A factorial design was used to evaluate the effects of processing variables on the morphology and microstructural characteristics of titanium dioxide (TiO2) fibers produced by solution blow spinning (SBS). For this, tests were carried out varying TiO2 precursor content, feed rate, air pressure, polymer, and solvent. The TTIP concentration and feed rate statistically influenced the average diameters of the PVC/TiO2 system. The proper combination between polymer and solvent enables the obtaining of TiO2 nanofibers with similar morphologies either using hydrophilic or hydrophobic polymer, however, fiber diameter is influenced by type of system (polymer/solvent) used. Only the anatase crystalline phase was found in the fibers with the PVC polymer and THF solvent, while two crystalline phases were obtained in the fibers with PVP and alcohol, anatase and rutile, indicating that the variation of the polymer and solvent influences the crystalline phases of the TiO2 fibers studied.

RESUMO Mulita é um material que tem recebido atenção especial devido às suas propriedades químicas, físicas e mecânicas, que estão correlacionadas com o método de síntese utilizado. O método sol-gel destaca-se frente aos outros métodos químicos devido à possibilidade de obtenção de materiais com elevado grau de pureza e baixas temperaturas de síntese. Sendo assim, este trabalho teve por objetivo a análise dos solventes água, álcool etílico, álcool isopropílico e tetrahidrofurano, na obtenção de mulita por meio da rota sol-gel. As amostras foram caracterizadas por difração de raios X (DRX), análise termogravimétrica e diferencial (TG/ATD), adsorção de nitrogênio, microscopia eletrônica de varredura (MEV) e microscopia eletrônica de transmissão (MET). Os resultados mostraram que a mulita foi sintetizada com todos os solventes, porém, o uso dos álcoois como solvente proporcionou a obtenção das amostras mais cristalinas, com as menores perdas de massa, com uma morfologia formada por agregados e partículas individualizadas.

ABSTRACT Mullite is a material that has received special attention due to its chemical, physical and mechanical properties, which are correlated with the synthesis method used. The sol-gel method stands out compared to other chemical methods due to the possibility of obtaining materials with a high degree of purity and low synthesis temperatures. Thus, this work aimed to analyze the solvents water, ethyl alcohol, isopropyl alcohol and tetrahydrofuran, in obtaining mullite using the sol-gel route. The samples were characterized by X-ray diffraction (XRD), thermogravimetric and differential analysis (TG/DTA), nitrogen adsorption (BET), scanning electron microscopy (SEM) and transmission electron microscopy (MET). The results showed that mullite was synthesized with all solvents, however, the use of alcohols as a solvent provided the obtaining of the most crystalline samples, with the lowest mass losses, with a morphology formed by aggregates and individualized particles.

RESUMO Este trabalho objetivou imobilizar metais pesados presentes nos resíduos de quartzito por meio da incorporação em argamassas em substituição total ao agregado natural. Dois tipos de resíduos foram utilizados: os resíduos de fragmentação das aparas (QS) e os do pó de serragem (QP). Os resíduos foram caracterizados por fluorescência de raios X, difração de raios X e ensaios de toxidade conforme metodologia da Norma Brasileira (NBR) 10005, da NBR 10006 e do Toxicity Characteristic Leaching Procedure (TCLP) 1311. Então, foram analisadas composições de argamassas contendo cimento, cal e os resíduos (QS, QP) utilizando-se a técnica de delineamento de mistura, determinando os melhores traços, o melhor tipo de cura (imersa ou úmida) e, posteriormente, avaliando a resistência dos corpos de prova após cura. A caracterização do resíduo de quartzito revelou a presença de vários metais pesados e extratos lixiviados em contato com a água, classificando-o como resíduo de Classe I — Perigoso. Os resultados indicam que as composições determinadas foram capazes de imobilizar os metais pesados presentes nos resíduos de quartzitos, bem como resultou em argamassas com resistências mecânicas superiores a 2 MPa. Por fim, mostrou-se que essa técnica de solubilização e estabilização dos contaminantes presentes nos resíduos de quartzito é uma alternativa tecnologicamente viável e ambientalmente adequada para a destinação final desses resíduos.

ABSTRACT This work aims to immobilize heavy metals present in the quartzite residues by means of the incorporation in mortars in total substitution to the natural aggregate. Two types of residues were used: quartzite sand (QS) and powder (QP). The residues were characterized by x-ray fluorescence, x-ray diffraction, and toxicity tests according to the methodology of the NBR 10005, 10006 and Toxicity Characteristic Leaching Procedure (TCLP) 1311. Then, compositions of mortar containing cement, lime and residues (QS, QP) were analyzed using technique of designing the mixture, determining the best mixture, the best type of cure (immersed or wet), and subsequently evaluated at resistance of the body of evidences after curing. The characterization of quartzite residue revealed the presence of multiple heavy metals and leached extracts in contact with the water, classifying it a Class I–Hazardous waste. Regarding the production of mortars, the results indicated that the compositions determined were able to immobilize the heavy metals present in the quartzite residues, as well as resulted in mortars with mechanical resistances higher than 2 MPa. Finally, it was shown that this technique of solubilization and stabilization of contaminants present in quartzite residues is a technologically viable and environmentally adequate alternative for the final destination of these residues.

RESUMO Resíduos de MDF (MediumDensityFiberboard) gerados nas indústrias de móveis de madeiras, geralmente, são depositados em locais inadequados, causando impactos ambientais. Este trabalho teve como objetivo desenvolver materiais porosos com a incorporação de resíduo de MDF (5, 10 e 15% de resíduo) em massas cerâmicas estruturais. As características mineralógicas, químicas e térmicas das massas foram analisadas. Corpos de prova (50mm x15mm x 5mm) foram conformados por prensagem uniaxial (13,3 MPa), os quais foram secos à 110 ºC/24 h e sinterizados à 750, 850 e 950 °C. Posteriormente, estes foram submetidos às seguintes caracterizações: absorção de água, densidade aparente, porosidade aparente e módulo de ruptura à flexão. As características mineralógicas e microestruturais, após queima, também foram analisadas. Os resultados evidenciaram que, até 10% do resíduo de MDF em forma de pó, poderá ser incorporado em massas cerâmicas estruturais para produção de materiais cerâmicos, como blocos porosos isolantes acústicos e térmicos. A porosidade aparente foi de 31,7%, a densidade aparente foi de 1,6 g/cm3 e o módulo de ruptura a flexão foi de 11,5 MPa.

ABSTRACT MDF industrial wastes (Medium Density Fiberboard) generated in the wood furniture industries, have been causing serious environmental impacts, since their improperly disponishment in the nature. In light of this, the purpose of this work is to develop new structural ceramic compositions, containing 5, 10 and 15% by mass of MDF waste. The mineralogical, chemical and thermal characteristics of the masses were analyzed. Test bodies (50mm x15mm x 5mm) were shaped by uniaxial press (13.3 MPa), which were dried at 110º C/24h and sintered at 750, 850 and 950 °C. Subsequently, these were subjected to the following characterizations: Water absorption, apparent density, apparent porosity and flexion rupture module. The mineralogical and microstructural characteristics, after firing, were also analyzed. The results showed that up to 10% of the residue of MDF in the form of powder could be incorporated into structural ceramic masses for the productions of ceramic materials, such as acoustic and thermal insulation porous bricks. The apparent porosity was 31.7 %, bulk density was 1.6 g/cm3, the flexural strength was 11.5 MPa.

RESUMO Os resíduos de rochas ornamentais, especialmente quartzito, causam grande impacto ambiental. Mais impulso tem sido dado à pesquisa sobre a reciclagem desses resíduos nos últimos anos, particularmente para uso como agregados em concreto e argamassa. No entanto, os estudos realizados até o momento não mencionam o comportamento da argamassa misturada com agregados provenientes de resíduos de rochas ornamentais quando submetidos a ataques químicos em ambientes ricos em sulfato. Assim, no presente trabalho buscou-se adicionar resíduos de quartzito à argamassa, verificando seu comportamento mecânico e sua durabilidade quando atacado por sulfato de sódio (Na2SO4). A durabilidade da argamassa mesclada com resíduos de quartzito sob ataque de sulfato foi avaliada pela variação dimensional dos corpos de prova quando imersos em solução de sulfato de sódio, de acordo com a metodologia da norma NBR 13583. Utilizaram-se as seguintes técnicas complementares: resistência à compressão simples, difração de raios X e análise termogravimétrica e diferencial. A partir dos ensaios verificou-se que as argamassas, após ataque de sulfato de sódio, apresentaram expansões dimensionais superiores a 0,06%, bem como aumento da resistência mecânica. Portanto, embora tenha sido constatado que os corpos de prova incorporados com resíduos de quartzito tenham sofrido ataques por sulfato, observou-se que não foi capaz de formar etringita secundária suficiente para deteriorar mecanicamente os corpos de prova submetidos ao ataque de sulfato de sódio.

ABSTRACT The residues of ornamental rocks, especially quartzite, cause great environmental impact. More impulse has been given to research on the recycling of these residues over the last years, particularly for use as aggregates in concrete and mortar. Nevertheless, the studies conducted so far do not mention the behavior of the mortar blended with aggregates coming from residues of ornamental rocks when under chemical attacks in sulfate-rich environment. Thus, in the present study it was sought to add quartzite residues to the mortar, verifying its mechanical behavior and its durability when attacked by sodium sulfate (Na2SO4). The durability of the mortar blended with quartzite residues under sulfate attack was evaluated by the dimensional variation of the test specimens when immersed in sodium sulfate solution, according to the methodology of the NBR 13583 standard. Were used the following complementary techniques: simple compressive strength, X-ray diffraction and thermogravimetric and differential analysis. From the tests, it was verified that the mortars, after attack of sodium sulfate, presented dimensional expansions superior to 0.06%, as well as increased mechanical strength. Therefore, although it was found that the specimens incorporated with quartzite residues were attacked by sulfate, it was observed that it was not able to form sufficient secondary ettringite to mechanically damage the specimens submitted to the sodium sulfate attack.

The purpose of this work was to produce submicrometric hydroxyapatite (HA) and beta-tricalcium phosphate (β-TCP) biphasic fibers by means of solution blow spinning (SBS). This method was chosen due to its lower cost and higher production rate than those of electrospinning, which is normally employed in ceramic fiber production. The fibers thus obtained were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and thermogravimetric analysis (TGA). The in vitro bioactivity and cytotoxicity of the fibers were also investigated. The XRD patterns indicated the formation of biphasic HA/βTCP fibers. SEM analysis revealed an interconnected cylindrical morphology with the presence of beads. Fiber diameters in the submicrometric range varied from 374 to 451 nm. TGA results indicated that organic losses occurred solely below 600ºC. All the fibers were non-cytotoxic, presenting an inhibitory concentration (IC) of > IC50. All the samples successfully formed acicular apatite layers when immersed in SBF, indicating a high potential for in vivo bone bioactivity.

The influence of MgO and La2O3 on the fast sintering of mullite was evaluated in this work. High-purity mullite was doped with MgO and La2O3, conventionally sintered, fast sintered, and microwave-sintered in rapid sintering cycles. The results showed that MgO and La2O3 strongly affected the densification of fast sintered samples; and only doped bodies reached high densities when fast sintered. However, the densification behavior of doped samples was dependent on the amount of sintering aids. MgO doped samples presented better densification behavior than La2O3 doped samples. Microwave-processed samples required a balance between power, time and amount of additives to obtain highly dense and homogenous microstructures.

In the present work the effect of the microwave hybrid fast sintering of mullite-Al2O3 with non-stoichiometric mullite composition was investigated. Samples were fast sintered using a range of microwave power from 1.2 to 2.1 kW. The mullitization process of the silica-rich composition was faster than that of the alumina-rich composition. Alumina-rich mullite showed higher densities and smaller grain size than alumina-poor mullite. It was concluded that the microwave hybrid sintering of mullite was very sensitive to composition.

Este trabalho tem como objetivo a análise da viabilidade técnica na incorporação de Cinza de Casca de Arroz (CCA), Lodo de Estação de Tratamento de Água (LETA) e Cinza de Lenha (CL) para massa cerâmica utilizada para cerâmica de revestimento. A metodologia consistiu na análise das propriedades tecnológicas de várias composições. Foram confeccionados corpos-de-prova por prensagem, com composições de 0 a 50% de resíduo e 50 a 100% de argila. A queima foi feita em forno tipo mufla. As propriedades analisadas foram solubilidade e lixiviação (caracterização ambiental), absorção de água e módulo de ruptura a flexão. Como resultados, concluiu-se ser viável a utilização de até 25% dos resíduos nas temperaturas de 1000ºC, 1100ºC e 1150ºC.

This paper presents a technical feasibility analysis of the incorporation of Rice Husk Ash (RHA), Sludge from Water Treatment Station (SWTS) and Wood Ash (WA) in clay for the mass used in ceramic coating. The methodology involved analyzing the technological properties of various compositions. Samples were prepared for pressing, with compositions from 0 to 50% waste and 50 to 100% clay. The sintering was carried out in a muffle furnace. The properties studied were: solubility and leaching (environmental characterization), water absorption and rupture strength modulus. It was concluded that the best condition was the use of up to 25% of the residuals at temperatures of 1000 ºC, 1100 ºC and 1150 ºC.

Commercially available alumina powder with high-purity submicrometer particle size and narrow particle size distribution was fully densified by a microwave hybrid fast firing technique. The alumina compacts were surrounded by susceptor material, which helped the heating of the samples, and sintered in a microwave oven at a frequency of 2.45 GHz and a power level of 1.8 kW. The sintered samples reached densities of 99% in sintering cycles of 30 to 40 minutes, a much shorter time than conventional sintering processes. The sintered samples showed uniform microstructures with powder particle size/average grain size rations higher than 1:2.

Mineral extraction and processing industries have been cited as sources of environmental contamination and pollution. However, waste recycling represents an alternative recovery option, which is interesting from an environmental and economic standpoint. In this work, recycling of kaolin processing waste in the manufacture of mullite-based ceramics was investigated based on the statistical design of mixture experiments methodology. Ten formulations using kaolin processing waste, alumina and ball clay were used in the experiment design. Test specimens were fired and characterized to determine their water absorption and modulus of rupture. Regression models were calculated, relating the properties with the composition. The significance and validity of the models were confirmed through statistical analysis and verification experiments. The regression models were used to analyze the influence of waste content on the properties of the fired bodies. The results indicated that the statistical design of mixture experiments methodology can be successfully used to optimize formulations containing large amount of wastes.

O caulim é um material com vasta gama de aplicações nos mais diversos setores industriais, como a indústria de papel e a cerâmica. No entanto, sua extração e beneficiamento provocam a geração de enorme quantidade de resíduos. Assim, esse trabalho tem por objetivo analisar a utilização do resíduo do beneficiamento do caulim como matéria-prima alternativa em argamassas para a construção civil. O resíduo foi caracterizado através da determinação de sua composição química, difração de raios X e determinação da distribuição granulométrica. Foram formuladas argamassas substituindo parcialmente a cal hidratada por resíduo. Em seguida, foram confeccionados corpos-de-prova e determinada sua resistência à compressão simples e à tração indireta. A substituição da cal por adições de até 20% de resíduo de caulim possibilitou o aumento da resistência das argamassas estudadas em até 80%. Com base nos resultados, pode-se concluir que o resíduo de caulim pode ser utilizado para a produção de argamassas para construção civil com propriedades mecânicas de acordo com a normalização e que a adição do resíduo pode melhorar a resistência mecânica das argamassas convencionais.

Kaolin is a material used in a wide range of applications in many industrial sectors, as the paper and the ceramic industry. However, the kaolin processing industry generates large amounts of waste. Thus, the aim of this work is to evaluate the kaolin processing waste suitability as an alternative raw material for the production of mortars. The waste was characterized by determining its chemical composition, particle size distribution, and X-ray diffraction. Mortars were prepared by partially substituting kaolin waste for hydrated lime. Test specimens were prepared and their compression and indirect tension strength determined. The substitution of the lime by additions of up to 20% of kaolin waste improved the mechanical strength of masonry mortars up to 80%. The mechanical properties of the alternative mortars are in accordance with standard values, which indicated that it is possible to use kaolin waste for the production of mortars. Moreover, the waste addition may improve the mechanical properties of the conventional mortars.