO treatment, demonstrating excellent biocompatibility of the surface. The main finding is that the biofunctionalization with higher Ca/P on Ti-surface can improve surface features, potentially considered as a candidate for dental implants.

Adherence in vitro of Candida albicans to plasma treated acrylic resin. Effect of plasma parameters, surface roughness and salivary pellicle.

UNLABELLED: The adhesion of Candida albicans to surfaces is the prerequisite for occurrence of denture stomatitis. OBJECTIVE: Hence, this study investigated if surface modifications with plasma treatments could reduce the adherence of C. albicans to a denture base resin. METHODS: Specimens (n=180) with roughened and smooth surfaces were made and divided into five groups: control-specimens were left untreated; experimental groups-specimens were submitted to plasma treatments to obtain surfaces with different hydrophobicity (Ar/50W; ArO2/70W; AAt/130W) or incorporation of fluorine (Ar/SF(6)70W). Contact angle measurements were performed immediately after the treatments and after immersion in water for 48h. For each group, half of the specimens were incubated with saliva prior to the adhesion assay. The number of adherent yeasts was evaluated by XTT reduction method. RESULTS: For the experimental groups, there was significant change in the mean contact angle after 48h of immersion in water. Groups ArO2/70W and ArSF6/70W showed significantly lower absorbance readings than the other groups, regardless the presence or absence of saliva and surface roughness. CONCLUSIONS: Results demonstrated that ArO2/70W and ArSF6/70W plasma treatments showed promising potential for reducing the adherence of C. albicans to denture base resins.