Addition of Chlorhexidine Gluconate to a Glass Ionomer Cement: A Study on Mechanical, Physical and Antibacterial Properties

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Recycling leather waste: preparing and studying on the microstructure, mechanical, and rheological properties of leather waste/rubber composite

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

Recycling leather waste: preparing and studying on the microstructure, mechanical, and rheological properties of leather waste/rubber composite

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

Development and characterization of non-oxide ceramic composites for mechanical and tribological applications

The main reasons for the attention focused on ceramics as possible structural materials are their wear resistance and the ability to operate with limited oxidation and ablation at temperatures above 2000°C. Hence, this work is devoted to the study of two classes of materials which can satisfy these requirements: silicon carbide -based ceramics (SiC) for wear applications and borides and carbides of transition metals for ultra-high temperatures applications (UHTCs). SiC-based materials: Silicon carbide is a hard ceramic, which finds applications in many industrial sectors, from heat production, to automotive engineering and metals processing. In view of new fields of uses, SiC-based ceramics were produced with addition of 10-30 vol% of MoSi2, in order to obtain electro conductive ceramics. MoSi2, indeed, is an intermetallic compound which possesses high temperature oxidation resistance, high electrical conductivity (21·10-6 Ω·cm), relatively low density (6.31 g/cm3), high melting point (2030°C) and high stiffness (440 GPa). The SiC-based ceramics were hot pressed at 1900°C with addition of Al2O3-Y2O3 or Y2O3-AlN as sintering additives. The microstructure of the composites and of the reference materials, SiC and MoSi2, were studied by means of conventional analytical techniques, such as X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (SEM-EDS). The composites showed a homogeneous microstructure, with good dispersion of the secondary phases and low residual porosity. The following thermo-mechanical properties of the SiC-based materials were measured: Vickers hardness (HV), Young’s modulus (E), fracture toughness (KIc) and room to high temperature flexural strength (σ). The mechanical properties of the composites were compared to those of two monolithic SiC and MoSi2 materials and resulted in a higher stiffness, fracture toughness and slightly higher flexural resistance. Tribological tests were also performed in two configurations disco-on-pin and slideron cylinder, aiming at studying the wear behaviour of SiC-MoSi2 composites with Al2O3 as counterfacing materials. The tests pointed out that the addition of MoSi2 was detrimental owing to a lower hardness in comparison with the pure SiC matrix. On the contrary, electrical measurements revealed that the addition of 30 vol% of MoSi2, rendered the composite electroconductive, lowering the electrical resistance of three orders of magnitude. Ultra High Temperature Ceramics: Carbides, borides and nitrides of transition metals (Ti, Zr, Hf, Ta, Nb, Mo) possess very high melting points and interesting engineering properties, such as high hardness (20-25 GPa), high stiffness (400-500 GPa), flexural strengths which remain unaltered from room temperature to 1500°C and excellent corrosion resistance in aggressive environment. All these properties place the UHTCs as potential candidates for the development of manoeuvrable hypersonic flight vehicles with sharp leading edges. To this scope Zr- and Hf- carbide and boride materials were produced with addition of 5-20 vol% of MoSi2. This secondary phase enabled the achievement of full dense composites at temperature lower than 2000°C and without the application of pressure. Besides the conventional microstructure analyses XRD and SEM-EDS, transmission electron microscopy (TEM) was employed to explore the microstructure on a small length scale to disclose the effective densification mechanisms. A thorough literature analysis revealed that neither detailed TEM work nor reports on densification mechanisms are available for this class of materials, which however are essential to optimize the sintering aids utilized and the processing parameters applied. Microstructural analyses, along with thermodynamics and crystallographic considerations, led to disclose of the effective role of MoSi2 during sintering of Zrand Hf- carbides and borides. Among the investigated mechanical properties (HV, E, KIc, σ from room temperature to 1500°C), the high temperature flexural strength was improved due to the protective and sealing effect of a silica-based glassy phase, especially for the borides. Nanoindentation tests were also performed on HfC-MoSi2 composites in order to extract hardness and elastic modulus of the single phases. Finally, arc jet tests on HfC- and HfB2-based composites confirmed the excellent oxidation behaviour of these materials under temperature exceeding 2000°C; no cracking or spallation occurred and the modified layer was only 80-90 μm thick.

Ab initio quantum mechanical investigation of structural and chemical-physical properties of selected minerals for minero-petrological, structural ceramic and biomaterial applications

The purpose of this thesis is the atomic-scale simulation of the crystal-chemical and physical (phonon, energetic) properties of some strategically important minerals for structural ceramics, biomedical and petrological applications. These properties affect the thermodynamic stability and rule the mineral-environment interface phenomena, with important economical, (bio)technological, petrological and environmental implications. The minerals of interest belong to the family of phyllosilicates (talc, pyrophyllite and muscovite) and apatite (OHAp), chosen for their importance in industrial and biomedical applications (structural ceramics) and petrophysics. In this thesis work we have applicated quantum mechanics methods, formulas and knowledge to the resolution of mineralogical problems ("Quantum Mineralogy”). The chosen theoretical approach is the Density Functional Theory (DFT), along with periodic boundary conditions to limit the portion of the mineral in analysis to the crystallographic cell and the hybrid functional B3LYP. The crystalline orbitals were simulated by linear combination of Gaussian functions (GTO). The dispersive forces, which are important for the structural determination of phyllosilicates and not properly con-sidered in pure DFT method, have been included by means of a semi-empirical correction. The phonon and the mechanical properties were also calculated. The equation of state, both in athermal conditions and in a wide temperature range, has been obtained by means of variations in the volume of the cell and quasi-harmonic approximation. Some thermo-chemical properties of the minerals (isochoric and isobaric thermal capacity) were calculated, because of their considerable applicative importance. For the first time three-dimensional charts related to these properties at different pressures and temperatures were provided. The hydroxylapatite has been studied from the standpoint of structural and phonon properties for its biotechnological role. In fact, biological apatite represents the inorganic phase of vertebrate hard tissues. Numerous carbonated (hydroxyl)apatite structures were modelled by QM to cover the broadest spectrum of possible biological structural variations to fulfil bioceramics applications.

Local degradation of structural, mechanical, electrical and chemical properties of membrane electrode assembly in polymer electrolyte fuel cell

Polymer electrolyte fuel cell (PEMFC) is promising source of clean power in many applications ranging from portable electronics to automotive and land-based power generation. However, widespread commercialization of PEMFC is primarily challenged by degradation. The mechanisms of fuel cell degradation are not well understood. Even though the numbers of installed units around the world continue to increase and dominate the pre-markets, the present lifetime requirements for fuel cells cannot be guarantee, creating the need for a more comprehensive knowledge of material’s ageing mechanism. The objective of this project is to conduct experiments on membrane electrode assembly (MEA) components of PEMFC to study structural, mechanical, electrical and chemical changes during ageing and understanding failure/degradation mechanism. The first part of this project was devoted to surface roughness analysis on catalyst layer (CL) and gas diffusion layer (GDL) using surface mapping microscopy. This study was motivated by the need to have a quantitative understanding of the GDL and CL surface morphology at the submicron level to predict interfacial contact resistance. Nanoindentation studies using atomic force microscope (AFM) were introduced to investigate the effect of degradation on mechanical properties of CL. The elastic modulus was decreased by 45 % in end of life (EOL) CL as compare to beginning of life (BOL) CL. In another set of experiment, conductive AFM (cAFM) was used to probe the local electric current in CL. The conductivity drops by 62 % in EOL CL. The future task will include characterization of MEA degradation using Raman and Fourier transform infrared (FTIR) spectroscopy. Raman spectroscopy will help to detect degree of structural disorder in CL during degradation. FTIR will help to study the effect of CO in CL. XRD will be used to determine Pt particle size and its crystallinity. In-situ conductive AFM studies using electrochemical cell on CL to correlate its structure with oxygen reduction reaction (ORR) reactivity

Microstructural and mechanical characterization of contemporary lingual orthodontic brackets.

OBJECTIVES To investigate the composition and the microstructural and mechanical characterization of three different types of lingual brackets. MATERIALS AND METHODS Incognito™ (3M Unitek), In-Ovation L (DENTSPLY GAC) and STb™ (Light Lingual System, ORMCO) lingual brackets were studied under the scanning electron microscope employing backscattered electron imaging and their elemental composition was analysed by energy-dispersive X-ray microanalysis. Additionally, Vickers hardness was assessed using a universal hardness-testing machine, and the indentation modulus was measured according to instrumented indentation test. Two-way analysis of variance was conducted employing bracket type and location (base and wing) as discriminating variable. Significant differences among groups were allocated by post hoc Student-Newman-Keuls multiple comparison analysis at 95% level of significance. RESULTS Three different phases were identified for Incognito and In-Ovation L bracket based on mean atomic number contrast. On the contrary, STb did not show mean atomic contrast areas and thus it is recognized as a single phase. Incognito is a one-piece bracket with the same structure in wing and base regions. Incognito consists mainly of noble metals while In-Ovation L and STb show similar formulations of ferrous alloys in wing and base regions. No significant differences were found between ferrous brackets in hardness and modulus values, but there were significant differences between wing and base regions. Incognito illustrated intermediate values with significant differences from base and wing values of ferrous brackets. CONCLUSIONS/IMPLICATIONS Significant differences exist in microstructure, elemental composition, and mechanical properties among the brackets tested; these might have a series of clinical implications during mechanotherapy.

Influence of cement properties in the reaction rate and mechanical behavior of concrete with high fl y ash content

The use of fly ash (FA) as an admixture to concrete is broadly extended for two main reasons: the reduction of costs that supposes the substitution of cement and the micro structural changes motivated by the mineral admixture. Regarding this second point, there is a consensus that considers that the ash generates a more compact concrete and a reduction in the size of the pore. However, the measure in which this contributes to the pozzolanic activity or as filler is not well defined. There is also no justification to the influence of the physical parameters, fineness of the grain and free water, in its behavior. This work studies the use of FA as a partial substitute of the cement in concretes of different workability (dry and wet) and the influence in the reactivity of the ash. The concrete of dry consistency which serves as reference uses a cement dose of 250 Kg/m 3 and the concrete of fluid consistency utilized a dose of cement of 350 Kg/m 3 . Two trademark of Portland Cement Type 1 were used. The first reached the resistant class for its fineness of grain and the second one for its composition. Moreover, three doses of FA have been used, and the water/binder ratio was constant in all the mixtures. We have studied the mechanical properties and the micro-structure of the concretes by means of compressive strength tests, mercury intrusion porosimetry (MIP) and thermal analysis (TA). The results of compressive strength tests allow us to observe that concrete mixtures with cements of the same classification and similar dosage of binder do not present the same mechanical behavior. These results show that the effective water/binder ratio has a major role in the development of the mechanical properties of concrete. The study of different dosages using TA, thermo-gravimetry and differential thermal analysis, revealed that the portlandite content is not restrictive in any of the dosages studied. Again, this proves that the rheology of the material influences the reaction rate and content of hydrated cement products. We conclude that the available free water is determinant in the efficiency of pozzolanic reaction. It is so that in accordance to the availability of free water, the ashes can react as an active admixture or simply change the porous distribution. The MIP shows concretes that do not exhibit significant changes in their mechanical behavior, but have suffered significant variation in their porous structure

Mechanical Characterization of Multicrystalline Silicon Substrates for Solar Cell Applications

The possibility of using more economical silicon feedstock, i.e. as support for epitaxial solar cells, is of interest when the cost reduction and the properties are attractive. We have investigated the mechanical behaviour of two blocks of upgraded metallurgical silicon, which is known to present high content of impurities even after being purified by the directional solidification process. These impurities are mainly metals like Al and silicon compounds. Thus, it is important to characterize their effect in order to improve cell performance and to ensure the survival of the wafers throughout the solar value chain. Microstructure and mechanical properties were studied by means of ring on ring and three point bending tests. Additionally, elastic modulus and fracture toughness were measured. These results showed that it is possible to obtain marked improvements in toughness when impurities act as microscopic internal crack arrestors. However, the same impurities can be initiators of damage due to residual thermal stresses introduced during the crystallization process.

Mechanical characterization of multicrystalline silicon wafers

The possibility of using more economical silicon feedstock, i.e. as support for epitaxial solar cells, is of interest when the cost reduction and the properties are attractive. We have investigated the mechanical behavior of two blocks of upgraded metallurgical silicon, which is known to present high content of impurities even after being purified by the directional solidification process. The impurities are mainly metals like Al and silicon compounds. Thus, it is important to characterize their effect in order to improve cell performance and to ensure the survival of the wafers throughout the solar value chain. Microstructure and mechanical properties were studied by means of ring on ring and three point bending tests. Additionally, Young’s modulus, hardness and fracture toughness were measured. These results showed that it is possible to obtain marked improvements in toughness when impurities act as microscopic internal crack arrestors. However, the same impurities can be initiators of damage due to residual thermal stresses introduced during the crystallization process.

Influence of proportion and particle size gradation of rubber from end-of-life tires on mechanical, thermal and acoustic properties of plaster-rubber mortars

This work presents the main experimental results obtained from the study of plaster test pieces and boards with addition of various volumetric rubber fractions from mechanical grinding of end-of-life tires (ELTs), in three different particle size gradations. It includes a description of the materials employed, and their proportions. The physical and mechanical properties, as well as the thermal conductivity and acoustic insulation properties are analyzed. Experimental results obtained for specimens with addition of recycled rubber are compared with similar ones, carried out on specimens of plaster of identical features without any addition, evaluating the influence of the particle size and mixture proportions. An improvement in thermal and acoustic performance has been obtained as well as a reduction in density, and as a result, some constructive applications for paving and slabs in rehabilitation works are proposed.

Microstructural and mechanical characterization of annealed tungsten (W) and potassium-doped tungsten foils

Here we show that potassium-doped tungsten foil should be preferred to pure tungsten foil when considering tungsten laminate pipes for structural divertor applications. Potassium-doped tungsten materials are well known from the bulb industry and show an enhanced creep and recrystallization behaviour that can be explained by the formation of potassium-filled bubbles that are surrounding the elongated grains, leading to an interlocking of the microstructure. In this way, the ultra-fine grained (UFG) microstructure of tungsten foil can be stabilized and with it the extraordinary mechanical properties of the foil in terms of ductility, toughness, brittle-to-ductile transition, and radiation resistance. In this paper we show the results of three-point bending tests performed at room temperature on annealed pure tungsten and potassium-doped tungsten foils (800, 900, 1000, 1100, 1200, 1300, 1400, 1600, 1800, 2000, 2200, and 2400 °C for 1 h in vacuum). The microstructural assessment covers the measurement of the hardness and analyses of fractured surfaces as well as a comparison of the microstructure by optical microscopy. The results show that there is a positive effect of potassium-doped tungsten foils compared to pure tungsten foil and demonstrate the potential of the doped foil

Mechanical, thermal and colorimetric properties of LLDPE coloured with a blue nanopigment and conventional blue pigments

Purpose – This research deals with a new kind of nanopigment, obtained from the combination of organic dyes and layered nanoclays, that the authors call nanoclay-colorant pigment (NCP). Whilst they have already been employed in inks and coatings, to date these nanopigments have not been used as pigments for polymers. The existing lack of knowledge surrounding them must be redressed in order to bridge the gap between current academic studies and commercial exploitation. Therefore, the main purpose of this paper is to examine the hitherto unknown aspects of the NCP, which relate specifically to their applicability as a new type of colorant for polymers. Design/methodology/approach – A blue NCP has been prepared at the laboratory according to the patented method of synthesis (patent WO0104216), using methylene blue and montmorillonite nanoclay. It has then been applied to a thermoplastic polymer (linear low-density polyethylene – LLDPE) to obtain a coloured sample. Furthermore, samples with the same polymer but using conventional blue colorants have been prepared under the same processing conditions. The mechanical, thermal and colorimetric properties of these materials have been compared. Findings – The thermal stability of the sample coloured with NCP is reduced to some extent, while the mechanical strength is slightly increased. Moreover, this sample has better colour performance than the conventionally pigmented samples. Originality/value – In this paper, a blue NCP has been synthesised and successfully employed with polyethylene and the obtained sample shows better colour performance than polyethylene with conventional pigments.

The metallurgy of yttrium and the rare earth metals.

"Materials Central, Contract No. AF33(616)-5905, Project No. 7351."

Influence of calcium on the microstructure and properties of an Al-7Si-0.3Mg-xFe alloy

The effect of Ca addition on the microstructure, physical characteristics (density/porosity), and mechanical properties (tensile and impact strength) has been investigated in an Al-7Si-0.3Mg-xFe (x = 0.2, 0.4, and 0.7) alloy. The size of Al-Fe intermetallic platelets (beta-Al5FeSi) increased with increasing Fe content. The addition of Ca modified the eutectic microstructure and also reduced the size of intermetallic Fe-platelets, causing improved elongation and impact strengths. A low level of Ca addition (39 ppm) reduced the porosity of the alloys. The tensile strength was decreased marginally with Ca addition. However, Ca addition improved the ductility of the alloy by 18.3, 16.7, and 44 pet and the impact strength by 44, 48, and 15.8 pct for Fe contents of 0.2, 0.4, and 0.7 pct, respectively.