Synthesis and crystal phase evaluation of hydroxylapatite using the rietveld-maximum entropy method

Bioceramic systems based on hydroxylapatite (HAP) are an important class of bioactive materials that may promote bone regeneration. The aim of this research was to evaluate how the stoichiometry of HAP influences its microstructural properties when diagnosed using the combined Rietveld method and Maximum entropy method (MEM). The Rietveld Method (RM) is recognizably a powerful tool used to obtain structural and microstructural information of polycrystalline samples analyzed by x-ray diffraction. Latterly have combined the RM with the maximum entropy method (MEM), with the goal of improve structural refinement results. The MEM provides high resolution maps of electron density and their analysis leave the accurate localization of atoms inside of unit cell. Like that, cycles Rietveld-MEM allow an excellent structural refinement In this work, a hydroxylapatite sample obtained by emulsion method had its structure refined using one cycle Rietveld-MEM with x-ray diffraction data. The indices obtained in initial refinement was Rwp = 7.50%, Re = 6.56%, S - 1.14% e RB = 1.03%. After MEM refinement and electron densities maps analysis to correction of atomics positions, the news indicators of Rietveld refinement quality was Rwp = 7.35%, Re = 6.56%, S = 1.12% and RB = 0.75%. The excellent result obtained to RB shows the efficiency of MEM as auxiliary in the refinement of structure of hydroxylapatite by RM.

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.

Detection of cracks in scratching tests in ceramic materials through acoustic emission

The mechanisms of material removal and the interactions among scratches performed in ceramic materials were investigated using acoustic emission signals, and scanning electron microscopy, in scratching experiments. Several testing conditions were used to produce different types of removing mechanism on a glass as well as on a polycrystalline alumina sample composed by heterogeneous grain size. It is known that the material removing process on a polycrystalline ceramic involves intergranular microfracture and grain dislodgement, unlike the chipping produced by the extension of lateral cracks in non-granular materials, such as glass. Distinct settings for velocities, loads, and two types of diamond indenter were tested. The material removal was carried out by three different methods of scratching: single passes, repeated overlapping passes, and parallel scratches. As a general result, there was a clear relationship between the acoustic emission signals and the damage intensity occurred in the material removal. More specifically, there were differences in the acoustic emission signal levels in the scratches made on the alumina and on the glass owing to the material removal mechanisms associated with the structure of these materials. A gradual increase in the acoustic emission levels was observed when the number of repeated passes was increased as a result of the damage accumulation process followed by severe material removal. It was also noticed that the acoustic emission signals were capable of reflecting the interactions between two parallel scratches.

Preparation of ceramic membranes from surface modified tin oxide nanoparticles

The preparation of crack-free SnO2 supported membranes requires the development of new strategies of synthesis capable to allow controlled changes of surface chemistry and to improve the processability of supported layers. In this way, the controlled modification of the SnO2 nanoparticle surface by adding capping molecules like Tiron(R) ((OH)(2)C6H2(SO3Na)(2)) during the sol-gel process was studied, aiming to obtain high performance membranes. Colloidal suspensions were prepared by hydrolyzing SnCl4.5H(2)O aqueous solution with NH4OH in presence of Tiron(R). The effect of the amount of Tiro(R) (from I to 20 wt.%) on the structural features of nanoparticles, powder redispersability and particle-solution interface properties was investigated by X-ray powder diffraction (XRPD), extended X-ray absorption fine structure (EXAFS), quasi-elastic light scattering and electrophoretic mobility measurements. XRPD and EXAFS results showed that the addition of Tiron(R) up to 20 wt.% to colloidal suspensions does not affect the crystallite size of SnO2 primary particles, determined around 2-3 nm. This value is comparable to the hydrodynamic size measured after redispersion of powder prepared with amount of Tiro(R) higher than 7.5 wt.%, indicating the absence of condensation reactions between primary particles after the initial precipitation step. As a consequence the powder with amount of Tiron(R) > 7.5 wt.%, can be fully redispersed in aqueous solution at pH greater than or equal to I I until a nanoparticle concentration of 6 vol.%. The electrophoresis measurements showed a decrease of the isoelectric point by increasing the amount of grafted Tiron(R) at the SnO2 nanoparticle surface, resulting in negatively charged particle-solution interface in all the studied pH range (2-11). These features govern the gelation process favoring the preparation of crack-free SnO2 supported membranes. The control exercised by Tiron(R) modifying agent in the aggregation process allows the fine-tuning of the porosity, from 0.124 to 0.065 cm(3) g(-1), and mean pore size, from 6.4 to 1.9 nm, as the amount of grafted molecules increases from 0 to 10 wt.%. In consequence, the membrane cut-off determined by filtration of polyethylene glycol standard solutions can be screened from 1500 to 3500 g mol(-1). (C) 2002 Elsevier B.V. B.V. All rights reserved.

Ceramic materials in dentistry: historical evolution and current practice

Dental ceramics are presented within a simplifying framework allowing for facile understanding of their development, composition and indications. Engineering assessments of clinical function are dealt with and literature is reviewed on the clinical behaviour of all-ceramic systems. Practical aspects are presented regarding the choice and use of dental ceramics to maximize aesthetics and durability, emphasizing what we know and how we know it.

MnO2 influence on the electrical properties of SnO2-based ceramic systems

Tin dioxide is an n-type semiconductor that when doped with other metallic oxides exhibits non-linear electric behavior with high non-linear coefficient values typical of a varistor. In this work, electrical properties of the SnO2.CoO.Ta2O5 and SnO2.CoO.MnO2.Ta2O5 ceramics systems were studied with the objective of analyzing the influence of MnO2 on sintering behavior and electrical properties of these systems. The compacts were prepared by powder mixture process and sintered at 1300°C for 1 hour, in air, using a constant heating rate of 10°C/min. The morphological and structural properties were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The densities of the sintered ceramics were measured using the Archimedes method. The SnO2.CoO.Ta2O5 and SnO2.CoO.MnO2.Ta2O5 systems presented breakdown fields (Eb) about 3100 V.cm-1 and 3800 V.cm-1, respectively, and non-linear coefficient (α) about 10 and 20, respectively.

Optical properties and energy-transfer frequency upconversion of Yb 3+-sensitized Ho3+- And Tb3+-doped lead-cadmium-germanate glass and glass ceramic

In this report we investigate the optical properties and energy-transfer upconversion luminescence of Ho3+- and Tb3+/Yb 3+-codoped PbGeO3-PbF2-CdF2 glass-ceramic under infrared excitation. In Ho3+/Yb 3+-codoped sample, green(545 nm), red(652 nm), and near-infrared(754 nm) upconversion luminescence corresponding to the 4S 2(5F4) → 5I8, 5F5 → 5I8, and 4S2(5F4) → 5I 7, respectively, was readly observed. Blue(490 nm) signals assigned to the 5F2,3 → 5I8 transition was also detected. In the Tb3+/Yb3+ system, bright UV-visible emission around 384, 415, 438, 473-490, 545, 587, and 623 nm, identified as due to the 5D3(5G6) → 7FJ(J=6,5,4) and 5D4→ 7FJ(J=6,5,4,3) transitions, was measured. The comparison of the upconversion process in glass ceramic and its glassy precursor revealed that the former samples present much higher upconversion efficiencies. The dependence of the upconversion emission upon pump power, and doping contents was also examined. The results indicate that successive energy-transfer between ytterbium and holmium ions and cooperative energy-transfer between ytterbium and terbium ions followed by excited-state absorption are the dominant upconversion excitation mechanisms herein involved. The viability of using the samples for three-dimensional solid-state color displays is also discussed.

Development of a micro heat exchanger made with ceramic multi-layers (LTCC) and its setup to gas flow measurements

A green ceramic tape micro heat exchanger was developed using LTCC technology. The device was designed by using a CAD software and 2D and 3D simulations using a CFD package (COMSOL Multiphysics) to evaluate the fluid behavior in the microchannels. The micro heat exchanger is composed of five thermal exchange plates in cross flow arrangement and two connecting plates; heat exchanger dimensions are 26 × 26 × 6 mm3. Preliminary tests were carried out to characterize the device both in atmospheric pressure and in vacuum. The same techniques used in vacuum technology were applied to check the rotameters and to prevent device leakages. Thermal performance of the micro heat exchanger was experimentally tested. © 2009 Elsevier B.V. All rights reserved.

Glass-ceramic material from the SiO 2-Al 2O 3-CaO system using sugar-cane bagasse ash (SCBA)

Brazil is the world's largest producer of alcohol and sugar from sugarcane. Currently, sugarcane bagasse is burned in boilers to produce steam and electrical energy, producing a huge volume of ash. The major component of the ash is SiO 2, and among the minor components there are some mineralizing agents or fluxing. Published works have shown the potential of transforming silicate-based residues into glass-ceramic products of great utility. This work reports the research results of SCBA use to produce glass-ceramics with wollastonite, rankinite and gehlenite as the major phases. These silicates have important applications as building industry materials, principally wollastonite, due to their special properties: high resistance to weathering, zero water absorption, and hardness among others. The glasses (frits) were prepared mixing ash, calcium carbonate and sodium or potassium carbonates as flux agents, in different concentrations. X-ray fluorescence was used to determine the chemical composition of the glasses and their crystallization was assessed by using thermal analysis (DTA/DSC/TGA) and X-ray diffraction. The crystallization kinetics was evaluated using the Kissinger method, giving activation energies ranging from 200 to 600 kJ/mol. © 2011 Ceramic Society of Japan.

The physicochemical characterization and in vivo response of micro/nanoporous bioactive ceramic particulate bone graft materials

In this study, the physicochemical characteristics of calcium phosphate based bioactive ceramics of different compositions and blends presenting similar micro/nanoporosity and micrometer scale surface texture were characterized and evaluated in an in vivo model. Prior to the animal experiment, the porosity, surface area, particle size distribution, phase quantification, and dissolution of the materials tested were evaluated. The bone regenerative properties of the materials were evaluated using a rabbit calvaria model. After 2, 4, and 8 weeks, the animals were sacrificed and all samples were subjected to histologic observation and histomorphometric analysis. The material characterization showed that all materials tested presented variation in particle size, porosity and composition with different degrees of HA/TCP/lower stoichiometry phase ratios. Histologically, the calvarial defects presented temporal bone filling suggesting that all material groups were biocompatible and osteoconductive. Among the different materials tested, there were significant differences found in the amount of bone formation as a function of time. At 8 weeks, the micro/nanoporous material presenting similar to 55,TCP:45%,HA composition ratio presented higher amounts of new bone regeneration relative to other blends and a decrease in the amount of soft tissue infiltration. (C) 2014 Elsevier B.V. All rights reserved.

CERAMIC MATERIAL FROM SEWAGE SLUDGE AS SUPPORT MATERIAL SUPPLY WATER FILTRATION

This study shows a possibility of using municipal sewage sludge after thermal treatment in the production of a filtering material to water treatment. Due to the fast urbanization and implementation of high standards for effluent in many countries in recent years, the sewage sludge is being produced in an ever increasing amount. Therefore, the use of sludge is a suitable solution for the expected large quantity of sludge. Dehydration of sludge was performed by controlled heating at temperatures of 1100 degrees C, 850 degrees C, 650 degrees C, 350 degrees C for 3 hours. After thermal treatment the sludge was characterized by X-ray fluorescence, TG/DTG/DTA, residue solubilization and residue lixiviation tests. The aim of the present work was to observe, thought the characterization techniques, if the treated sewage sludge is or not adequate to be used as filter material to water treatment. It will be verified which treatment temperature of the sludge offer possibility to its use in water treatment without carrying pollutants in concentrations out of the standards.

Use of Sludge as Ceramic Materials

Nowadays, with increase amounts of sludge derived from the treatment of domestic sewage put pressure into research on systems for the adequate use of these materials. The aim of the present work is to study the use of sludge ash, from sintering and calcinated process, as a raw material for the ceramic industry. Using the sewage sludge ashes as ceramic raw material there will be no contamination of soil and underground water. Metals and toxic compounds like Al, Fe, Ba, Cr, Cu, Mn and Zn oxides were analyzed and characterized by X-ray fluorescence (XRF), scanning electron microscopy (SEM) and plasma emission spectroscopy (ICP-OES). The leached material was chemically analyzed where the integration of oxides into the ceramic matrix of sludge ash was observed. Residual decomposition was analyzed by TG, DTG and DTA curves.

Vibrational spectroscopy applied to the study of archeological ceramic artifacts from Guarani culture in Brazil

An archeological artifact can be seen as a chronological element, which helps to determine the age of certain society and to understand the thinking, values and the way of life of this society. Thus, the classification of archeological artifacts is one of the approaches used to study the cultural system of antique societies trying to reconstruct their history. The "Centro de Museologia, Antropologia e Argueologia (CEMAARQ)" of the "Unesp Univ Estadual Paulista" in Presidente Prudente, São Paulo state, Brazil, develops projects within this context (identification and preservation). This is the case of the archeological site named "Lagoa São Paulo-02" discovered in 1993 at the margins of the Parana river in the region of Presidente Epitacio city, São Paulo state, Brazil. This site has ceramic fragments of different shapes and sizes that have a strong influence of traces of the Guarani culture, which is one of the Brazilian native populations. These samples were basically characterized via micro-Raman scattering and Fourier transform infrared absorption (FTIR) spectroscopies. The main objective was to identify the pigments used in the manufacture of the ceramic artifacts and to analyze the composition of the ceramic body to understand how the artifacts were made. Three pigments were found: red, black and white. For the red pigment were identified characteristic bands of hematite, an iron oxide found in the red rocks of the river banks that were eroded by water. The black pigment, probably, is due to the use of vegetal charcoal, which is found in nature as the product of burning organic material such as wood. For the white pigment, the FTIR spectra suggested the use of kaolin, either in the ceramic body or in the proper white pigment, due to the presence of the characteristic bands of the kaolinite. Complementary, the additives applied as anti-plastics were identified as charcoal and quartz, being the latter found in the rocks present in the archeological site. (C) 2010 Elsevier B.V. All rights reserved.

Sugarcane bagasse ash as a potential quartz replacement in red ceramic

Sugarcane bagasse ash (SCBA) is an industrial waste that contains silicon and aluminum oxides as the major components and iron, calcium, magnesium, and potassium oxides as the main minor components. In this paper, SCBA from one Brazilian factory was characterized and tested for its influence on the ceramic properties of clay/ash ceramic probes. Prismatic probes were pressed (18 MPa) using a ceramic mass mixed with 0%, 5%, 8%, and 10% ash. The probes were fired at temperatures between 800 degrees and 1200 degrees C. X-ray diffraction, X-ray fluorescence, thermal analysis (differential thermal analysis, thermo-gravimetric analysis/differential thermogravimetric analysis), and tests for texture (particle-size analysis), flexural strength, and linear shrinkage were carried out to characterize the samples. The results showed that the amount of ash to be incorporated will depend on mainly the composition of clay but also ash, and indicated that the clay used in this work can incorporate up to 10% weight of ash to produce solid bricks. The results also showed an improvement in ceramic/ash properties up to sintering temperatures higher than 1000 degrees C.