Effect of the iron doping on the thermal decomposition of the polymeric precursor for the titanium dioxide powder synthesis

The Polymeric Precursor Method has proved suitable for synthesizing reactive powders using low temperatures of calcination, especially when compared with conventional methods. However, during the thermal decomposition of the polymeric precursor the combustion event can be releases an additional heat that raises the temperature of the sample in several tens of degrees Celsius above the set temperature of the oven. This event may be detrimental to some material types, such as the titanium dioxide semiconductor. This ceramic material has a phase transition at around 600 ° C, which involves the irreversible structural rearrangement, characterized by the phase transition from anatase to rutile TiO2 phase. The control of the calcination step then becomes very important because the efficiency of the photocatalyst is dependent on the amount of anatase phase in the material. Furthermore, use of dopant in the material aims to improve various properties, such as increasing the absorption of radiation and in the time of the excited state, shifting of the absorption edge to the visible region, and increasing of the thermal stability of anatase. In this work, samples of titanium dioxide were synthesized by the Polymeric Precursor Method in order to investigate the effect of Fe (III) doping on the calcination stages. Thermal analysis has demonstrated that the Fe (III) insertion at 1 mol% anticipates the organic decomposition, reducing the combustion event in the final calcination. Furthermore, FTIR-PAS, XRD and SEM results showed that organic matter amount was reduced in the Fe (III)-doped TiO2 sample, which reduced the rutile phase amount and increased the reactivity and crystallinity of the powder samples.

Effects of the addition of ions barium on the structural and electrical properties of PZT ceramic

Lead zirconate titanate, with Zr/Ti ratio of 53/47 was prepared by the polymeric precursor method. It was investigated the barium (II) modification at 0.0, 0.2, 0.4 and 0.6 mol% in substitution to the lead (II) cation in A site of perovskite structure. The powder samples were characterized by XRD and the diffraction patterns were used to Rietveld refinement. The percentages of tetragonal and rhombohedral phases and a systematic study of the effect of barium (II) on the morphology and the dielectric properties of PZT were carried out. The results showed that the tetragonal phase is favored and the ceramic density is improved with the barium (II) insertion. The Curie temperature (Tc) is increased besides the slight reduction of dielectric constant (Kc).

High activity photocatalyst powder formed by three ceramic oxides

A Photocatalyst ceramic powder that presented high photoactivity based on TiO2 modified with 25% molar of SnO2 and up to 5% molar of Ag2O was obtained in the present work. The aforementioned ceramic powder was obtained using all commercial oxides as well as the oxides mixture technique. The powders were ground in high energy mill for one hour with subsequent thermal treatment at 400°C for four hours. They were, furthermore, characterized using surface area of around 6m2/g, where the X-Ray diffraction results provided evidence for the presence of anatase and rutile phases, known to be typical characteristics of both the TiO2 and SnO2 used. During the thermal treatment, Ag2O was reduced to metallic silver. The photodegradation rehearsals were carried out using a 0.01 mmol/L Rhodamine B solution in a 100mg/L photocatalyst suspension in a 500ml beaker, which was irradiated with 4W germicide Ultraviolet light of 254nm. In addition, samples were removed after duration of about 10 minutes to an hour, where they were analyzed thoroughly in UV-vis spectrophotometer. The analysis of the results indicated that for the compositions up to 2.5% molar of Ag2O, the photoactivity was found to be greater than that of Degussa P25 photocatalyst powder, and as such it was then used as a reference. Taking into account 90% degradation of Rhodamine B, a duration period of 11 minutes was obtained for the developed photocatalyst powder compared to the 38 minutes observed for the Degussa P25. FEG-SEM micrographies enabled the verification of the morphology as well as the interaction of the oxide particles with the metallic silver, which led us to propose a model for the increase in photoactivity observed in the photocatalyst powder under investigation.

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.

Effect of particle size on the flexural strength and phase transformation of an airborne-particle abraded yttria-stabilized tetragonal zirconia polycrystal ceramic.

Statement of problem Because airborne-particle abrasion is an efficient method of improving the bond at the zirconia-cement interface, understanding its effect on the strength of yttria-stabilized tetragonal zirconia polycrystal is important. Purpose The purpose of this study was to evaluate the effect of the particle size used for airborne-particle abrasion on the flexural strength and phase transformation of a commercially available yttria-stabilized tetragonal zirconia polycrystal ceramic. Material and Methods For both flexural strength (20.0 × 4.0 × 1.2 mm) (n=14) and phase transformation (14.0-mm diameter × 1.3-mm thickness) (n=4), the zirconia specimens were made from Lava, and their surfaces were treated in the following ways: as-sintered (control); with 50-μm aluminum oxide (Al2O3) particles; with 120-μm Al2O3 particles; with 250-μm Al2O3 particles; with 30-μm silica-modified Al2O3 particles (Cojet Sand); with 120-μm Al2O3 particles, followed by 110-μm silica-modified Al2O3 particles (Rocatec Plus); and with Rocatec Plus. The phase transformation (%) was assessed by x-ray diffraction analysis. The 3-point flexural strength test was conducted in artificial saliva at 37°C in a mechanical testing machine. The data were analyzed by 1-way ANOVA and the Tukey honestly significant difference post hoc test (α=.05). Results Except for the Cojet Sand group, which exhibited statistically similar flexural strength to that of the as-sintered group and for the group abraded with 250-μm Al2O3 particles, which presented the lowest strength, airborne-particle abrasion with the other particle sizes provided the highest values, with no significant difference among them. The as-sintered specimens presented no monoclinic phase. The groups abraded with smaller particles (30 μm and 50 μm) and those treated with the larger ones (110 μm and/or 120 μm particles and 250 μm) exhibited percentages of monoclinic phase that varied from 4% to 5% and from 8.7% to 10%. Conclusions Except for abrasion with Cojet Sand, depending on the particle size, zirconia exhibited an increase or a decrease in its flexural strength. Airborne-particle abrasion promoted phase transformation (tetragonal to monoclinic), and the percentage of monoclinic phase varied according to the particle size.

Effect of surface treatments on the shear bond strength of luting cements to Y-TZP ceramic

Statement of problem Because zirconia is a glass-free material, alternative surface treatments such as airborne-particle abrasion or silica coating should be used for long-term bonding. However, these surface treatments in combination with different bonding agents and luting cements have not yet been studied. Purpose The purpose of the study was to evaluate the effect of surface treatments on the shear bond strength (SBS) of luting cements to Y-TZP ceramic. Material and methods Zirconia disks (N=240) were airborne-particle abraded with the following particles (n=48): 50 μm Al2O3; 120 μm Al2O3; 30 μm silica-coated Al2O3 (Rocatec Soft); 120 μm Al2O3+110 μm silica-coated Al2O3 (Rocatec Plus); and Rocatec Plus. After silanization of the zirconia surface, composite resin disks were bonded with (n=12) RelyX Luting 2; RelyX ARC; RelyX U100; and Panavia F. The bonded specimens were thermocycled (10 000 cycles) and tested for SBS. Failure mode was determined with a stereomicroscope (×20). The morphology and elemental composition of airborne-particle abraded surfaces were evaluated with scanning electron microscopy (×500) and energy-dispersive x-ray spectroscopy (×50). Results Surface treatments, cements, and their interaction were significant (P<.001). For RelyX ARC, Rocatec Soft and Rocatec Plus provided the highest SBS. In general, surface treatments did not influence the SBS of RelyX U100 and Panavia F. Regardless of the cement, no significant difference was found between 50 μm and 120 μm Al2O3 particles, between Rocatec Soft and Rocatec Plus, or between Rocatec Plus and 120 μm Al2O3 particles+Rocatec Plus. All groups showed adhesive failures. Different particle sizes provided differences in morphological patterns. The elemental composition comprised Al and Al/Si for alumina and silica-abraded zirconia. Conclusions Particle size did not influence the SBS of the groups abraded exclusively with alumina or silica-coated particles. RelyX ARC was more surface-treatment dependent than RelyX U100 or Panavia F.

In vitro study of color stability of polycrystalline and monocrystalline ceramic brackets

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Impacto da energia de micro-ondas na sinterização da zircônia odontológica

Pós-graduação em Odontologia Restauradora - ICT

Surface degradation of lithium disilicate ceramic after immersion in acid and fluoride solutions

Purpose: To analyze whether immersion in sodium fluoride (NaF) solutions and/or common acidic beverages (test solutions) would affect the surface roughness or topography of lithium disilicate ceramic. Methods: 220 ceramic discs were divided into four groups, each of which was subdivided into five subgroups (n = 11). Control group discs were immersed in one of four test beverages for 4 hours daily or in artificial saliva for 21 days. Discs in the experimental groups were continuously immersed in 0.05% NaF, 0.2% NaF, or 1.23% acidulated phosphate fluoride (APF) gel for 12, 73, and 48 hours, respectively, followed by immersion in one of the four test beverages or artificial saliva. Vickers microhardness, surface roughness, scanning electron microscopy (SEM) associated with energy dispersive spectroscopy, and atomic force microscopy (AFM) assessments were made. Data were analyzed by nested analysis of variance (ANOVA) and Tukey's test (alpha = 0.05). Results: Immersion in the test solutions diminished the microhardness and increased the surface roughness of the discs. The test beverages promoted a significant reduction in the Vickers microhardness in the 0.05% and 0.2% NaF groups. The highest surface roughness results were observed in the 0.2% NaF and 1.23% APF groups, with similar findings by SEM and AFM. Acidic beverages affected the surface topography of lithium disilicate ceramic. Fluoride treatments may render the ceramic surface more susceptible to the chelating effect of acidic solutions.

Effect of ceramic etching protocols on resin bond strength to a feldspar ceramic

This study sought to evaluate the resin micro-tensile bond strength (MTBS) stability of a leucite-reinforced ceramic after different ceramic etching protocols. The microtensile test had 40 ceramic blocks (5x5x6 mm) assigned to five groups (n=8), in accordance with the following surface etching protocols: NE nonetched (control); 9HF: hydrofluoric (HF) acid etching (9% HF)+wash/dry; 4HF: 4%HF+wash/dry; 5HF: 5%HF+wash/dry; and 5HF+N: 5%HF+neutralizer+wash/dry+ultrasonic-cleaning. Etched ceramic surfaces were treated with a silane agent. Next, resin cement blocks were built on the prepared ceramic surface and stored for 24 hours in distilled water at 37 degrees C. The specimens were then sectioned to obtain microtensile beams (32/block), which were randomly assigned to the following conditions, nonaged (immediate test) and aged (water storage for 150 days plus 12,000 thermal cycles), before the microtensile test. Bond strength data were submitted to one-way analysis of variance and Tukey test (alpha=0.05). Additional ceramic samples were subjected to the different ceramic etching protocols and evaluated using a scanning electron microscope (n=2) and atomic force microscopy (n=2). Aging led to a statistically significant decrease in the MTBS for all groups, except the untreated one (NE). Among the groups submitted to the same aging conditions, the untreated (NE) revealed inferior MTBS values compared to the 9HF and 4HF groups. The 5HF and 5HF+N groups had intermediate mean values, being statistically similar to the higher values presented by the 9HF and 4HF groups and to the lower value associated with the NE group. The neutralization procedure did not enhance the ceramic/resin cement bond strength. HF acid etching is a crucial step in resin/ceramic bonding.

Hard machining, glaze firing and hydrofluoric acid etching: Do these procedures affect the flexural strength of a leucite glass-ceramic?

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Interdisciplinary project applied to engineering education: construction of a miniature ceramic industry

The greatest challenge of undergraduate engineering courses is to encourage creativity, cooperation with other students, teamwork, and motivation in the first years of their courses. While students have little or no contact with advanced disciplines, it is very difficult to attract their interests and encourage them to develop the skills in their undergraduate courses. This work aims to achieve these objectives through a mini-factory project involving the construction of a production line of ceramic tiles on a laboratory scale, from the ceramic processing using raw materials to the shipping of the final product. Having been given an established monthly demand for ceramic tiles, the students determined the construction requirements of the mini-factory, as they have created the layout, including the processing equipment, the dimensioning of equipment, and its operational structure. This article intends to describe the successful creation of the ceramic tile mini-factory, including the objectives, benefits, and inherent difficulties of the process and the receptivity of the exercise by the students involved.

Local structure and hybridization states in Ba0.9Ca0.1Ti1-xZrxO3 ceramic compounds: Correlation with a normal or relaxor ferroelectric character

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Electrophoretic deposition of (Zn, Nb)SnO2-films varistor superficially modified with Cr3+

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)