Light curing through glass ceramics: effect of curing mode on micromechanical properties of dual-curing resin cements

OBJECTIVES The aim of this study was to investigate micromechanical properties of five dual-curing resin cements after different curing modes including light curing through glass ceramic materials. MATERIALS AND METHODS Vickers hardness (VH) and indentation modulus (Y HU) of Panavia F2.0, RelyX Unicem 2 Automix, SpeedCEM, BisCem, and BeautiCem SA were measured after 1 week of storage (37 °C, 100 % humidity). The resin cements were tested following self-curing or light curing with the second-generation light-emitting diode (LED) curing unit Elipar FreeLight 2 in Standard Mode (1,545 mW/cm(2)) or with the third-generation LED curing unit VALO in High Power Mode (1,869 mW/cm(2)) or in XtraPower Mode (3,505 mW/cm(2)). Light curing was performed directly or through glass ceramic discs of 1.5 or 3 mm thickness of IPS Empress CAD or IPS e.max CAD. VH and Y HU were analysed with Kruskal-Wallis tests followed by pairwise Wilcoxon rank sum tests (α = 0.05). RESULTS RelyX Unicem 2 Automix resulted in the highest VH and Y HU followed by BeautiCem SA, BisCem, SpeedCEM, and finally Panavia F2.0. Self-curing of RelyX Unicem 2 Automix and SpeedCEM lowered VH and Y HU compared to light curing whereas self-curing of Panavia F2.0, BisCem, and BeautiCem SA led to similar or significantly higher VH and Y HU compared to light curing. Generally, direct light curing resulted in similar or lower VH and Y HU compared to light curing through 1.5-mm-thick ceramic discs. Light curing through 3-mm-thick discs of IPS e.max CAD generally reduced VH and Y HU for all resin cements except SpeedCEM, which was the least affected by light curing through ceramic discs. CONCLUSIONS The resin cements responded heterogeneously to changes in curing mode. The applied irradiances and light curing times adequately cured the resin cements even through 1.5-mm-thick ceramic discs. CLINICAL RELEVANCE When light curing resin cements through thick glass ceramic restorations, clinicians should consider to prolong the light curing times even with LED curing units providing high irradiances.

Light curing through glass ceramics with a second- and a third-generation LED curing unit: effect of curing mode on the degree of conversion of dual-curing resin cements

Objectives The aim of this study was to measure the degree of conversion (DC) of five dual-curing resin cements after different curing modes with a second- and a third-generation light-emitting diode (LED) curing unit. Additionally, irradiance of both light curing units was measured at increasing distances and through discs of two glass ceramics for computer-aided design/manufacturing (CAD/CAM). Materials and methods Irradiance and spectra of the Elipar FreeLight 2 (Standard Mode (SM)) and of the VALO light curing unit (High Power Mode (HPM) and Xtra Power Mode (XPM)) were measured with a MARC radiometer. Irradiance was measured at increasing distances (control) and through discs (1.5 to 6 mm thickness) of IPS Empress CAD and IPS e.max CAD. DC of Panavia F2.0, RelyX Unicem 2 Automix, SpeedCEM, BisCem, and BeautiCem SA was measured with an attenuated total reflectance–Fourier transform infrared spectrometer when self-cured (negative control) or light cured in SM for 40 s, HPM for 32 s, or XPM for 18 s. Light curing was performed directly (positive control) or through discs of either 1.5- or 3-mm thickness of IPS Empress CAD or IPS e.max CAD. DC was analysed with Kruskal–Wallis tests followed by pairwise Wilcoxon rank sum tests (α = 0.05). Results Maximum irradiances were 1,545 mW/cm2 (SM), 2,179 mW/cm2 (HPM), and 4,156 mW/cm2 (XPM), and all irradiances decreased by >80 % through discs of 1.5 mm, ≥95 % through 3 mm, and up to >99 % through 6 mm. Generally, self-curing resulted in the lowest DC. For some cements, direct light curing did not result in higher DC compared to when light cured through ceramic discs. For other cements, light curing through ceramic discs of 3 mm generally reduced DC. Conclusions Light curing was favourable for dual-curing cements. Some cements were more susceptible to variations in curing mode than others. Clinical relevance When light curing a given cement, the higher irradiances of the third-generation LED curing unit resulted in similar DC compared to the second-generation one, though at shorter light curing times.

Incorporation of RANKL promotes osteoclast formation and osteoclast activity on β-TCP ceramics.

β-Tricalcium phosphate (β-TCP) ceramics are approved for the repair of osseous defects. In large defects, however, the substitution of the material by authentic bone is inadequate to provide sufficient long-term mechanical stability. We aimed to develop composites of β-TCP ceramics and receptor activator of nuclear factor κ-B ligand (RANKL) to enhance the formation of osteoclasts and promote cell mediated calcium phosphate resorption. RANKL was adsorbed superficially onto β-TCP ceramics or incorporated into a crystalline layer of calcium phosphate by the use of a co-precipitation technique. Murine osteoclast precursors were seeded onto the ceramics. After 15 days, the formation of osteoclasts was quantified cytologically and colorimetrically with tartrate-resistant acidic phosphatase (TRAP) staining and TRAP activity measurements, respectively. Additionally, the expression of transcripts encoding the osteoclast gene products cathepsin K, calcitonin receptor, and of the sodium/hydrogen exchanger NHA2 were quantified by real-time PCR. The activity of newly formed osteoclasts was evaluated by means of a calcium phosphate resorption assay. Superficially adsorbed RANKL did not induce the formation of osteoclasts on β-TCP ceramics. When co-precipitated onto β-TCP ceramics RANKL supported the formation of mature osteoclasts. The development of osteoclast lineage cells was further confirmed by the increased expression of cathepsin K, calcitonin receptor, and NHA2. Incorporated RANKL stimulated the cells to resorb crystalline calcium phosphate. Our in vitro study shows that RANKL incorporated into β-TCP ceramics induces the formation of active, resorbing osteoclasts on the material surface. Once formed, osteoclasts mediate the release of RANKL thereby perpetuating their differentiation and activation. In vivo, the stimulation of osteoclast-mediated resorption may contribute to a coordinated sequence of material resorption and bone formation. Further in vivo studies are needed to confirm the current in vitro findings.

Cytotoxicity evaluation of polymer-derived ceramics for pacemaker electrode applications.

Ceramics are known to be chemically stable, and the possibility to electrically dope polymer-derived ceramics makes it a material of interest for implantable electrode applications. We investigated cytotoxic characteristics of four polymer-derived ceramic candidates with either electrically conductive or insulating properties. Cytotoxicity was assessed by culturing C2C12 myoblast cells under two conditions: by exposing them to material extracts and by putting them directly in contact with material samples. Cell spreading was optically evaluated by comparing microscope observations immediately after the materials insertion and after 24 h culturing. Cell viability (MTT) and mortality (LDH) were quantified after 24-h incubation in contact with the materials. Comparison was made with biocompatible positive references (alumina, platinum, biocompatible stainless steel 1.4435), negative references (latex, stainless steel 1.4301) and controls (no material present in the culture wells). We found that the cytotoxic properties of tested ceramics are comparable to established reference materials. These ceramics, which are reported to be very stable, can be microstructured and electrically doped to a wide range of conductivity and are thus excellent candidates for implantable electrode applications including pacemakers.

Effect of the Synthesis Route on the Microstructure and the Dielectric Behavior of CaCu3Ti4O12 Ceramics

CaCu3Ti4O12 (CCTO) was prepared by a conventional synthesis (CS) and through reaction sintering, in which synthesis and sintering of the material take place in one single step. The microstructure and the dielectric properties of CCTO have been studied by XRD, FE-SEM, EDS, AFM, and impedance spectroscopy to correlate structure, microstructure, and electrical properties. Samples prepared by reactive sintering show very similar dielectric behavior to those prepared by CS. Therefore, it is possible to prepare CCTO by means of a single-step processing method.

Dielectric behaviour of Hf-doped CaCu3Ti4O12 ceramics obtained by conventional synthesis and reactive sintering

CaCu3(Ti4xHfx)O12 ceramics (JC = 0.04, 0.1 and 0.2) were prepared by conventional synthesis (CS) and through reactive sintering (RS), in which synthesis and sintering of the material take place in one single step. The microstructure and the dielectric properties of Hf-doped CCTO (CCTOHf) have been studied by XRD, FE-SEM, AFM, Raman and impedance spectroscopy (IS) in order to correlate the structure, microstructure and the electrical properties. Samples prepared by reactive sintering show slightly higher dielectric constant than those prepared by conventional synthesis in the same way than the pure CCTO. Dielectric constant and dielectric losses decrease slightly increasing Hf content. For CCTOHf ceramics with x> 0.04 for CS and x> 0.1 for RS, a secondary phase HfTi04 appears. As expected, the reactive sintering processing method allows a higher incorporation of Hf in the CCTO lattice than the conventional synthesis one.

Efecto del Cross-talk en la respuesta de un Transductor Ultrasónico tipo PZT

El presente trabajo de tesis investiga el efecto del fenómeno conocido como “Cross-talk” generado por el modo lateral de vibración, en la respuesta de un transductor ultrasónico formado por un arreglo de elementos piezoeléctricos tipo PZT (Zircanato Titanato de Plomo), la investigación se lleva a cabo desde el punto de vista de la naturaleza física de este efecto, así como de los parámetros asociados al mismo, así como un análisis del efecto del “Cross-talk” en la respuesta del transductor, formado por arreglos de elementos piezoeléctricos. Diversas investigaciones han abordado el fenómeno del “Cross-talk” y de sus efectos en la respuesta de los transductores, estos se han enfocado principalmente al modo espesor (thickness) de vibración. Sin embargo no ha habido un estudio a fondo para el estudio de este fenómeno en el modo lateral de vibración tema de interés de este trabajo de tesis. Este trabajo incluye simulaciones del fenómeno del “Cross-talk” mediante el método de los elementos finitos (MEF), así como la construcción de un transductor tipo matricial (arrray) de 2x3 elementos, en el que fueron realizadas las mediciones físicas del fenómeno. El trabajo abarca un estudio comparativo entre las simulaciones y las mediciones realizadas en el transductor, considerando que las cerámicas del transductor están montadas sobre diferentes materiales (backing) en donde la propagación de la energía emitida por las cerámicas piezoeléctricas provoca un mayor o menor grado de “Cross-talk” dependiendo de la velocidad en que se propaga dicha energía. Esta investigación también llevó a cabo el estudio del efecto del “Cross-talk” en el patrón de radiación que emite el arreglo de elementos piezoeléctricos, siendo este patrón de radiación un factor importante en la respuesta del transductor, motivo por el cual se realizó un análisis de cómo se ve afectado este patrón bajo la influencia del fenómeno del “Cross-talk”. Como ya se mencionó debido a la falta de un estudio a profundidad del fenómeno del “Cross-talk” en el modo lateral, la contribución del presente trabajo es importante ya que se enfoca al modo lateral de vibración de los elementos piezoeléctricos del arreglo. En particular se desarrollo una ecuación que permite cuantificar el fenómeno del “Cross-talk” y visualizar sus efectos en el arreglo. Derivando de este estudio se concluye que el fenómeno del “Cross-talk” generado por el modo lateral de vibración tiene un efecto significativo en la respuesta de los diferentes transductores matriciales considerados. ABSTRACT This thesis investigates the effect of the phenomenon known as crosstalk from the point of view of its physical nature and the elements that lead to the formation of this phenomenon to an analysis of how it may affect the performance of the ultrasonic transducer. This phenomenon occurs primarily in matrix arrays and this phenomenon is magnified by certain factors causing serious problems in the performance of a transducer. Researchers have addressed the phenomenon of crosstalk and their effects on the response of these transducers. They have mainly focused in the thickness vibration mode, and there has been no comprehensive study of this phenomenon in the lateral vibration mode, issue of interest of this thesis. This work includes simulations of the crosstalk phenomenon using the finite element method (FEM), and the construction of a matrix type transducer (array) of 2x3 elements, in which physical measurements were made. The work includes a comparative study between simulations and measurements in the transducer, whereas the ceramic transducer are mounted on different materials (backing) where the spread of the energy emitted by the piezoelectric ceramic causes a greater or lesser degree of crosstalk depending on the speed at which this energy spreads. This research also carried out the study of the effect of the crosstalk in the radiation pattern emitted by the piezoelectric array. The radiation pattern is an important factor in the response of the transducer that is why we conducted an analysis of how this pattern is affected under the influence of the crosstalk phenomenon. As mentioned before because of the lack of an in-depth study of the crosstalk phenomenon in the lateral vibration mode, the contribution of this work is important because it focuses in this vibration mode of the piezoelectric elements in the array. In particular, an equation was developed to quantify the crosstalk phenomenon and to see its effects in the array. Deriving from this study it is possible to conclude that the crosstalk phenomenon generated by the lateral vibration mode has a significant effect on the response of the different matrix transducers considered in this work.

D-depth profiling in as-implanted and annealed Li-based breeder blanket ceramics

In future power plants (i.e. DEMO), the nuclear fusion of hydrogen isotopes will be used for energy production. The behaviour of hydrogen isotopes in lithium-enriched ceramics for breeder blankets (BBs) is one of the most important items to be understood. In this paper we present the chemical, microstructural and morphological features of Li4SiO4, Li2TiO3 and a third ceramic candidate with a higher Li:Si proportion (3:1), implanted with D at an energy of 100 keV and at room temperature at a fluence of 1 × 1017 cm−2. The D depth-profile in as-implanted and annealed ceramics (at T ⩽ 200 °C) was characterised by Resonance Nuclear Reaction Analysis (RNRA). The RNRA data indicate that the total amount of D is retained at room temperature, while annealing at 100 °C promotes D release and annealing at T ⩾ 150 °C drives D to completely desorb from all the studied ceramics. D release will be discussed as a function of the microstructurural and morphological features of each material.

Mechanical properties up to 1900 K of Al2O3/Er3Al5O12/ZrO2 eutectic ceramics grown by the laser floating zone method

Directionally solidified Al2O3–Er3Al5O12–ZrO2 eutectic rods were processed using the laser floating zone method at growth rates of 25, 350and 750 mm/h to obtain microstructures with different domain size. The mechanical properties were investigated as a function of the processing rate. The hardness, 15.6 GPa, and the fracture toughness, 4 MPa m1/2, obtained from Vickers indentation at room temperature were practically independent of the size of the eutectic phases. However, the flexural strength increased as the domain size decreased, reaching outstanding strength values close to 3 GPa in the samples grown at 750 mm/h. A high retention of the flexural strength was observed up to 1500 K in the materials processed at 25 and 350 mm/h, while superplastic behaviour was observed at 1700 K in the eutectic rods solidified at the highest rate of 750 mm/h