Effect of Nanosilica on Rheology, Fresh Properties, and Strength of Cement-Based Grouts

The effect of colloidal nanosilica on the fresh and rheological parameters, plastic shrinkage, heat of hydration, and compressive strength of cement-based grouts is investigated in this paper. The fresh and rheological properties were evaluated by the minislump flow, Marsh cone flow time, Lombardi plate cohesion meter, yield value, and plastic viscosity. The key parameters investigated were the dosages of nanosilica and superplasticizer and temperature of mixing water. Statistical models and isoresponse curves were developed to capture the significant trends. The dosage of nanosilica had a significant effect on the results. The increase in the dosage of nanosilica led to increasing the values of flow time, plate cohesion meter, yield stress, plastic viscosity, heat of hydration at 1 day and 3 days, and compressive strength at 1 day, while reducing the minislump, plastic shrinkage up 24 h, and compressive strength at 3, 7, and 28 days. Conversely, the increase in the dosage of superplasticizer led to decreasing the values of flow time, plate cohesion meter, yield stress, plastic viscosity, heat of hydration at 1 day and 3 days, and compressive strength at 1 day, while increasing the minislump, plastic shrinkage, and compressive strength at 3 and 7 days. Increasing the temperature of mixing water led to a notable increase in the results of minislump, flow time, plastic viscosity, heat of hydration at 3 days, and compressive strength at 1 day, while it reduced the plate cohesion, compressive strength at 3, 7, and 28 days. The statistical models developed in this study can facilitate optimizing the mixture proportions of grouts for target performance by reducing the number of trial batches needed.

Conductivity/activation energy relationships for cement-based materials undergoing cyclic thermal excursions

The electrical conductivity of a range of concrete mixes, with and without supplementary cementitious materials (SCM), is studied through multiple cycles of heating and cooling over the extended temperature range −30/+70 °C. When presented in an Arrhenius format, the experimental results display hysteresis effects at the low-temperature end of the thermal cycle and, in those concretes containing supplementary cementitious materials at higher water/binder ratios, hysteresis effects were evident over the entire temperature range becoming more discernible with increasing number of thermal cycles. The depression in both the freezing and thawing point could be clearly identified and was used to estimate pore-neck and pore-cavity radii. A simplified approach is presented to evaluate the volumetric ratio of frozen pore water in terms of conductivity measurements. The results also show that the conductivity and activation energy of the concrete specimens were related to the water/binder ratio, type of SCM, physical state of the pore water and the thermal cycling regime.

Internal curing in cement-based materials

O desenvolvimento de betões de elevado desempenho, durante o início da década de 80, revelou que este tipo particular de materiais com base em cimento é susceptível a problemas de cura. São bem conhecidos os efeitos dos fenómenos autogéneos em sistemas de elevado desempenho com base em cimento, nomeadamente a fissuração em idade jovem. Esta é, aliás vista como a maior limitação no desenvolvimento de novos materiais com durabilidade superior. Desenvolvimentos recentes de métodos de cura interna provaram ser uma boa estratégia de mitigação dos efeitos da auto-dissecação destes sistemas, onde a presente tese ganha o seu espaço no tempo. Este estudo centra-se essencialmente em sistemas de elevado desempenho com base em cimento com cura interna através de partículas superabsorventes, dando particular importância à alteração de volume em idade jovem. Da análise mais aprofundada deste método, resultam algumas limitações na sua aplicabilidade, especialmente em sistemas modificados com sílica de fumo. Conclui-se que a natureza física e química dos polímeros superabsorventes pode afectar significativamente a eficiência da cura interna. Em adição, os mecanismos de cura interna são discutidos mais profundamente, sendo que para além dos mecanismos baseados em fenómenos físicos e químicos, parecem existir efeitos mecânicos significativos. Várias técnicas foram utilizadas durante o decorrer desta investigação, com o objectivo, para além da caracterização de certas propriedades dos materiais, de perseguir as questões deixadas em aberto pela comunidade internacional, relativamente aos mecanismos que fundamentam a explicação dos fenómenos autogéneos. Como exemplo, são apresentados os estudos sobre hidratação dos sistemas para avaliação do problema numa escala microscópica, em vez de macroscópica. Uma nova técnica de cura interna emerge da investigação, baseada na utilização de agregados finos como veiculo para mitigar parcialmente a retracção autogénea. Até aqui, esta técnica não encontra par em investigação anterior, mas a extensão da cura interna ou a eficácia na mitigação baseada neste conceito encontra algumas limitações. A significância desta técnica em prevenir a micro fissuração é um aspecto que está ainda em aberto, mas pode concluir-se que os agregados finos podem ser benéficos na redução dos efeitos da restrição localizada no sistema, reduzindo o risco de micro fissuração. A utilização combinada de partículas finas de agregado e polímeros super absorventes pode ter como consequência betão sem microfissuração, ou pelo menos com nanofissuração.

Surface properties of eucalyptus pulp fibres as reinforcement of cement-based composites

The objective of the present work is to evaluate the effects of the surface properties of unrefined eucalyptus pulp fibres concerning their performance in cement-based composites. The influence of the fibre surface on the microstructure of fibre-cement composites was evaluated after accelerated ageing cycles, which simulate natural weathering. The surface of unbleached pulp is a thin layer that is rich in cellulose, lignin, hemicelluloses, and extractives. Such a layer acts as a physical and chemical barrier to the penetration of low molecular components of cement. The unbleached fibres are less hydrophilic than the bleached ones. Bleaching removes the amorphous lignin and extractives from the surface and renders it more permeable to liquids. Atomic force microscopy (AFM) helps in understanding the fibre-cement interface. Bleaching improved the fibre- cement interfacial bonding, whereas fibres in the unbleached pulp were less susceptible to the re-precipitation of cement hydration products into the fibre cavities (lumens). Therefore, unbleached fibres can improve the long-term performance of the fibre-cement composite owing to their delayed mineralization.

Physicochemical and mechanical properties of zirconium oxide and niobium oxide modified Portland cement-based experimental endodontic sealers

Aim: To evaluate the physicochemical and mechanical properties of Portland cement-based experimental sealers (ES) with different radiopacifying agents (zirconium oxide and niobium oxide micro- and nanoparticles) in comparison with the following conventional sealers: AH Plus, MTA Fillapex and Sealapex. Methodology: The materials were tested for setting time, compressive strength, flow, film thickness, radiopacity, solubility, dimensional stability and formaldehyde release. Data were subjected to anova and Tukey tests (P < 0.05). Results: MTA Fillapex had the shortest setting time and lowest compressive strength values (P < 0.05) compared with the other materials. The ES had flow values similar to the conventional materials, but higher film thickness (P < 0.05) and lower radiopacity (P < 0.05). Similarly to AH Plus, the ES were associated with dimensional expansion (P > 0.05) and lower solubility when compared with MTA Fillapex and Sealapex (P < 0.05). None of the endodontic sealers evaluated released formaldehyde after mixing. Conclusion: With the exception of radiopacity, the Portland cement-based experimental endodontic sealers presented physicochemical properties according to the specifications no 57 ANSI/ADA (ADA Professional Product Review, 2008) and ISO 6876 (Dentistry - Root Canal Sealing Materials, 2012, British Standards Institution, London, UK). The sealers had setting times and flow ability that was adequate for clinical use, satisfactory compressive strength and low solubility. Additional studies should be carried out with the purpose of decreasing the film thickness and to determine the ideal ratio of radiopacifying agents in Portland cement-based root canal sealers. © 2013 International Endodontic Journal.

Chemical characterization and bioactivity of epoxy resin and Portland cement-based sealers with niobium and zirconium oxide radiopacifiers

The purpose of this study was to characterize and to evaluate the bioactivity potential of experimental root canal sealers (ES) based on Portland cement, epoxy resin with nano- and micro-particles of niobium or zirconium oxide used as radiopacifiers in comparison to AH Plus and MTA Fillapex. Methods Specimens of the sealers (10 mm in diameter × 1 mm thick) were prepared and the radiopacity was evaluated according to ISO 6876 (2012) specifications. Characterization of the sealers was performed under the scanning electron microscope (SEM) immediately after setting and after immersion for 28 days in Hank's balanced salt solution (HBSS). In addition X-ray energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy were also performed. The pH and calcium ion release were measured after 1, 7, 14, 21 and 28 days after completion of seating using a digital pH meter and an atomic absorption spectrophotometer, respectively. Results The experimental sealers exhibited an average radiopacity of 2.5 mm thickness of aluminum, which was similar to MTA Fillapex (P > 0.05) and inferior to AH Plus (P < 0.05). AH Plus did not show bioactivity. Although the experimental sealers did not exhibit the formation of hydration product, they encouraged the deposition of crystalline spherical structures of calcium deficient phosphate. The highest pH and calcium release values were observed with the experimental sealers (P < 0.01). ES-Nb-micro was the only sealer to present hexagonal shaped crystal deposition. Significance Novel root canal sealers based on a mixture of Portland cement, epoxy resin and radiopacifier exhibited a degree of bioactivity although no evidence of cement hydration was demonstrated on material characterization. The radiopacifier particle size had limited effect on the sealer microstructure and chemical properties.

Non-conventional cement-based composites reinforced with vegetable fibers: a review of strategies to improve durability

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