Biocompatibility of a porous alumina ceramic scaffold coated with hydroxyapatite and bioglass

This study aimed to evaluate the osteointegration and genotoxic potential of a bioactive scaffold, composed of alumina and coated with hydroxyapatite and bioglass, after their implantation in tibias of rats. For this purpose, Wistar rats underwent surgery to induce a tibial bone defect, which was filled with the bioactive scaffolds. Histology analysis (descriptive and morphometry) of the bone tissue and the single-cell gel assay (comet) in multiple organs (blood, liver, and kidney) were used to reach this aim after a period of 30, 60, 90, and 180 days of material implantation. The main findings showed that the incorporation of hydroxyapatite and bioglass in the alumina scaffolds produced a suitable environment for bone ingrowth in the tibial defects and did not demonstrate any genotoxicity in the organs evaluated in all experimental periods. These results clearly indicate that the bioactive scaffolds used in this study present osteogenic potential and still exhibit local and systemic biocompatibility. These findings are promising once they convey important information about the behavior of this novel biomaterial in biological system and highlight its possible clinical application. © 2013 Wiley Periodicals, Inc.

Mechanical properties of vulcanized natural rubber nanocomposites containing functional ceramic nanoparticles

Rubber nanocomposites containing different concentrations of ferroelectric and paramagnetic nanoparticles were fabricated. Nanostructures of ferroelectric potassium strontium niobate and paramagnetic nickel-zinc ferrite were synthesized using a modified polyol method. The nanoparticle characterization was carried out by transmission electron microscopy and X-ray diffraction, showing that the materials were produced with nanometer dimensions, specific crystallinity and microstrain. Mechanical tests such as hardness type Shore A, stress-strain and compression resistance were performed. They showed that increasing the concentration of nanoparticles enhance the rigidity of vulcanized films of natural rubber and this change is more pronounce for the nanocomposites formed with ferrite nanoparticles, likely due to the effect of its morphological and surface properties. © 2013 by American Scientific Publishers.

Optical properties of the MoO3-TiO2 particulate system and its use as a ceramic pigment

Mo-doped TiO2 powders were prepared using a dry mixture of TiO2 and MoO3 oxides with several compositions, followed by a calcination step at several temperatures. The resulting oxide system develops yellow and green tones. The XRD patterns showed only traces of MoO 3; however, EDS results, combined with TG/DTA data, confirmed the presence of molybdenum ions, suggesting that the changes in optical properties of the oxide system is due to the incorporation of Mo ions into the TiO 2 matrix, substituting Ti+4 with Mo+6 ions. The band gap decreased with increasing of MoO3 content; on the other hand, the band gap reached a maximum value at about 850°C to 910°C when plotted as a function of the calcination temperature. The glazes produced showed that the oxide system under study is a potential material for use as abinary ceramic pigment. Copyright © 2013 Taylor & Francis Group, LLC.

The impact of hydrofluoric acid etching followed by unfilled resin on the biaxial strength of a glass-ceramic

Objectives: To evaluate the null hypotheses that hydrofluoric (HF) acid etching time would neither decrease the biaxial flexural strength of a glass-based veneering ceramic nor enhance it after silane and unfilled resin (UR) applications. Methods: Disc-shaped IPS e.max ZirPress specimens were allocated into 12 groups: G1-control (no-etching), G2-30 s, G3-60 s, G4-90 s, G5-120 s, G6-60 s + 60 s. Groups (G7-G12) were treated in the same fashion as G1-G6, but followed by silane and UR applications. Surface morphology and roughness (Ra and Rq) of the ceramics were assessed by means of scanning electron microscopy (SEM) and profilometry, respectively. Flexural strength was determined by biaxial testing. Data were analyzed by two-way ANOVA and the Sidak test (α = 0.05). Weibull statistics were estimated and finite element analysis (FEA) was carried out to verify the stress concentration end areas of fracture. Results: The interaction (etching time vs. surface treatment) was significant for Ra (p = 0.008) and Rq (0.0075). Resin-treated groups presented significantly lower Ra and Rq than non-treated groups, except for the 60 s group (p < 0.005). SEM revealed that etching affected the ceramic microstructure and that the UR was able to penetrate into the irregularities. A significant effect of etching time (p = 0.029) on flexural strength was seen. G7-G12 presented higher strength than G1-G6 (p < 0.0001). None of experimental groups failed to show 95% confidence intervals of σ 0 and m overlapped. FEA showed lower stress concentration after resin treatment. Significance: HF acid etching time did not show a damaging effect on the ceramic flexural strength. Moreover, the flexural strength could be enhanced after UR treatment. © 2013 Academy of Dental Materials.

Air-particle abrasion on zirconia ceramic using different protocols: Effects on biaxial flexural strength after cyclic loading, phase transformation and surface topography

This study evaluated the effect of different air-particle abrasion protocols on the biaxial flexural strength and structural stability of zirconia ceramics. Zirconia ceramic specimens (ISO 6872) (Lava, 3M ESPE) were obtained (N=336). The specimens (N=118, n=20 per group) were randomly assigned to one of the air-abrasion protocols: Gr1: Control (as-sintered); Gr2: 50 μm Al2O3 (2.5 bar); Gr3: 50 μm Al2O3 (3.5 bar); Gr4: 110 μm Al2O3(2.5 bar); Gr5: 110 μm Al2O3 (3.5 bar); Gr6: 30 μm SiO2 (2.5 bar) (CoJet); Gr7: 30 μm SiO2(3.5 bar); Gr8: 110 μm SiO2 (2.5 bar) (Rocatec Plus); and Gr9: 110 μm SiO2 (3.5 bar) (duration: 20 s, distance: 10 mm). While half of the specimens were tested immediately, the other half was subjected to cyclic loading in water (100,000 cycles; 50 N, 4 Hz, 37 °°C) prior to biaxial flexural strength test (ISO 6872). Phase transformation (t→m), relative amount of transformed monoclinic zirconia (FM), transformed zone depth (TZD) and surface roughness were measured. Particle type (p=0.2746), pressure (p=0.5084) and cyclic loading (p=0.1610) did not influence the flexural strength. Except for the air-abraded group with 110 μm Al2O3 at 3.5 bar, all air-abrasion protocols increased the biaxial flexural strength (MPa) (Controlnon-aged: 1030±153, Controlaged: 1138±138; Experimentalnon-aged: 1307±184-1554±124; Experimentalaged: 1308±118-1451±135) in both non-aged and aged conditions, respectively. Surface roughness (Ra) was the highest with 110 μm Al2O3(0.84 μm. FM values ranged from 0% to 27.21%, higher value for the Rocatec Plus (110 μm SiO2) and 110 μm Al2O3 groups at 3.5 bar pressure. TZD ranged between 0 and 1.43 μm, with the highest values for Rocatec Plus and 110 μm Al2O3 groups at 3.5 bar pressure. © 2013 Elsevier Ltd.

Local order of Pb1-xLaxZr0.40Ti 0.60O3 ferroelectric ceramic materials probed by X-ray absorption and Raman spectroscopies

This paper reports on the structural characterization of Pb 1-xLaxZr0.40Ti0.60O3 (PLZT) ferroelectric ceramic compositions prepared by the conventional solid state reaction method. X-ray absorption spectroscopy (XAS) and Raman spectroscopy were used to probe the local structure of PLZT samples that exhibits a normal and relaxor ferroelectric behavior. From the Zr K-edge and Pb LIII-edge EXAFS spectra, a considerable dissymmetry of Zr and Pb sites was observed in all samples, including those showing a long-range order cubic symmetry and a relaxor behavior. The Raman spectroscopy results confirmed the existence of a local disorder in all PLZT samples through the observation of Raman active vibrational modes. The variation in the intensity of the E(TO 3) mode in the PLZT relaxor samples indicates that the process of correlation between nanodomains stabilizes at temperatures lower than T m. © 2013 Elsevier B.V. All rights reserved.

Estudo da formação de espumas cerâmicas à base de zircônio a partir do processo sol-gel

Pós-graduação em Química - IQ

Mineralogy and chemistry of archaeological ceramic fragments from archaeological Dark Earth site in Colombian Amazon

Vários sítios arqueológicos de Terra Preta Arqueológica (TPA) encontrados na floresta Amazônica Colombiana também contêm alto conteúdo de fragmentos cerâmicos semelhantes aqueles da Amazônia Brasileira, como mostra o sítio Quebrada Tacana. Seus fragmentos cerâmicos são amarelo a cinza, exibem matriz argilosa calcinada envolvendo fragmentos de cariapé, carvão e partículas de cinza, grãos de quartzo e micas. A matriz é composta de metacaulinita a material amorfo, quartzo, folhas de micas, clorita e sepiolita. Cariapé e cauixi são constituídos de cristobalita, da mesma forma o carvão e as cinzas. Embora não detectados pela difração de raios x, os fosfatos devem estar presentes, pois foram detectados teores de P2O5 de até 2,90 %, possivelmente como fosfatos de alumínio, já que o conteúdo de Ca está abaixo 0,1 %, o que elimina a possibilidade da presença de apatita. Estas características mineralógicas e químicas permitem relacionar estes fragmentos cerâmicos com aqueles encontrados nos sítios de TPA no Brasil e reforça o fósforo como um importante componente químico, originado pelo contato dos vasos cerâmicos com os alimentos do cotidiano dos povos amazônicos pré-históricos.

The ceramic artifacts in archaeological black earth (terra preta) from Lower Amazon Region, Brazil: chemistry and geochemical evolution

Neste trabalho realizou-se a caracterização química de fragmentos de artefatos cerâmicos encontrados em sítios arqueológicos com terra preta no Baixo Amazonas (Cachoeira-Porteira, Pará, Brasil), representativos da cultura Konduri (de 900 a 400 anos AP). Esses fragmentos são constituídos de SiO₂, Al₂O₃, Fe₂O₃, Na₂O e P₂O₅, sendo que SiO₂ e Al₂O₃, juntos, perfazem mais de 80 % em peso. Os teores de P₂O,₅ são relativamente elevados (2,37 % em média) sob a forma de (Al,Fe)-fosfatos, incomuns em cerâmicas vermelhas primitivas, mas encontrados em algumas cerâmicas arqueológicas egípcias e romanas. As concentrações dos elementos traços são comparáveis ou mesmo inferiores ao nível crustal, embora a composição total seja próxima a mesma. A composição química (exceto P₂O₅) em conjunto com os dados mineralógicos e texturais indicam material saprolítico derivado de rochas ígneas félsicas ou rochas sedimentares como matéria-prima das cerâmicas. Os teores de K, Ca e Na mostram que os feldspatos e fragmentos de rochas foram adicionados ao material argiloso, como sugerido pela mineralogia. Os altos teores de sílica respondem pela presença de cauixi, cariapé e/ou areias quartzosas. Fósforo deve ter sido incorporadoà matriz argilosa da cerâmica, quando do cozimento de alimentos nos vasos cerâmicos, e ainda, em parte, durante a formação do perfil de solo tipo ABE sobre Latossolos Amarelos. A matéria prima e os temperos (cauixi, cariapé, rochas trituradas e fragmentos de vasos cerâmicos descartados) encontram-se disponíveis próximos aos sítios até a atualidade, e, portanto foram a área fonte dos mesmos para a confecção dos artefatos cerâmicos.

The ceramic artifacts in archaeological black earth (terra preta) from lower Amazon region, Brazil: Mineralogy

Sítios arqueológicos com Terra Preta, denominados de Terra Preta de Índio ou ainda Terra Preta Arqueológica (TPA) são muito freqüentes na Amazônia. As TPA geralmente contém fragmentos de vasos cerâmicos, por vezes abundantes, além de líticos, que são materiais de grande importância para os estudos arqueológicos. Para consubstanciar esses estudos, realizou-se pesquisas mineralógicas e químicas em fragmentos cerâmicos provenientes de dois sítios arqueológicos da região de Cachoeira-Porteira, Estado do Pará. Os fragmentos foram classificados segundo seus principais temperos em: cauixi, cariapé, areia+feldspatos e caco de vaso cerâmico. Mineralogicamente são compostos de quartzo, minerais de argila calcinados (especialmente caulinita), feldspatos (albita e microclínio), hematita, goethita, maghemita, variscita-estrengita, fosfatos amorfos, anatásio, e raramente apatita, rhabdophana e óxidos de Mn e Ba. Cauixi e cariapé são componentes orgânicos silicosos e amorfos a DRX. A composição mineralógica e a morfologia dos seus grãos indicam saprólito (material argiloso rico em quartzo) derivado de rochas ígneas félsicas de granulação fina ou rochas sedimentares ricas em argilominerais como matéria-prima dos vasos cerâmicos. Neste material argiloso cauixi, cariapé e/ou areias, ricas em sílica, foram intencionalmente adicionados. O elevado conteúdo de fosfatos de Al-Fe, amorfos ou como de baixa cristalinidade, originou-se a partir do contato entre a matriz argilosa da parede do vaso cerâmico com a solução aquosa quente durante o cozimento diário de alimentos de origem animal (principal fonte de fósforo). A cristalização dos fosfatos deve ter prosseguida mesmo depois que os vasos foram descartados, e juntos com os restos de matéria orgânica vegetal e animal incorporaram-se aos solos residuais. Participaram desta forma na formação dos solos tipo TPA.

Chemical and mineralogical characterization of portuguese ceramic tiles in the historic center of São Luís do Maranhão (Brazil): an approximation of the mineralogy and firing temperature of the raw materials

Nesse trabalho, foram caracterizados, pela primeira vez, azulejos históricos portugueses do Centro Histórico de São Luís (CHSL) do Maranhão. A caracterização foi realizada através dos ensaios de microscopia ótica, difração de raios X (DRX) e análise química, visando ao uso dessa informação para a determinação das possíveis matérias-primas utilizadas na sua fabricação, bem como a provável temperatura de queima desses materiais. Os resultados mostraram que a microestrutura desses materiais é constituída por poros de tamanhos variados, apresentando incrustações de calcita e grãos de quartzo de tamanhos inferiores a 500 µm, distribuídos numa matriz de cor rosa-amarelo, onde foram identificadas, por DRX, as fases minerais calcita, gelhenita, wollastonita, quartzo e amorfo. A partir da informação obtida, é possível inferir que as matérias-primas originais estiveram constituídas, provavelmente, por mistura de argilas caoliníticas (Al₂O₃•2SiO,₂•2H₂O), ricas em carbonatos de cálcio e quartzo ou misturas de argilas caoliniticas, quartzo e calcita. Essas matérias-primas originais não atingiram a temperatura de cocção de 950ºC.

Ceramic raw materials from the State of Maranhão, Brazil. Part 1: chemical and mineralogical characterization and technological properties of clays from São Luis, Rosário, Pinheiro and Mirinzal

Nesse trabalho, foram caracterizadas algumas argilas coletadas nos municípios de São Luís, Rosário, Pinheiro e Mirinzal. A caracterização foi realizada através dos ensaios de difração de raios X, massa específica real, capacidade de troca de cátions (CTC), área superficial, distribuição granulométrica, análise química, análise térmica (TG-DTA) e limites de Atterberg. Ensaios tecnológicos de retração linear, antes e após a queima, absorção de água e tensão de ruptura a flexão, em três pontos, foram realizados em corpos de prova prensados uniaxialmente a 20 MPa e tratados termicamente em 850, 950, 1050, 1150 e 1250ºC. Os resultados obtidos permitiram identificar duas argilas de queima branca, constituídas de quartzo, caolim, feldspato e anatásio, com excelentes propriedades para uso em cerâmica branca. As restantes são queima vermelha e possuem composição mineralógica de quartzo, caolim, feldspato, montmorilonita, hematita e goetita. Estas últimas apresentaram valores moderados de plasticidade e são adequadas para aplicações em cerâmica vermelha.

Phase transitions and interface phenomena in the cryogenic temperature domain of a niobate nanostructured ceramic

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

Valorization of sugarcane bagasse ash: Producing glass-ceramic materials

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

Measurement of Radiant Energy using Pyroelectric Polymer/Ceramic Composite

Monitoring non-ionizing radiant energy is increasingly demanded for many applications such as automobile, biomedical and security system. Thermal type infrared (IR) sensors can operate at room temperature and pyroelectric materials have high sensitivity and accuracy for that application. Working as thermal transducer pyroelectric sensor converts the non-quantified thermal flux into the output measurable quantity of electrical charge, voltage or current. In the present study the composite made of poly(vinylidene fluoride) -PVDF and lead zirconate titanate (PZT) partially recovered with polyaniline (PAni) conductor polymer has been used as sensor element. The pyroelectric coefficient p(T) was obtained by measuring the pyroelectric reversible current, i.e., measuring the thermally stimulated depolarization current (TSDC) after removing all irreversible contribution to the current such as injected charge during polarization of the sample. To analyze the sensing property of the pyroelectric material, the sensor is irradiated by a high power light source (halogen lamp of 250 W) that is chopped providing a modulated radiation. A device assembled in the laboratory is used to change the light intensity sensor, an aluminum strip having openings with diameters ranging from 1 to 10 mm incremented by one millimeter. The sensor element is assembled between two electrodes while its frontal surface is painted black ink to maximize the light absorption. The signal from the sensor is measured by a Lock-In amplifier model SR530 -Stanford Research Systems. The behavior of the output voltage for an input power at several frequencies for PZT-PAni/PVDF (30/ 70 vol%) composite follows the inverse power law (1/ f) and the linearity can be observed in the frequency range used.