Preparation and characterization of glass-ceramic materials in the BaO-Li2O-ZrO2-SiO2 system and their dependence on treatment temperatures

The preparation and characterization of transparent glass-ceramics in the composition of 30Li2O:5ZrO2:xBaO:(100-x) SiO2 with x = 0, 5, 10, 15, and 20 mol% are described. Glasses were melted in a platinum crucible at 1100°C for 2 h and then heat-treated at 900°C for 3 h. The characterizations were performed by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman and infrared spectroscopy, and scanning electron microscopy (SEM). The experimental results indicate that there was a structural change in the glass-ceramics as the BaO concentration in the mixture increased. In the XRD patterns of samples without heat treatment, only the halo was observed. After heat treatment, the appearance of the materials was verified by X-ray diffraction peaks. The reorganization of the amorphous solid was confirmed by Raman and IR spectroscopy along with XPS and SEM, with a more homogeneous phase formation being observed.

Sand-water slurry erosion of API 5L X65 pipe steel as quenched from intercritical temperature

The objective of this study was to analyze the erosion of API 5L X65 pipe steel whose microstructure consisted of ferrite and martensite obtained by quenching from intercritical temperature (770 °C). Jet impingement tests with sand-water slurry were used. The changes in mechanical properties, caused by heat treatment carried out, did not induce changes in either the mechanism or erosion resistance. The erosion rate increased with angle of attack until 30° and later decreased until 90°. The microtexture of the eroded surfaces, at angles of attack of 30° and 90°, were similar for both conditions and were composed of craters and platelets at several stages of evolution. The erosion mechanism was by extrusion with the forming and forging of platelets.

Influence of thermal treatments in the corrosion behaviour of HVOF Cr 3C2-NiCr coatings

Thermal spray coatings as Cr3C2-NiCr obtained by high velocity oxy-fuel spraying (HVOF) are mainly applied due to their behaviour against aggressive erosive-abrasive and corrosive atmospheres and their thermal stability at high temperatures [1]. In order to increase the corrosion protection that it offers to the substrate trying to close the interconnected pores, it is possible to apply a thermal treatment with the gun during the spraying of the coating. This treatment could be applied in different ways. One of these ways consists of spraying only a few layers of coating followed by thermal treatment and finally the spray of the rest of layers. This thermal treatment on spraying is studied related to the corrosion properties of the system. The study comprises the electrochemical characterisation of the system by open circuit potential (OC), polarisation resistance (Rp), cyclic voltammetry (CV) and impedance spectroscopy measurements (EIS). Optical and scanning electron microscopy characterisation (OM and SEM) of the top and cross-section of the system has been used in order to justify the electrochemical results.

Transparent Er3+-activated lead fluorogermanate glass ceramics

Transparent glass ceramics containing β-PbF2:Er 3+ nanocrystals were obtained through appropriate thermal treatments of a glass of molar composition 60PbGeO3-10PbF2-30CdF 2 doped with 0.5 mol% Er3+. Their optical properties, as well as upconversion processes among erbium ions in the glass and glass ceramic matrix were studied. From absorption spectra, Judd-Ofelt parameters and radiative transition rates for several excited levels were calculated. Emission spectra in the visible and NIR regions were collected, and stimulated emission cross sections were obtained by McCumber theory for the 4F 13/2→4I15/2 transition at 1.5 μm. Red and green upconversion emissions were measured in glass and glass ceramics upon excitation at 980 nm; lifetimes were measured in order to assess the upconversion mechanisms.

Effect of post-polymerization heat treatments on the cytotoxicity of two denture base acrylic resins

Introduction: Most denture base acrylic resins have polymethylmethacrylate in their composition. Several authors have discussed the polymerization process involved in converting monomer into polymer because adequate polymerization is a crucial factor in optimizing the physical properties and biocompatibility of denture base acrylic resins. To ensure the safety of these materials, in vitro cytotoxicity assays have been developed as preliminary screening tests to evaluate material biocompatibility. 3H-thymidine incorporation test, which measures the number of cells synthesizing DNA, is one of the biological assays suggested for cytotoxicity testing. Aim: The purpose of this study was to investigate, using 3H-thymidine incorporation test, the effect of microwave and water-bath post-polymerization heat treatments on the cytotoxicity of two denture base acrylic resins. Materials and Methods: Nine disc-shaped specimens (10 x 1 mm) of each denture base resin (Lucitone 550 and QC 20) were prepared according to the manufacturers' recommendations and stored in distilled water at 37°C for 48 h. The specimens were assigned to 3 groups: 1) post-polymerization in a microwave oven for 3 min at 500 W; 2) post-polymerization in water-bath at 55°C for 60 min; and 3) without post-polymerization. For preparation of eluates, 3 discs were placed into a sterile glass vial with 9 mL of Eagle's medium and incubated at 37°C for 24 h. The cytotoxic effect of the eluates was evaluated by 3H-thymidine incorporation. Results: The results showed that the components leached from the resins were cytotoxic to L929 cells, except for the specimens heat treated in water bath (p<0.05). Compared to the group with no heat treatment, water-bath decreased the cytotoxicity of the denture base acrylic resins. Conclusion: The in vitro cytotoxicity of the tested denture base materials was not influenced by microwave post-polymerization heat treatment.

Vickers hardness of cast commercially pure titanium and Ti-6Al-4V alloy submitted to heat treatments

The purpose of this study was to evaluate the effect of heat treatments on the Vickers hardness of commercially pure titanium and Ti-6Al-4V cast alloys. Six-millimeter-diameter cylindrical specimens were cast in a Rematitan System. Commercially pure titanium and Ti-6Al-4V alloy specimens were randomly assigned to 3 groups (n=10) that received the following heat treatments: control (no heat treatment); treatment 1 (T1): heating at 750°C for 2 h; and treatment 2 (T2): annealing at 955°C for 1 h and aging at 620°C for 2 h. After heat treatments, the specimens were embedded in acrylic resin and their surface was ground and polished and hardness was measured. Vickers hardness means (VHN) and standard deviations were analyzed statistically by Kruskal-Wallis test at 5% significance level. For commercially pure titanium, Vickers hardness means of group T2 (259.90 VHN) was significantly higher than those of the other groups (control - 200.26 VHN and T1 - 202.23 VHN), which presented similar hardness means to each other (p>0.05). For Ti-6Al-4V alloy, statistically significant differences were observed among the three groups: T2 (369.08 VHN), T1 (351.94 VHN) and control (340.51 VHN) (p<0.05). The results demonstrated different hardness of CP Ti and Ti-6Al-4V when different heat treatments were used. For CP Ti, VHN means of T2 group was remarkably higher than those of control and T1 group, which showed similar VHN means to each other. For Ti-6Al-4V alloy, however, VHN means recorded for each group may be presented as follows: T2>T1>control.

Effect of thermal treatment under oxygen atmosphere on the superconducting properties of RuSr2GdCu2O8

The discovery of the spatial uniform coexistence of superconductivity and ferromagnetism in rutheno-cuprates, RuSr2GdCu2O8 (Ru-1212), has spurred an extraordinary development in the study of the competition between magnetism and superconductivity. However, several points of their preparation process and characterization that determine their superconductive behavior are still obscure. The improvement of sample preparation conditions involves some thermal treatments in inert atmosphere. The first treatment results in the immediate formation of Sr2GdRuO 6. Using the CuO composition as a precursor, we produced Ru-1212. To turn it metallic and superconductor, besides the previous treatment, a final sinterization is carried out in oxygen flow for several days. Three Ru-1212 samples were produced by varying the last sinterization time (two, four, and six days under oxygen flow). Through measurements of x-ray diffraction, scanning electron microscopy, differential thermal analysis, magnetic susceptibility and mechanical spectroscopy, it was studied the influence of the treatments under oxygen atmosphere on the structural and superconducting properties of the material.

Effects of heat treatments on the electrocatalytic activity of Pt-Ru/C for methanol oxidation

The Pt-Ru/C materials of this study were prepared by a microemulsion method with fixed water to surfactant molar ratio and heat treated at low temperatures, to avoid changes in the average particle size, in different atmospheres. All samples were characterized by X-ray diffraction (XRD) and the mean crystallite size was estimated by using Scherrer's equation. Catalysts morphology was characterized by transmission electron microscopy (TEM). Average composition was obtained by energydispersive X-ray analysis (EDX). The general electrochemical behavior was evaluated by cyclic voltammetry in 0.5 M sulfuric acid and the electrocatalytic activity towards the oxidation of methanol was studied in 0.5 M methanol acid solutions by potential sweeps and chronoamperometry. Oxidation of adsorbed CO was used to estimate the electrochemical active area and to infer the surface properties. ©The Electrochemical Society.

Plasma nitriding and nitrocarburising of a supermartensitic stainless steel

Supermartensitic stainless steels (SMSSs) are a new generation of the classic 13%Cr martensitic steels, lower in carbon and with additional alloying of nickel and molybdenum offering better weldabilty and low temperature toughness. Several works have shown that plasma nitriding and nitrocarburising of stainless steels at low temperatures produces a hard surface layer which results in increased wear resistance. In this work, SMSS samples were plasma nitrided and nitrocarburised at 400, 450 and 500 °C. The plasma treated SMSS samples were characterised by means of optical microscopy, microhardness, X-ray diffraction and dry wear tests. The thickness of the layers produced increases as temperature is raised, for both plasma nitriding and nitrocarburising. X-ray diffraction demonstrates that the chromium nitride content grows with temperature for nitriding and nitrocarburising, which also showed increasing content of iron and chromium carbides with temperature. After plasma treating, it was found that the wear volume decreases for all temperatures and the wear resistance increased as the treatment temperature was raised. The main wear mechanism observed for both treated and untreated samples was grooving abrasion. © 2012 IHTSE Partnership Published by Maney on behalf of the Partnership.

Histological analysis of the osseointegration of Ti-30Ta dental implants after surface treatment

Metallic biomaterials are used to reinforce or to restore the form and function of hard tissues. Implants and prosthesis are used to replace shoulders, knees, hips and teeth. When these materials are inserted in bone several biological reactions happen. This process can be associated to surface properties (topography, roughness and surface energy). In this work, the influence of biomimetic surface treatment in the osseointegration of Ti-30Ta dental implants was evaluated. Ingots were obtained from titanium and tantalum by using an arc-melting furnace. They were submitted to heat treatment at 1,100°C for 1 h, cooled in water and cold worked by swaging. Then, screw-shaped implants (2.0 mm diameter by 2.5 mm length) were manufactured and they were implanted in a rat's femur. Animals were divided into two groups: untreated (control group) and treated (biomimetic surface treatment). They were sacrificed 30 days after implantation. For histological analysis, implants with surrounding tissue were removed and immersed in formaldehyde. Samples were embedded in polymethyl methacrylate and after polymerization, cut with a saw, polished and mounted on glass slides. The results obtained suggest that biomimetic surface treatment was able to promote an increase osseointegration on the surface of dental implants. © Springer-Verlag Berlin Heidelberg 2013.

Analysis of the bioactive surface of Ti-35Nb-7Zr alloy after alkaline treatment and solution body fluid

The purpose of this work was to evaluate the Ti-35Nb-7Zr experimental alloy after surface treatment and soaking in solution body fluid (SBF) to form bonelike apatite. The Ti-35Nb-7Zr alloy was produced from commercially pure materials (Ti, Nb and Zr) by an arc melting furnace. All ingots were submitted to sequences of heat treatment (1100 °C/2 h and water quenching), cold working by swaging procedures and heat treatment (1100 °C/2 h and water quenching). Discs with 13 mm diameter and 3 mm in thickness were cut. The samples were immersed in NaOH aqueous solution with 5 M at 60 °C for 72 h, washed with distilled water and dried at 40 °C for 24 h. After the alkaline treatment, samples were heat treated in both conditions: at 450 and 600 °C for 1 h in an electrical furnace in air. Then, they were soaking in SBF for 24 h to form an apatite layer on the surface. The surfaces were investigated by using scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDX), infrared spectroscopy (FTIR) and contact angle measurements. The results indicate that calcium phosphate could form on surface of Ti-35Nb-7Zr experimental alloy. © Springer-Verlag Berlin Heidelberg 2013.

Piezoresponse force microscopy characterization of rare-earth doped BiFeO3 thin films grown by the soft chemical method

The multiferroic behavior with ion modification using rare-earth cations on crystal structures, along with the insulating properties of BiFeO3 (BFO) thin films was investigated using piezoresponse force microscopy. Rare-earth-substituted BFO films with chemical compositions of (Bi 1.00-xRExFe1.00O3 (x=0; 0.15), RE=La and Nd were fabricated on Pt (111)/Ti/SiO2/Si substrates using a chemical solution deposition technique. A crystalline phase of tetragonal BFO was obtained by heat treatment in ambient atmosphere at 500 °C for 2 h. Ion modification using La3+ and Nd3+ cations lowered the leakage current density of the BFO films at room temperature from approximately 10-6 down to 10-8 A/cm2. The observed improved magnetism of the Nd3+ substituted BFO thin films can be related to the plate-like morphology in a nanometer scale. We observed that various types of domain behavior such as 71° and 180° domain switching, and pinned domain formation occurred. The maximum magnetoelectric coefficient in the longitudinal direction was close to 12 V/cm Oe. © 2012 Elsevier Ltd and Techna Group S.r.l.

Effect of Post-silanization Heat Treatments of Silanized Feldspathic Ceramic on Adhesion to Resin Cement

Purpose: To evaluate the effect of post-silanization heat treatment of a silane agent and rinsing with hot water of silanized CAD/CAM feldspathic ceramic surfaces on the microtensile bond strength between resin cement and the ceramic, before and after mechanical cycling.Materials and Methods: Blocks measuring 10 x 5.7 x 3.25 mm(3) were produced from feldspathic ceramic cubes (VITA Mark II, VITA Zanhfabrik). Each ceramic block was duplicated in composite resin using a template made of polyvinylsiloxane impression material. Afterwards, ceramic and corresponding resin composite blocks were ultrasonically cleaned and randomly divided according to the 5 strategies used for conditioning the ceramic surface (n = 10): GHF: etching with hydrofluoric acid 10% + rinsing with water at room temperature + silanization at 20 degrees C; G20: silanization; G77: silanization + oven drying at 77 degrees C; G20r: silanization + hot water rinsing; G77r: silanization + oven drying at 77 C + hot water rinsing. The resin and ceramic blocks were cemented using a dual-curing resin cement. Every group was divided in two subgroups: aging condition (mechanical cycling, designated as a) or non-aging (designated as n). All the bonded assemblies were sectioned into microsticks for microtensile bond strength (mu TBS) testing. The failure mode of the tested specimens was assessed and mu TBS data were statistically analyzed in two ways: first 2-way ANOVA (GHF, G20 and G77 in non-aging/aging conditions) and 3-way ANOVA (temperature x rinsing x aging factors, excluding GHF), followed by Tukey's test (p = 0.05).Results: The 2-way ANOVA revealed that the mu TBS was significantly affected by the surface treatment (p < 0.001) but not by aging (p = 0.68), and Tukey's test showed that G77-n/G77-a (18.0 MPa) > GHF-n/GHF-a (12.2 MPa) > G20-n/G20-a (9.1 MPa). The 3-way ANOVA revealed that the mu TBS was significantly affected by the heat treatment and rinsing factors (p < 0.001), but not affected by aging (p = 0.36). The rinsing procedure decreased, while oven drying increased the bond strengths. Group G77, in both non-aging and aging conditions (18.6-17.4 MPa), had the highest bond values. Failure modes were mainly mixed for all groups.Conclusion: Oven drying at 77 degrees C improved the bond strength between the resin cement and feldspathic ceramic, but hot water rinsing reduced the bond strength and should not be recommended.

Effect of surface and heat treatments on the biaxial flexural strength and phase transformation of a Y-TZP ceramic

To evaluate the effect of grinding and airborne-particle abrasion on the biaxial flexural strength (BFS) and phase transformation of a Y-TZP ceramic, and examine whether sintering the veneering porcelain renders the previous heat treatment recommended by the manufacturer unnecessary. Materials and Methods: Lava zirconia specimens (N = 108) were obtained with the following dimensions: 14.0 mm diameter × 1.3 mm thickness (n = 36) and 14.0 mm × 1.6 mm (n = 72). The thicker specimens were ground with diamond burs under irrigation and received (heat-treated groups) or not (non-heat-treated groups) a heat treatment (1000°C for 30 min) prior to the four firing cycles applied to simulate the sintering of the veneering porcelain. All specimens were air abraded as follows (n = 12): 1) 30-μm silica-modified Al2O3 particles (Rocatec Soft); 2) 110-μm silica-modified Al2O3 particles (Rocatec Plus); and 3) 120-μm Al2O3 particles, followed by Rocatec Plus. Three specimens of each group were analyzed by x-ray diffraction (XRD) to assess the monoclinic phase content (%). The BFS test was performed in a mechanical testing machine (Instron 8874). Data (MPa) were analyzed by two-way ANOVA (grinding × airborne-particle abrasion and heat treatment × airborne-particle abrasion) and Tukey's post-hoc test (α = 0.05). The strength reliability was analyzed using the Weibull distribution. Results: Grinding significantly decreased the BFS of the non-heat-treated groups (p < 0.01). Within the ground groups, the previous heat treatment did not influence the BFS (p > 0.05). Air abrasion only influenced the BFS of the ground/heat-treated groups (p < 0.01). For the non-heat-treated groups, the grinding did not decrease the Weibull modulus (m), but it did decrease the characteristic strength (σ0). For Rocatec Soft and 120-μm Al2O3 particles + Rocatec Plus, the heat-treated groups presented lower m and higher σ0 than the ground/non-heat-treated groups. The independent variables did not seem to influence phase transformation. Air-abraded surfaces presented higher monoclinic zirconia content than the as-sintered and ground surfaces, which exhibited similar content. Conclusion: Even under irrigation, grinding compromised the Y-TZP ceramic strength. The sintering of the veneering porcelain rendered the previous heat treatment recommended by the manufacturer unnecessary. Airborneparticle abrasion influenced the strength of heat-treated zirconia.

Effect of surface and heat treatments on the biaxial flexural strength and phase transformation of a y-tzp ceramic

To evaluate the effect of grinding and airborne-particle abrasion on the biaxial flexural strength (BFS) and phase transformation of a Y-TZP ceramic, and examine whether sintering the veneering porcelain renders the previous heat treatment recommended by the manufacturer unnecessary. Materials and Methods: Lava zirconia specimens (N = 108) were obtained with the following dimensions: 14.0 mm diameter × 1.3 mm thickness (n = 36) and 14.0 mm × 1.6 mm (n = 72). The thicker specimens were ground with diamond burs under irrigation and received (heat-treated groups) or not (non-heat-treated groups) a heat treatment (1000°C for 30 min) prior to the four firing cycles applied to simulate the sintering of the veneering porcelain. All specimens were air abraded as follows (n = 12): 1) 30-μm silica-modified Al2O3 particles (Rocatec Soft); 2) 110-μm silica-modified Al2O3 particles (Rocatec Plus); and 3) 120-μm Al2O3 particles, followed by Rocatec Plus. Three specimens of each group were analyzed by x-ray diffraction (XRD) to assess the monoclinic phase content (%). The BFS test was performed in a mechanical testing machine (Instron 8874). Data (MPa) were analyzed by two-way ANOVA (grinding × airborne-particle abrasion and heat treatment × airborne-particle abrasion) and Tukey's post-hoc test (α = 0.05). The strength reliability was analyzed using the Weibull distribution. Results: Grinding significantly decreased the BFS of the non-heat-treated groups (p < 0.01). Within the ground groups, the previous heat treatment did not influence the BFS (p > 0.05). Air abrasion only influenced the BFS of the ground/heat-treated groups (p < 0.01). For the non-heat-treated groups, the grinding did not decrease the Weibull modulus (m), but it did decrease the characteristic strength (σ0). For Rocatec Soft and 120-μm Al2O3 particles + Rocatec Plus, the heat-treated groups presented lower m and higher σ0 than the ground/non-heat-treated groups. The independent variables did not seem to influence phase transformation. Air-abraded surfaces presented higher monoclinic zirconia content than the as-sintered and ground surfaces, which exhibited similar content. Conclusion: Even under irrigation, grinding compromised the Y-TZP ceramic strength. The sintering of the veneering porcelain rendered the previous heat treatment recommended by the manufacturer unnecessary. Airborneparticle abrasion influenced the strength of heat-treated zirconia.