Effect of the sintering conditions on the electrical properties of Nd(3+) modified PLZT ceramics

The effect of the sintering method on the microstructural and electrical properties of (Pb(0.89)Nd(0.02)La(0.09))(Zr(0.65)Ti(0.35))O(3) (PNLZT) ceramics was studied by impedance spectroscopy. Structural and microstructural analyses were performed using x-ray and scanning electron microscopy techniques. Two different sintering routes were employed: the conventional and the hot-pressing sintering methods. The impedance analysis provided a convincing evidence for the existence of both grain (g) and grain boundary (gb) contributions to the conduction process. An equivalent circuit for the impedance behaviour has been proposed and discussed. The variation in the sintering method produces significant changes in the grain and grain boundary conductivities. For the grain effect, the main conduction mechanism has been associated with oxygen vacancy migration. Otherwise, for grain boundary conductivity the impedance behaviour has been discussed in terms of the brick-layer and the constriction resistance models (BLM and CRM, respectively).

Effect of heat treatment on the generation of structural defects in LaTaO4 ceramics and their correlation with photoluminescent properties

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

Structural Investigations of Glass Ceramics in the Ga2S3-GeS2-CsCl System

Transparent glass ceramics have been prepared in the Ga2S3-GeS2-CsCI pseudoternary system appropriate heat treatment time and temperature. In situ X-ray diffraction at the heat treatment temperature and Cs-133 and Ga-71 solid-state nuclear magnetic resonance have been performed in function of annealing time to understand the crystallization process. Both techniques have evidenced the nucleating agent role played by gallium with the formation of Ga2S3 nanocrystals. on the other hand, cesium is incorporated very much later into the crystallites during the ceramization. Moreover, the addition of CsCl, which is readily integrated into the glassy network, permits us to shift the optical band gap toward shorter wavelength. Thus, new glass ceramics transmitting in the whole visible range up to 11.5 mu m have been Successfully synthesized from the (Ga2S3)(35)-(GeS2)(25)-CsCl40 base glass composition.

Synthesis and Structural Studies of Er3+ Containing Lead Cadmium Fluoroborate Glasses and Glass-Ceramics

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

Effects of powder preparation and sintering procedure on microstructure and dielectric properties of PLZT ceramics

PLZT ceramics belong to one of the very important groups of functional materials that make a basis for the production of a large range of electronic devices. The microstructure and properties of ceramics depend on the powder preparation and thermal processing conditions. Various techniques have been used to obtain chemically homogeneous and fine starting powders. PLZT powders have been prepared by two different production routes: by a modified Pechini method, using a polymeric precursor method (PMM) and by a partial oxalate method. A two-step sintering process, including a hot pressing, was carried out at 1100 and 1200degreesC Distinct phases obtained during the sintering process have been investigated by SEM and EDS techniques and dielectric properties such as permittivity and dielectric loss were measured in a frequency range from 1 to 20 kHz.. A significant difference in microstructure and dielectric properties, depending on powder origin and sintering procedure, has been noticed.

Lead-cadmium oxyfluoride glasses and glass-ceramics

Glasses and glass-ceramics have been obtained in oxyfluoride systems involving lead and cadmium fluorides and one of the well-known glass former oxides SiO2, B2O3 and TeO2. Vitreous domains were established and a wide range of compositions including high heavy metal contents lead to stable glasses. Amorphous structures have been studied by short-range order spectroscopy techniques (Raman scattering and x-ray absorption) and molecular basic structures have been identified. Besides the usual oxides, the role of glass former could also be proposed for cadmium ions. Special attention has been paid for crystallization process. Cubic lead fluoride, cubic lead tellurite, tetragonal tellurium oxide and a solid solution of the type Pb1-xCdxF2 are obtained as crystallization products depending on the composition and temperature of heat treatments. Pb1-xCdxF2 solid solutions are well known superionic materials and obtaining this solid solution as a crystal phase could be very interesting for applications concerning ionic electrical conduction properties. The addition of rare earth ions led to the control of the crystallization process. In the presence of the nucleating ion only the cubic form beta-PbF2 was identified. Rare earth ions are present in the crystal phase and crystal-like spectroscopic properties were observed suggesting interesting applications for these perfectly transparent glass ceramics in photonics.

Piezoelectric effect in composite polyurethane-ferroelectric ceramics

Flexible and free-standing films of piezoelectric composites made up of lead zirconate titanate (PZT) ceramic powder dispersed in a castor oil-based polyurethane (PU) matrix were obtained by spin coating and characterized as materials for sensor applications. The piezoelectric coefficients d 31 and d 33 were measured with the usual technique. The piezoelectric charge constant d 33 yields values up to ≤24 pC/N, even at lower PZT content (33 vol%). Some desirable properties like piezoelectricity, flexibility and good mechanical resistance show this new material to be a good alternative for use as sensors and actuators.

Bonding all-ceramic restorations with two resins cement techniques: A clinical report of three-year follow-up

Ceramics have been widely used for esthetic and functional improvements. The resin cement is the material of choice for bonding ceramics to dental substrate and it can also dictate the final esthetic appearance and strength of the restoration. The correct use of the wide spectrum of resin luting agents available depends on the dental tooth substrate. This article presents three-year clinical results of a 41 years old female patient B.H.C complaining about her unattractive smile. Two all-ceramic crowns and two laminates veneers were placed in the maxillary incisors and cemented with a self-adhesive resin luting cement and conventional resin luting cement, respectively. After a three-year follow-up, the restorations and cement/teeth interface were clinically perfect with no chipping, fractures or discoloration. Proper use of different resin luting cements shows clinical appropriate behavior after a three-year follow-up. Self-adhesive resin luting cement may be used for cementing all-ceramic crowns with high predictability of success, mainly if there is a large dentin surface available for bonding and no enamel at the finish line. Otherwise, conventional resin luting agent should be used for achieving an adequate bonding strength to enamel.

Infrared to visible up-conversion emission in Er3+/Yb 3+ codoped fluoro-phosphate glass-ceramics

Erbium Er3+ and ytterbium Yb3+ codoped fluoro-phosphate glasses belonging to the system NaPO3-YF 3-BaF2-CaF2 have been prepared by the classical melt-quenching technique. Glasses containing up to 10 wt% of erbium and ytterbium fluorides have been obtained and characterized using differential scanning calorimetry (DSC) and UV-visible and near-infrared spectroscopy. Transparent and homogeneous glass-ceramics have been then reproducibly synthetized by appropriate heat treatment above glass transition temperature of a selected parent glass. Structural investigations of the crystallization performed through X-ray diffractometry (XRD) and scanning electron microscopy (SEM) have evidenced the formation of fluorite-type cubic crystals based during the devitrification process. Finally, infrared to visible up-conversion emission upon excitation at 975 nm has been studied on the Er3+ and Yb 3+ codoped glass-ceramics as a function of thermal treatment time. A large enhancement of intensity of the up-conversion emissions-about 150 times- has been observed in the glass-ceramics if compared to the parent glass one, suggesting an incorporation of the rare-earth ions (REI) into the crystalline phase. © 2012 The American Ceramic Society.

White Light and Multicolor Emission Tuning in Triply Doped Yb3+/Tm3+/Er3+ Novel Fluoro-phosphate Transparent Glass-ceramics

New Yb3+, Er3+ and Tm3+ doped fluoro-phosphate glasses belonging to the system NaPO3–YF3–BaF2–CaF2 and containing up to 10 wt% of rare-earth ion fluorides were prepared and characterized by differential scanning calorimetry, absorption spectroscopy and up-conversion emission spectroscopy under excitation with a 975 nm laser diode. Transparent and homogeneous glass-ceramics have been reproducibly obtained with a view to manage the red, green and blue emission bands and generate white light. X-ray diffraction as well as electron microscopy techniques have confirmed the formation of fluorite-type cubic nanocrystals at the beginning of the crystallization process while complex nanocrystalline phases are formed after a longer heat-treatment. The prepared glass-ceramics exhibit high optical transparency even after 170 h of thermal treatment. An improvement of up-conversion emission intensity – from 10 to 160 times larger – was measured in the glass-ceramics when compared to the parent glass, suggesting an important incorporation of the rare-earth ions into the crystalline phase(s). The involved mechanisms and lifetime were described in detail as a function of heat-treatment time. Finally, a large range of designable color rendering (from orange to turquoise through white) can be observed in these materials by controlling the laser excitation power and the crystallization rate.

Raman and infrared investigations of glass and glass-ceramics with composition 2Na2O·1CaO·3SiO2

Precursor glass and glass-ceramics with molar composition 2Na2O·1CaO·3SiO2 are studied by infrared, conventional, and microprobe Raman techniques. The Gaussian deconvoluted Raman spectrum of the glass presents bands at 625 and 660 cm-1, attributed to bending vibrations of Si-O-Si bonds, and at 860, 920, 975, and 1030 cm-1, attributed to symmetric stretching vibrations of SiO4 tetrahedra with 4, 3, 2, and 1 nonbridging oxygens, respectively. The Raman microprobe spectrum of a highly crystallized sample presents two narrow and intense bands at about 590 and 980 cm-1, associated with vibrations of SiO4 tetrahedra with two nonbridging oxygens, in agreement with the predicted chain-like structure of crystalline metasilicates. Scanning electron microscopy shows that the crystals distributed in partially crystallized samples have a spherical shape, built up by radially oriented needle-like single crystals. The Raman microprobe spectra of these spherulites show that they still contain residual amorphous material. A comparison of Raman and infrared spectra of amorphous and highly crystallized samples is presented.

Determination of carrier mobility in MEH-PPV thin-films by stationary and transient current techniques

Charge transport and shelf-degradation of MEH-PPV thin-films were investigated through stationary (e.g. current versus voltage - JxV) and transient (e.g. Time-of-Flight - ToF, Dark-Injection Space-Charge-Limited Current - DI-SCLC, Charge Extraction by Linearly Increasing Voltage - CELN) current techniques. Charge carrier mobility in nanometric films was best characterized through JxV and DI-SCLC. It approaches 10(-6) cm(2)Ns under a SCLC regime with deep traps for light-emitting diode applications. ToF measurements performed on micrometric layers (i.e. - 3 mu m) confirmed studies in 100 nm-thick films as deposited in OLEDs. All results were comparable to a similar poly(para-phenylene vinylene) derivative, MDMO-PPV. Electrical properties extracted from thin-film transistors demonstrated mobility dependence on carrier concentration in the channel (similar to 10(-7)-10(-4) cm(2)/Vs). At low accumulated charge levels and reduced free carrier concentration, a perfect agreement to the previously cited techniques was observed. Degradation was verified through mobility reduction and changes in trap distribution of states. (C) 2011 Elsevier B.V. All rights reserved.

Performance of different polishing techniques for direct CAD/CAM ceramic restorations

This in vitro study evaluated the performance of three ceramic and two commonly used polishing methods on two CAD/CAM ceramics. Surface roughness and quality were compared. A glazed group (GLGR) of each ceramic material served as reference. One-hundred and twenty specimens of VITABLOCS Mark II (VITA) and 120 specimens of IPS Empress CAD (IPS) were roughened in a standardized manner. Twenty VITA and 20 IPS specimens were glazed (VITA Akzent Glaze/Empress Universal Glaze). Five polishing methods were investigated (n=20/group): 1) EVE Diacera W11DC-Set (EVE), 2) JOTA 9812-Set (JOTA), 3) OptraFine-System (OFI), 4) Sof-Lex 2382 discs (SOF) and 5) Brownie/Greenie/Occlubrush (BGO). Polishing quality was measured with a surface roughness meter (Ra and Rz values). The significance level was set at alpha=0.05. Kruskal Wallis tests and pairwise Wilcoxon rank sum tests with Bonferroni-Holm adjustment were used. Qualitative surface evaluation of representative specimens was done with SEM. On VITA ceramics, SOF produced lower Ra (p<0.00001) but higher Rz values than GLGR (p=0.003); EVE, JOTA, OFI and BGO yielded significantly higher Ra and Rz values than GLGR. On IPS ceramics, SOF and JOTA exhibited lower Ra values than GLGR (p<0.0001). Equivalent Ra but significantly higher Rz values occurred between GLGR and EVE, OFI or BGO. VITA and IPS exhibited the smoothest surfaces when polished with SOF. Nevertheless, ceramic polishing systems are still of interest to clinicians using CAD/CAM, as these methods are universally applicable and showed an increased durability compared to the investigated silicon polishers.

Etching and microstructure of engineering ceramics

Engineering ceramics are often difficult to prepare metallographically because of their hardness, wear resistance and chemical inertness. Two silicon carbides, a silicon nitride and a sialon, are prepared and etched using several different techniques. The most efficient methods are identified. © 1995.