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During the curing process of light curing dental composites the mobility of molecules and molecule segments is reduced leading to a significant increase of the viscosity as well as the ion viscosity. Thus, the kinetics of the curing behavior of 6 different composites was derived from dielectric analysis (DEA) using especially redesigned flat sensors with interdigit comb electrodes allowing for irradiation at the top side and measuring the ion viscosity at the bottom side. As the ion viscosities of dental composites change 1-3 orders of magnitude during the curing process, DEA provides a sensitive approach to evaluate their curing behavior, especially in the phase of undisturbed chain growth. In order to determine quantitative kinetic parameters a kinetic model is presented and examined for the evaluation of the ion viscosity curves. From the obtained results it is seen that DEA might be employed in the investigation of the primary curing process, the quality assurance of ingredients as well as the control of processing stability of the light curing dental composites.
- Klíčová slova
- Curing behavior, Curing kinetics, Dental composites, Dielectric analysis (DEA), Ion viscosity, Visible light curing,
- MeSH
- kinetika MeSH
- složené pryskyřice chemie účinky záření MeSH
- stomatologické polymerizační lampy * MeSH
- teplota MeSH
- testování materiálů MeSH
- tvrdost MeSH
- viskozita MeSH
- změna skupenství MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
- Názvy látek
- složené pryskyřice MeSH
OBJECTIVES: The aim of this study is to investigate depth dependent changes of polymerization process and kinetics of visible light-curing (VLC) dental composites in real-time. The measured quantity - "ion viscosity" determined by dielectric analysis (DEA) - provides the depth dependent reaction rate which is correlated to the light intensity available in the corresponding depths derived from light transmission measurements. METHODS: The ion viscosity curves of two composites (VOCO Arabesk Top and Grandio) were determined during irradiation of 40s with a light-curing unit (LCU) in specimen depths of 0.5/0.75/1.0/1.25/1.5/1.75 and 2.0mm using a dielectric cure analyzer (NETZSCH DEA 231 with Mini IDEX sensors). The thickness dependent light transmission was measured by irradiation composite specimens of various thicknesses on top of a radiometer setup. RESULTS: The shape of the ion viscosity curves depends strongly on the specimen thickness above the sensor. All curves exhibit a range of linear time dependency of the ion viscosity after a certain initiation time. The determined initiation times, the slopes of the linear part of the curves, and the ion viscosities at the end of the irradiation differ significantly with depth within the specimen. The slopes of the ion viscosity curves as well as the light intensity values decrease with depth and fit to the Lambert-Beer law. The corresponding attenuation coefficients are determined for Arabesk Top OA2 to 1.39mm(-1) and 1.48mm(-1), respectively, and for Grandio OA2 with 1.17 and 1.39mm(-1), respectively. For thicknesses exceeding 1.5mm a change in polymerization behavior is observed as the ion viscosity increases subsequent to the linear range indicating some kind of reaction acceleration. SIGNIFICANCE: The two VLC composites and different specimen thicknesses discriminate significantly in their ion viscosity evolution allowing for a precise characterization of the curing process even with respect to the polymerization mechanism.
- Klíčová slova
- Composite resin, Curing depth, Dental material, Dielectric analysis, Light attenuation, Real-time measurement, Restorative composite, Visible light-curing,
- MeSH
- složené pryskyřice * MeSH
- stomatologické polymerizační lampy * MeSH
- vazba zubní * MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
- Názvy látek
- složené pryskyřice * MeSH
The presented research program is focused on the design of a structural lightweight fiber-reinforced concrete harnessing an internal curing process. Pre-soaked waste red ceramic fine aggregate and pre-soaked artificial clay expanded coarse aggregate were utilized for the creation of the mix. Copper-coated steel fiber was added to the mix by volume in amounts of 0.0%, 0.5%, 1.0%, and 1.5%. Test specimens in forms of cubes, cylinders, and beams were tested to specify the concrete characteristics. Such properties as consistency, compressive strength, splitting tensile strength, static and dynamic modulus of elasticity, flexural characteristics, and shear strength were of special interest. The achieved concrete can be classified as LC12/13. A strength class, according to fib Model Code, was also assigned to the concretes in question. The proposed method of preparation of concrete mix using only pre-soaked aggregate (with no extra water) proved to be feasible.
- Klíčová slova
- SFRC, internal curing, recycling, sustainability, waste ceramic,
- Publikační typ
- časopisecké články MeSH
The rheometer curing curves of 50/50 blends of natural rubber (NR) and two different halogenated rubbers with a combination of conventional accelerated sulfur (CV) and 3 phr of a bismaleimide (MF3) at 170 °C indicates that a co-curing reaction has been taken place between NR and the halogenated rubbers via Diels-Alder reaction. To further confirm whether the co-curing reaction has taken place in the early stage of curing, a complex test methodology was applied with the help of a rubber process analyzer. In this test, the blends with CV and with CVMF3 were subjected to cure at 170 °C for a predetermined time so that both the CV and CVMF3 cured blends will have the same magnitude of curing torque. It is then cooled down to 40 °C and the storage modulus (G') was evaluated as a function of strain from 0.5% to 100% at a constant frequency of 1 Hz. The results reveal that the blends cured with CVMF3 exhibit a higher G' due to the enhanced network strength because of the formation of bismaleimide crosslinks than the same cured with only the CV system. The swelling resistance and the mechanical properties of the blends cured with CVMF3 were significantly higher than those cured with only the CV system.
- Klíčová slova
- curing, rheometer, rubber, rubber process analyzer, strain sweep,
- Publikační typ
- časopisecké články MeSH
In this study, a new generalized regression neural network model for predicting the curing characteristics of rubber blends with different contents of carbon black filler cured at various temperatures is proposed for the first time The carbon black contents in the rubber blend and cure temperature were used as input parameters, while the minimum and maximum elastic torque, scorch time, and optimal cure time, obtained from the analysis of 11 rheological cure curves registered at 10 various temperatures, were considered as output parameters of the model. A special pre-processing procedure of the experimental input and target data and the training algorithm is described. Less than 55% of the experimental data were used to significantly reduce the total number of input and target data points needed for training the model. Satisfactory agreement between the predicted and experimental data, with a maximum error in the prediction not exceeding 5%, was found. It is concluded that the generalized regression neural network is a powerful tool for intelligently modelling the curing process of rubber blends even in the case of a small dataset, and it can find a wide range of practical applications in the rubber industry.
- Klíčová slova
- curing process, generalized regression neural network, modelling, rubber blends,
- Publikační typ
- časopisecké články MeSH
Repair procedures with the use of composite patches are considered to be the most effective among the current technologies of repair of the structures of various applications. In the process of moulding-on of a patch made of polymeric composite material by means of curing, technological stresses arise in the patch. Determination of residual technological stresses is a priority task for the modelling of the repair process. Reduction of residual stresses can be achieved by optimization of the mode of repair patch curing. For meeting this objective, the method for determination of technological stresses, which arise in the structure under repair in the process of curing of a composite patch, has been developed. The method takes into account the shrinkage, change in physico-mechanical characteristics, rheological processes occurring in the binder during moulding process, and determination of stresses in the structure under repair at any time. Therefore, premature failure of the repair joint at the stage of repair can be avoided. It is shown that the method adequately describes the level of deformations and stresses in the structure being repaired at the stage of heating and holding of the composite patch. Increase in the moulding temperature leads to a reduction in residual stresses in the structure under repair. However, current stresses at the stages of heating and temperature holding are increased significantly. Reliability of assumptions and developed method is confirmed by the comparison with the experimental data. The obtained experimental graph of total deformation of the composite patch allowed us to clearly determine the moment of residual stress occurrence in the structure under repair. This moment matches quite exactly (with the discrepancy not exceeding 5 min) the gel point determined analytically based on dependence of the degree of curing on the moulding mode. Consequently, the research together with the results previously obtained allows making an integrated choice of geometric parameters of the repair composite patch and temperature-time regime of its curing in order to ensure the specified level of strength and stiffness of the structure under repair.
- Klíčová slova
- binder shrinkage, gelation, temperature–time regime,
- Publikační typ
- časopisecké články MeSH
The state of cure and the vulcanizate properties of a conventional accelerated sulfur (CV) cured 50/50 blend of natural rubber (NR) and bromobutyl rubber (BIIR) were inferior. However, this blend exhibits a higher extent of cure with remarkable improvements in its mechanical properties, particularly the tensile strength, modulus and hardness after curing with a combination of accelerated sulfur and three parts per hundred rubber (phr) of a bismaleimide (MF3). Moreover, with the use of 0.25 phr of dicumyl peroxide (DCP) along with the CV/MF3 system, the compression set property of the CV-only cured blend could be reduced from 68% to 15%. The enhanced compatibility between NR and BIIR with the aid of bismaleimide via the Diels-Alder reaction was identified as the primary reason for the improved cure state and the mechanical properties. However, the incorporation of a certain amount of bismaleimide as a crosslink in the NR phase of the blend, via a radical initiated crosslinking process by the action of DCP, is responsible for the improved compression set properties.
- Klíčová slova
- Diels–Alder reaction, bismaleimide, compression set, curing, rubber, tensile strength,
- Publikační typ
- časopisecké články MeSH
In this study, the influence of the technological parameters of autoclave curing on the resulting mechanical properties of laminates was investigated. The main criterion for optimizing the curing was to extend the processing window with a lower prepreg viscosity. At the same time, the issue of setting the pressure level before the heat ramp to the final cure temperature was also addressed. An experimental method of measuring the indentation viscosity of the prepreg was used to determine the viscosity profile. Despite the experimental nature of the method, the reliability of this method for rapid approximate identification of the processing window of the prepreg was verified by the results of the study. Several laminates with the same ply orientation were produced using the selected cure cycles, from which test specimens were cut with a water jet and inspected by confocal microscopy. The mechanical properties of tension and flexure were measured within the individual curing cycles using tests according to ISO standards. The data reported demonstrate that the experimental method of optimizing the curing parameters has successfully increased the selected mechanical properties. The resulting mechanical properties of the laminates were enhanced by up to 20% compared to the non-optimized cure cycle. The influence of the type of cure cycle on the resulting thickness of the cured laminate was evaluated in this study.
- Klíčová slova
- autoclave, carbon–epoxy prepreg, composite curing, cure cycle, mechanical properties,
- Publikační typ
- časopisecké články MeSH
Typically, polymeric composites containing nanoparticles are realized by incorporating pre-made nanoparticles into a polymer matrix by using blending solvent or by the reduction of metal salt dispersed in the polymeric matrix. Generally, the production of pre-made Au NPs occurs in liquids with two-step processes: producing the gold nanoparticles first and then adding them to the liquid polymer. A reproducible method to synthetize Au nanoparticles (NPs) into polydimethylsiloxane (PDMS) without any external reducing or stabilizing agent is a challenge. In this paper, a single-step method is proposed to synthetize nanoparticles (NPs) and at the same time to realize reproducible porous and bulk composites using laser ablation in liquid. With this single-step process, the gold nanoparticles are therefore produced directly in the liquid polymer. The optical properties of the suspensions of AuNPs in distilled water and in the curing agent have been analyzed by the UV-VIS spectroscopy, employed in the transmission mode, and compared with those of the pure curing agent. The electrical dc conductivity of the porous PDMS/Au NPs nanocomposites has been evaluated by the I-V characteristics. Scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) analysis have monitored the composition and morphology of the so-obtained composites and the size of the fabricated Au nanoparticles. Atomic force microscopy (AFM) has been used to determine the roughness of the bulk PDMS and its Au NP composites.
- Klíčová slova
- absorbance, curing time, laser ablation in medium, nanoparticles, polydimethylsiloxane, porous composite, scanning electron microscopy,
- MeSH
- dimethylpolysiloxany chemie MeSH
- kovové nanočástice chemie MeSH
- laserová terapie * MeSH
- nanokompozity chemie MeSH
- poréznost MeSH
- zlato chemie MeSH
- Publikační typ
- časopisecké články MeSH
- Názvy látek
- dimethylpolysiloxany MeSH
- zlato MeSH
At present, the most commonly used electrical insulating materials, including cold-curing epoxy resins, are well designed for normal operating conditions. However, new generations of materials should also be capable of withstanding extreme emergency conditions, e.g., in case of fire. For this reason, this study presents the possibilities of an improved cold-curing epoxy resin using halloysite nanotubes (HNTs) to increase its operational safety. The positive effect of HNT addition is indicated mainly in terms of the suppression of thermo-oxidation processes, which has been demonstrated by the decreases in the maximum heat flow peaks as well as the specific enthalpy values during the thermal decomposition of the epoxy resin. The observed dielectric parameters of the HNT-added materials differ only slightly from those without a filler, whereas their mechanical properties strongly depend on the amount of dispersed HNTs.
- Klíčová slova
- dielectric properties, epoxy-based composites, fire retardancy, halloysite nanotubes, mechanical properties, thermal properties,
- Publikační typ
- časopisecké články MeSH