Evaluation of interface characterization and adhesion of glass ceramics to commercially pure titanium and gold alloy after thermal- and mechanical-loading

Objectives. This study evaluated the effect of thermal- and mechanical-cycling on the shear bond strength of three low-fusing glassy matrix dental ceramics to commercial pure titanium (cpTi) when compared to conventional feldspathic ceramic fused to gold alloy.Methods. Metallic frameworks (diameter: 5 min, thickness: 4 mm) (N = 96, n = 12 per group) were cast in cpTi and gold alloy, airborne particle abraded with 150 mu m aluminum oxide. Low-fusing glassy matrix ceramics and a conventional feldspathic ceramic were fired onto the alloys (thickness: 4mm). Four experimental groups were formed; Gr1 (control group): Vita Omega 900-Au-Pd alloy; Gr2: Ticeram-cpTi; Gr3: Super Porcelain Ti-22-cpTi and G4: Vita Titankeramik-cpTi. While half of the specimens from each ceramic-metal combination were randomly tested without aging (water storage at 37 C for 24h only), the other half were first thermocycled (6000 cycles, between 5 and 55 C, dwell time: 13 s) and then mechanically loaded (20,000 cycles under SON load, immersion in distilled water at 37 C). The ceramic-alloy interfaces were loaded under shear in a universal test machine (cross-head speed: 0.5 mm/min) until failure occur-red. Failure types were noted and the interfaces of the representative fractured specimens from each group were examined with stereo microscope and scanning electron microscope (SEM). in an additional study (N = 16, n = 2 per group), energy dispersive X-ray spectroscopy (EDS) analysis was performed from ceramic-alloy interfaces. Data were analyzed using ANOVA and Tukey's test.Results. Both ceramic-metal combinations (p < 0.001) and aging conditions (p < 0,001) significantly affected the mean bond strength values. Thermal- and mechanical-cycling decreased the bond strength (MPa) results significantly for Gr3 (33.4 +/- 4.2) and Gr4 (32.1 +/- 4.8) when compared to the non-aged groups (42.9 +/- 8.9, 42.4 +/- 5.2, respectively). Gr1 was not affected significantly from aging conditions (61.3 +/- 8.4 for control, 60.7 +/- 13.7 after aging) (p > 0.05). Stereomicroscope images showed exclusively adhesive failure types at the opaque ceramic-cpTi interfacial zone with no presence of ceramic on the substrate surface but with a visible dark titanium oxide layer in Groups 2-4 except Gr1 where remnants of bonder ceramic was visible. EDS analysis from the interfacial zone for cpTi-ceramic groups showed predominantly 34.5-85.1% O(2) followed by 1.1-36.7% Aland 0-36.3% Si except for Super Porcelain Ti-22 where a small quantity of Ba (1.4-8.3%), S (0.7%) and Sn (35.3%) was found. In the Au-Pd alloy-ceramic interface, 56.4-69.9% O(2) followed by 15.6-26.2% Si, 3.9-10.9% K, 2.8-6% Na, 4.4-9.6% Al and 0-0.04% Mg was observed.Significance. After thermal-cycling for 6000 times and mechanical-cycling for 20,000 times, Triceram-cpTi combination presented the least decrease among other ceramic-alloy combinations when compared to the mean bond strength results with Au-Pd alloy-Vita Omega 900 combination. (c) 2008 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Mechanical and thermal cycling effects on the flexural strength of glass ceramics fused to titanium

This study evaluated the effects of mechanical and thermal cycling on the flexural strength (ISO 9693) of three brands of ceramics fused to commercially pure titanium (cpTi). Metallic frameworks of 25 x 3 x 0.5 mm dimensions (N = 84) were cast in cpTi, followed by 150-mu m aluminum oxide airborne particle abrasion at a designated area of the frameworks (8 x 3 mm). Bonder and opaque ceramic were applied on the frameworks, and then the corresponding ceramic (Triceram, Super Porcelain Ti-22, Vita Titankeramik) was fired onto them (thickness: 1 mm). Half of the specimens from each ceramic-metal combination were randomly tested without aging (only water storage at 37 degrees C for 24 hours), while the other half were mechanically loaded (20,000 cycles under 10 N load, immersion in distilled water at 37 degrees C) and thermocycled (3,000 cycles, between 5-55 degrees C, dwell time of 13 seconds). After the flexural strength test, failure types were noted. Mechanical and thermal cycling decreased the mean flexural strength values significantly (p<0.05) for all the three ceramic-cpTi combinations tested when compared to the control group. In all the three groups, failure type was exclusively adhesive at the opaque ceramic-cpTi interfacial zone with no presence of ceramic on the substrate surface except for a visible oxide layer.

Pump excited state absorption in holmium-doped fluoride glass

The primary excited state absorption processes relating to the (5)I(6) -> (5)I(7) 3 mu m laser transition in singly Ho(3+)-doped fluoride glass have been investigated in detail using time-resolved fluorescence spectroscopy. Selective laser excitation of the (5)I(6) and (5)I(7) energy levels established the occurrence of two excited state absorption transitions from these energy levels that compete with previously described energy transfer upconversion processes. The (5)I(7) -> (5)I(4) excited state absorption transition has peak cross sections at 1216 nm (sigma(esa)=2.8x10(-21) cm(2)), 1174 nm (sigma(esa)=1x10(-21) cm(2)), and 1134 nm (sigma(esa)=7.4x10(-22) cm(2)) which have a strong overlap with the (5)I(8) -> (5)I(6) ground state absorption. on the other hand, it was established that the excited state absorption transition (5)I(6) -> (5)S(2) had a weak overlap with ground state absorption. Using numerical solution of the rate equations, we show that Ho(3+)-doped fluoride fiber lasers employing pumping at 1100 nm rely on excited state absorption from the lowest excited state of Ho(3+) to maintain a population inversion and that energy transfer upconversion processes compete detrimentally with the excited state absorption processes in concentrated Ho(3+)-doped fluoride glass. (c) 2008 American Institute of Physics.

Color tunability of intense upconversion emission from Er3+-Yb3+ co-doped SiO2-Ta2O5 glass ceramic planar waveguides

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

Effects of maturation and scarification on seed germination of Syagrus schizophylla (Mart.) glass. (Arecaceae)

Syagrus schizophylla (Mart.) Glass. belongs to the Arecaccae family. This palm is native of Brazil and presents great potential for use in gardens and cultivation in pot. Palms species, with relatively few exceptions, can only be propagated from seeds; even so, there are no reports in the literature about the germination of this palm seeds. The seed maturity is a factor that interferes in the success of the germination process. For some species, studies showed that palm seeds germinated better when the fruits were completely ripe (showing full color) and for other, when they were with green coloration. Several species of the Arecaccae family presents physical dormancy of seeds in varied degrees, demanding treatments for improve germination. The objective of this work was to study the effects of maturation and of the scarification on seed germination of S. schizophylla. The experimental design used was a factorial 3 x 2 (3 maturation stadiums: green, half-ripe - yellow and completely ripe - red; and mechanical scarification: with and without), entirely casualized, with four replications of 15 seeds per plot. The seeds (with 32,43% of humidity) were placed in plastic boxes with sand (60% of humidity, placing water according to weight in each three days), under controlled conditions of alternated temperature of 25-35 degrees C, photoperiod of 12 hours. The percentage of germination and the speed germination index (SGI) were evaluated until 79 days. It was observed that, so much for germination percentage as for SGI, there was not significant difference for the interaction among the two factors, maturation stadium and scarification, however, there were significant differences among the maturation stadiums and between seeds scarified or not. The seeds from green fruits presented lower germination percentage and slower germination when compared with seeds from yellow or red fruits; the seeds from yellow or red fruits didn't differ statistically to each other. To seeds scarificated, independently of the maturation stadium, presented germination percentage significantly larger and the germination was significantly faster when compared with the seeds without scarification.

Development of an experimental glass ionomer cement containing niobium and fluoride

Glass ionomer cements (GICs) are currently used for various dental applications such as luting cements or as restorative materials. The calcium fluoro-alumino-silicate system is the basis for degradable glasses used to obtain the GICs. The purpose of the present paper is to add niobium to conventional glass system because according to previous papers niobium addition improves the chemical resistance and the mechanical properties of glasses. Therefore, the GICs prepared from these glasses would result in cements with higher chemical and mechanical resistance. The niobium fluoride powders were prepared using the sol-gel process and were characterized by X-ray diffraction, differential thermal analysis (DTA) and Al-27 and Si-29 MAS NMR. The results obtained by XRD showed that the powders prepared by this method are glass-ceramic. In the DTA curve was detected the presence of T-g and T-c temperatures. The analysis of MAS NMR spectra indicated that the framework of the powders is formed by SiO4 and AlO4 linked tetrahedra which are essential structures to yield the cements. Thus, we concluded that niobium fluoride silicate powders can be used in the preparation of GICs. (c) 2005 Elsevier B.V. All rights reserved.

Bond strength of resin modified glass ionomer cement to primary dentin after cutting with different bur types and dentin conditioning

The aim of this in vitro study was to evaluate the effect of different bur types and acid etching protocols on the shear bond strength (SBS) of a resin modified glass ionomer cement (RM-GIC) to primary dentin. Forty-eight clinically sound human primary molars were selected and randomly assigned to four groups (n=12). In G1, the lingual surface of the teeth was cut with a carbide bur until a 2.0-mm-diameter dentin area was exposed, followed by the application of RM-GIC (Vitremer - 3M/ESPE) prepared according to the manufacturer's instructions. The specimens of G2, received the same treatment of G1, however the dentin was conditioned with phosphoric acid. In groups G3 and G4 the same procedures of G1 and G2 were conducted respectively, nevertheless dentin cutting was made with a diamond bur. The specimens were stored in distilled water at 37 degrees C for 24h, and then tested in a universal testing machine. SBS. data were submitted to 2-way ANOVA (= 5%) and indicated that SBS values of RM-GIC bonded to primary dentin cut with different burs were not statistically different, but the specimens that were conditioned with phosphoric acid presented SBS values significantly higher that those without conditioning. To observe micromorphologic characteristics of the effects of dentin surface cut by diamond or carbide rotary instruments and conditioners treatment, some specimens were examined by scanning electron microscopy. Smear layer was present in all specimens regardless of the type of rotary instrument used for dentin cutting, and specimens etched with phosphoric acid presented more effective removal of smear layer. It was concluded that SBS of a RM-GIC to primary dentin was affected by the acid conditioning but the bur type had no influence.

Nonlinear refractive index measurements in antimony-sulfide glass films using a single beam nonlinear image technique

The nonlinear refractive index, n(2), of films based on the new glass system Sb(2)O(3)-Sb(2)S(3) was measured at 1064 nm with laser pulses of 15 ps, using a single-beam nonlinear image technique in presence of a phase object. The films were prepared from bulk glasses by RF-sputtering. A large value of n(2) = 3 x 10-(15) m(2)/W, which is three orders of magnitude larger than for CS(2), was determined. The result shows the strong potential of antimony-sulfide glass films for integrated nonlinear optics. (c) 2005 Elsevier B.V. All rights reserved.

Optical properties and frequency upconversion fluorescence in a Tm3+-doped alkali niobium tellurite glass

Optical spectroscopic properties of Tm3+-doped 60TeO(2)-10GeO(2)-10K(2)O-10Li(2)O-10Nb(2)O(5) glass are reported. The absorption spectra were obtained and radiative parameters were determined using the Judd-Ofelt theory. Characteristics of excited states were studied in two sets of experiments. Excitation at 360 nm originates a relatively narrow band emission at 450 nm attributed to transition D-1(2)-->F-3(4) of the Tm3+ ion with photon energy larger than the band-gap energy of the glass matrix. Excitation at 655 nm originates a frequency upconverted emission at 450 nm (D-1(2)-->F-3(4)) and emission at 790 nm (H-3(4)-->H-3(6)). The radiative lifetimes of levels D-1(2) and H-3(4) were measured and the differences between their experimental values and the theoretical predictions are understood as due to the contribution of energy transfer among Tm3+ ions. (C) 2003 American Institute of Physics.

Energy transfer between Tm3+ and Er3+ ions in a TeO2-based glass pumped at diode laser wavelength

In this paper we investigate the energy transfer processes in TM3+/Er3+ doped telluride glass pumped at the commercial diode laser pump wavelength similar to 800 nm. Tailoring the rare-earths content in the glass matrix, seven main energy transfer channels within the doping range considered were identified, A 6-fold enhancement of the Er3+ visible frequency upconversion fluorescence at similar to 660 nm is observed due to the inclusion of Tm3+ ions. This is evidence of the relevant contribution of the route Er-1(I-4(11/2)) + Er-2(I-4(13/2)) -> Er-1(I-4(15/2)) + Er-2(F-4(9/2)) to the process. Energy migration among pumped I-4(9/2) level reducing the efficiency of the upconversion emission rate (H-3(11/2), S-4(3/2), and F-4(9/2)) is observed for Er3+ above 1.5 wt%. The rate equations regarding the observed energy transfer routes are determined and a qualitative analysis of the observed processes is reported. (c) 2006 Elsevier B.V. All rights reserved.

Effectiveness of surface protection for resin-modified glass-ionomer materials

Objective: the purpose of this study was to evaluate the effectiveness of various surface treatments for resin-modified glass-ionomer restorative materials by determining dye uptake spectrophotometrically. Method and materials: Two hundred twenty-four specimens, 4.1 mm in diameter and 2.0 mm thick, were made of 3 materials: Vitremer, Fuji II LC, and Photac-Fil Aplicap. Specimens were divided into 15 groups. The positive and negative control specimens remained unprotected, while the experimental specimens were protected with Heliobond light-activated bonding resin, Colorama nail varnish, or surface coatings indicated by the manufacturers of the glass-ionomer materials. Finishing Gloss for Vitremer, Fuji Varnish for Fuji II LC, and Ketac Glaze for Photac-Fil. The disks were immersed in 0.05% methylene blue for 24 hours except for the negative control group, which was immersed in deionized water. After 24 hours, the disks were removed, washed, and individually placed in 1 mL of 65% nitric acid for 24 hours. The solutions were centrifuged and the spectrophotometric absorbance was determined at 606 nm. The dye uptake was expressed in micrograms of dye per milliliter, and the results were analyzed with the Kruskal-Wallis test. Results: There were no differences in dye uptake among the 3 resin-modified glass-ionomer restorative materials, however, all of them required surface protection. Conclusion: the best surface protection for the 3 evaluated materials was obtained with Heliobond light-activated bonding resin.

Upconversion luminescence in transparent glass ceramics containing beta-PbF2 nanocrystals doped with erbium

Frequency upconversion luminescence in erbium-doped PbGeO3-PbF2-CdF2-based transparent glass ceramics (TGC) under 980 nm infrared excitation is investigated. Upconversion emission signals around 410, 525, 550, 660, and 850 nm were generated and identified as due to the H-2(9/2) H-2(11/2), S-4(3/2), and F-4(9/2) transitions to the I-4(15/2) ground-state, and S-4(3/2)-I-4(13/2), respectively. The erbium ions excited-state emitting levels were populated via a combination of stepwise ground-state absorption (GSA), excited-state absorption (ESA), and cross-relaxation processes. The results also disclosed that both blue (410 nm) and red (660 nm) upconversion emission signals in the transparent glass ceramic sample presented twice as much intensity as compared to its vitreous counterpart. (C) 2003 Elsevier B.V. All rights reserved.

Influence of ceramic surface conditioning and resin cements on microtensile bond strength to a glass ceramic

Statement of problem. It is not clear how different glass ceramic surface pretreatments influence the bonding capacity of various luting agents to these surfaces.Purpose. The purpose of this study was to evaluate the microtensile bond strength (mu TBS) of 3 resin cements to a lithia disilicate-based ceramic submitted to 2 surface conditioning treatments.Material and methods. Eighteen 5 X 6 X 8-mm ceramic (IPS Empress 2) blocks were fabricated according to manufacturer's instructions and duplicated in composite resin (Tetric Ceram). Ceramic blocks were polished and divided into 2 groups (n=9/treatment): no conditioning (no-conditioning/control), or 5% hydrofluoric acid etching for 20 seconds and silanization for 1 minute (HF + SIL). Ceramic blocks were cemented to the composite resin blocks with I self-adhesive universal resin cement (RelyX Unicem) or 1 of 2 resin-based luting agents (Multilink or Panavia F), according to the manufacturer's instructions. The composite resin-ceramic blocks were stored in humidity at 37 degrees C for 7 days and serially sectioned to produce 25 beam specimens per group with a 1.0-mm(2) cross-sectional area. Specimens were thermal cycled (5000 cycles, 5 degrees C-55 degrees C) and tested in tension at 1 mm/min. Microtensile bond strength data (MPa) were analyzed by 2-way analysis of variance and Tukey multiple comparisons tests (alpha=.05). Fractured specimens were examined with a stereomicroscope (X40) and classified as adhesive, mixed, or cohesive.Results. The surface conditioning factor was significant (HF+SIL > no-conditioning) (P<.0001). Considering the unconditioned groups, the mu TBS of RelyX Unicem was significantly higher (9.6 +/- 1.9) than that of Multilink (6.2 +/- 1.2) and Panavia F (7.4 +/- 1.9). Previous etching and silanization yielded statistically higher mu TBS values for RelyX Unicem (18.8 +/- 3.5) and Multilink (17.4 +/- 3.0) when compared to Panavia F (15.7 +/- 3.8). Spontaneous debonding after thermal cycling was detected when luting agents were applied to untreated ceramic surfaces.Conclusion. Etching and silanization treatments appear to be crucial for resin bonding to a lithia disilicate-based ceramic, regardless of the resin cement used.

Energy upconversion luminescence in neodymium-doped tellurite glass

Infrared-to-visible upconversion luminescence emission in Nd3+-doped 60TeO(2)-10GeO(2)-10K(2)O-10Li(2)O-10Nb(2)O(5) tellurite glasses under cw excitation around 800 nm is investigated. Blue (430, and 475 nm), green (5 0 nm) and yellow-orange (590 nm) energy upconversion emission owing to the P-2(1/2) --> I-4(j) (j=9/2, 11/2, 13/2 and 15/2) transitions of the Nd3+ ions, respectively, was recorded. The dependence of the upconversion intensity upon the excitation wavelength and pump power is also studied. The upconversion excitation mechanism responsible for the observed emission signals is attributed to stepwise multiphoton absorption. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Evaluation of glass ionomer cements properties obtained from niobium silicate glasses prepared by chemical process

Glass ionomer cements (GICs) are glass and polymer composite materials. These materials currently find use in the dental field. The purpose of this work is to obtain systems based on composition 4.5SiO(2)-3Al(2)O(3)-XNb2O5-2CaO to be used in Dentistry. The systems were prepared by chemical route at 700 degrees C. The results obtained by XRD and DTA showed that all systems prepared are glasses. The structures of the obtained glasses were compared to commercial material using Al-27 and Si-29 MAS NMR. The analysis of MAS NMR spectra indicated that the systems developed and commercial material are formed by SiO4 and AlO4 linked tetrahedra. The properties of glass ionomer cements based on the glasses prepared with several niobium contents were studied. Setting and working times of the cement pastes, microhardness and diametral tensile strength were evaluated for the experimental GICs and commercial luting cements. It was concluded that setting time of the cement pastes increased with increasing niobium content of the glasses (X). The properties to the GICs such as setting time and microhardness were influenced by niobium content. (c) 2005 Elsevier B.V. All rights reserved.