Preparation and characterization of glass-ceramic materials in the BaO-Li2O-ZrO2-SiO2 system and their dependence on treatment temperatures

The preparation and characterization of transparent glass-ceramics in the composition of 30Li2O:5ZrO2:xBaO:(100-x) SiO2 with x = 0, 5, 10, 15, and 20 mol% are described. Glasses were melted in a platinum crucible at 1100°C for 2 h and then heat-treated at 900°C for 3 h. The characterizations were performed by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman and infrared spectroscopy, and scanning electron microscopy (SEM). The experimental results indicate that there was a structural change in the glass-ceramics as the BaO concentration in the mixture increased. In the XRD patterns of samples without heat treatment, only the halo was observed. After heat treatment, the appearance of the materials was verified by X-ray diffraction peaks. The reorganization of the amorphous solid was confirmed by Raman and IR spectroscopy along with XPS and SEM, with a more homogeneous phase formation being observed.

Reaction of dogs' teeth to root canal filling with mineral trioxide aggregate or a glass ionomer sealer

This study was conducted to observe the reaction of apical tissues of dogs' teeth after root canal filling with gutta-percha and mineral trioxide aggregate (MTA) or a glass ionomer (Ketac-Endo) as a sealer. The root canals were instrumented and filled by the lateral condensation technique with the sealers studied. Animals were killed 6 months later, and the specimens were removed and prepared for histological analysis. Results showed no inflammatory reaction of apical tissue and total closure of the apical foramen of all the teeth sealed with MTA. The teeth sealed with Ketac-Endo showed two cases of partial closure and different degrees of chronic inflammatory reaction. In conclusion, MTA exhibited better biological properties than Ketac-Endo. Copyright © 1999 by The American Association of Endodontists.

Control of nonlinear absorption and amplification of light in Er3+-doped fluoroindate glass

Nonlinear absorption and amplification of a probe laser beam can be controlled by adjustment of the intensity-modulation frequency and the wavelength of a pump laser beam. A demonstration of this effect in Er3+-doped fluoroindate glass is presented. The results show maximum amplification of the probe beam (∼12%) when a pump laser emitting 16 mW of power is modulated at ∼30 Hz. In the limit of low modulation frequencies, or cw pumping, induced absorption of the probe beam is the dominant nonlinear process. © 1999 Optical Society of America.

Densification and residual stresses induced in glass surfaces by Vickers indentations

Images and profiles of Vickers impressions produced on as-received float-glass were obtained using atomic force microscopy (AFM). The images show that the impression edges undergo elastic recovery parallel to surface. The profiles made it possible to measure vertical elastic recovery, ev(r). For a 40 g nominal load, maximum penetration depth of indenter was (2.20 ± 0.03) μm, and recovery at the impression center was ev(0) = (0.98 ± 0.03) μm. Vertical elastic recovery was non-uniform along profiles. Permanent impressions produced resulted from glass mass displacement downward, producing an increase in glass density in impression vicinity, which is discussed in terms of changes in O-Si-O and Si-O-Si bond angles and Si-O bond length. Near impression edges, pileup was observed for which a simplified model is proposed taking into account the compaction and stresses near the impressions. © 2000 Elsevier Science B.V. All rights reserved.

Crystallization mechanism and properties of a blast furnace slag glass

The complex crystallization process of a Brazilian blast-furnace slag glass was investigated using differential scanning calorimetry (DSC), X-ray diffraction, optical microscopy, transmission electron microscopy (TEM), selected area diffraction (SAD), energy dispersive spectroscopy (EDS) and micro-Raman spectroscopy. Three crystalline phases (merwinite, melilite and larnite) were identified after heat treatment between Tg (742°C) and the DSC crystallization peak (T = 1000°C). Merwinite was identified as a metastable phase. A small amount (0.004 wt%) of metallic platinum was found in the glass composition. Particles of Pt3Fe, detected by EDS and SAD-TEM, were the starting points of crystallization acting, therefore, as heterogeneous nucleating sites. Only melilite and larnite precipitated in a glass sample heat-treated at 1000°C for 1 h. The flexural strength of this crystallized sample was less than that of the glass, probably due the allotropic phase transformation of larnite. © 2000 Published by Elsevier Science B.V. All rights reserved.

Thermally enhanced frequency upconversion in Nd3+-doped fluoroindate glass

Multiphonon assisted frequency upconversion was observed in a Nd3+-doped fluoroindate glass pumped at 866 nm. A near-infrared upconverted emission at 750 nm with a peculiar linear dependence with the laser intensity was observed and explained. The intensity of the upconverted emission experienced a 40-fold enhancement when the sample's temperature was varied from 298 to 498 K. A rate equation model that includes light pumping and multiphonon absorption via thermally coupled electronic excited states of Nd3+ was used, describing quite well the experimental results. © 2001 American Institute of Physics.

Energy transfer assisted frequency upconversion in Ho 3+ doped fluoroindate glass

Experimental results are reported which show a strong evidence of energy transfer between Ho 3+ ions in a fluoroindate glass excited by a pulsed laser operating at 640 nm. We identified the origin of the blue and green upconverted fluorescence observed as being due to a Ho 3+-Ho 3+ pair interaction process. The dynamics of the fluorescence revealed the pathways involved in the energy transfer assisted upconversion process. © 2002 American Institute of Physics.

Blue upconversion enhancement by a factor of 200 in Tm 3+-doped tellurite glass by codoping with Nd 3+ ions

We investigated near-infrared-to-blue upconversion from thulium (Tm 3+) doped in tellurite glasses upon continuous wave excitation near 800 nm. We observed an enhancement of over two orders of magnitude of the upconverted emission at ∼480nm when neodymium (Nd 3+) ions were codoped with Tm 3+ ions. For comparison, using a Tm 3+:Nd 3+ codoped fluorozirconate glass as a reference material we observed a 40-fold enhancement of the blue emission. Analysis of the blue emission for samples with different doping levels of Nd 3+ ions showed that energy transfer between Nd 3+ and Tm 3+ is the mechanism responsible for the enhancement in upconversion. © 2002 American Institute of Physics. © 2002 American Institute of Physics.

Enhanced frequency upconversion in Er3+ doped fluoroindate glass due to energy transfer from Tm3+

Energy transfer processes between Er3+ and Tm3+ were investigated examining the frequency upconversion emissions in a fluoroindate glass pumped at 790 nm. A 60-fold enhancement in the emission at ≈670 nm originating from Er3+ was observed when Tm3+ at concentration of 2% was introduced in a sample containing 2% of Er3+. The results are explained considering the influence of cross-relaxation processes between the active ions. © 2002 Elsevier Science B.V. All rights reserved.

Phonon-assisted cooperative energy transfer and frequency upconversion in a Yb3+/Tb3+ codoped fluoroindate glass

Phonon-assisted cooperative energy transfer and frequency upconversion (UC) in Yb3+/Tb3+ codoped fluoroindate glass were investigated. Anti-Stokes quasiresonant excitation of Yb3+ ions was used to study the influence of multiphonon transitions in the UC process. A rate equation model was used to describe the temperature dependence of the UC emission intensities and the theoretical results are in good agreement with the experimental data.

Spectroscopic properties of Tm3+ doped fluoroindate glass

Optical absorption and fluorescence were investigated in Tm3+ doped fluoroindate glass. The spectroscopic parameters for transitions in the 4f11 configuration were determined. The fluorescence study revealed the origin of the frequency upconversion process as well as allowed to quantify the interaction between Tm3+ ions.

Transparent Er3+-activated lead fluorogermanate glass ceramics

Transparent glass ceramics containing β-PbF2:Er 3+ nanocrystals were obtained through appropriate thermal treatments of a glass of molar composition 60PbGeO3-10PbF2-30CdF 2 doped with 0.5 mol% Er3+. Their optical properties, as well as upconversion processes among erbium ions in the glass and glass ceramic matrix were studied. From absorption spectra, Judd-Ofelt parameters and radiative transition rates for several excited levels were calculated. Emission spectra in the visible and NIR regions were collected, and stimulated emission cross sections were obtained by McCumber theory for the 4F 13/2→4I15/2 transition at 1.5 μm. Red and green upconversion emissions were measured in glass and glass ceramics upon excitation at 980 nm; lifetimes were measured in order to assess the upconversion mechanisms.

Infrared-to-visible frequency upconversion in transparent glass ceramics containing trivalent-rare-earth-doped nanocrystals

In this work we report on visible upconversion emission in Er 3+-, and Ho3+-doped PbGeO3-PbF 2-CdF2-based transparent glass ceramics under 980 nm infrared excitation. In erbium-doped vitroceramic samples, blue(410 ran), green(530, and 550 nm) and red(660 nm) emission signals were generated, which were identified as due to the 2H9/2, 2H 11/2, 4S3/2, and 4F9/2 transitions to the 4I15/2 ground-state, respectively. Intense red(650 nm) upconversion emission corresponding to the 5F5 - 5I8 transition and very small blue(490 nm) and green(540 nm) signals assigned to the 5F 2,3 - 5I8 and 4S2, 5F4 - 5I8 transitions, respectively, were observed in the holmium-doped samples. The 540 nm is the dominant upconversion signal in Ho3+-doped vitroceramics under 850 nm excitation. The dependence of the upconversion processes upon pump power and doping concentration are also investigated, and the main routes for the upconversion excitation processes are also identified. The comparison of the upconversion process in transparent glass ceramics and the precursor glass was also examined and the results revealed that the former present higher upconversion efficiencies.

Red, green, and blue upconversion luminescence in ytterbium-sensitized praseodymium-doped lead-cadmium-germanate glass

Blue, green, red, and near-infrared upconversion luminescence in the wavelength region of 480 - 740 nm in Pr3+/Yb3+-codoped lead-cadmium-germanate glass under 980 nm diode laser excitation, is presented. Upconversion emission peaks around 485, 530, 610, 645, and 725 nm which were ascribed to the 3P0 - 3HJ (J=4, 5, and 6), and 3P0 - 3FJ (J=2, and 3,4), transitions, respectively, were observed. The population of the praseodymium upper 3P0 emitting level was accomplished through a combination of ground-state absorption of Yb3+ ions at the 2F7/2, energy-transfer Yb3+(2F 5/2) Pr3+(3H4), and excited-state absorption of Pr3+ ions provoking the 1G4 - 3P0 transition. The dependence of the upconversion luminescence upon the Yb3+-concentration and diode laser power, is also examined, in order to subsidize the proposed upconversion excitation mechanism.

Dynamics of energy transfer and frequency upconversion in Tm3+ doped fluoroindate glass

The spectroscopic properties of Tm3+-doped fluoroindate glasses (FIG) were described by single wavelength pumping in the red region. The Judd-Ofelt (J-O) theory was used to obtain the quantum efficiency of the 4f-4f transitions and other spectroscopic parameters. The dynamics of the fluorescence was investigated and energy transfer (ET) processes among Tm3+ ions were studied. The results indicate that a two-step one-photon absorption process is responsible for the ultraviolet upconversion (UC) emissions, and dipole-dipole interaction provides the main contribution for ET rate is equal to the decay rate of noninteracting among active ions.