In the present work the value of the degree of the area swept by the polymer chain due to an electrical force for a given mesostructure was related to the corresponding value of the dielectric strength. This value was deduced from the electric inclusion formalism applied to dynamic mechanical analysis (DMA) studies conducted under high electric field, which were performed in commercial ethylene-propylene-diene M-class rubber (EPDM); used for the housing of polymeric electrical insulators. EPDM samples with different arrangements of the polymer chains and crystalline degree, promoted by controlled neutron irradiation were studied. Several characterization techniques, as infrared absorption spectroscopy (IR), differential scanning calorimetry (DSC), positron annihilation lifetime spectroscopy (PALS) and dielectric strength (DS) were also used. The relationship between the DS and the degree of movement of polymer chains promoted by electrical forces coming from the electric field applied in a non destructive test as the DMA was successfully established. In fact, a larger empty space in the sample leads to larger areas swept by the polymer chains during bending under the application of the field strength in the dynamic mechanical analysis tests. Therefore, an increase in the capability of movement of charges occurs, corresponding to smaller dielectric strength values. Crystallinity improves the dielectric strength due to the increase in the internal stresses which decreases the capability of movement of the polymer chains and electric carriers by electric forces.
In order to find the best combination of three synthetic rubbers, that is, styrene‐butadiene rubber (SBR) grade 1712, SBR grade 1721 and high‐1,4‐cis polybutadiene, that produce a compound with specific end‐use properties, a statistical experimental design is proposed in this work. The design consists of ten mixtures containing specific amounts of total styrene and BR content. A number of properties are tested in each mixture, selecting those related to requirements for the tread of a high performance tire: glass transition temperature (Tg), the ratio between the viscous modulus and the elastic modulus (tanδ@60 °C), Mooney viscosity, and the tensile properties. The values obtained for each property are fit to statistically significant models, obtaining the respective response surfaces. These are next used to define a desirable formulation with the optimal ratio of each rubber, and finally the optimized formulation is validated by comparing the experimental and predicted values for each modeled property. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018, 135, 46548.
The changes in the degree of crystallinity in commercial Ethylene Propylene Diene rubber-type M (EPDM) irradiated with neutrons at different doses has been studied by means of inelastic neutron scattering and infrared absorption spectroscopy experiments. EPDM samples were taken from the housing of non-ceramic electrical insulators which are used in outdoor transmission lines of 66 kV. Inelastic neutron scattering spectra were recorded at 5 K with an accessible energy-transfer range between 180 -3500 cm -1 . Infrared studies were performed at room temperature with an energy transfer between 4000 -400 cm -1 . Controlled neutron irradiation allows to obtain different volume fraction and size of crystalline zones in EPDM. The obtained results are discussed and correlated with studies of differential scanning calorimetry, dynamic mechanical analysis and positron annihilation lifetime spectroscopy from where the changes in crystallinity in EPDM were indirectly studied. Inelastic neutron scattering studies were not appropriate for determining the changes in the crystallinity degree in neutron irradiated commercial EPDM. In contrast, from infrared absorption spectroscopy the changes in crystallinity could be determined successfully.
RESUMEN Cuando se fabrica una pieza de goma, se parte de un “compuesto de caucho” que puede estar conformado por uno o más elastómeros y diferentes cargas. El desarrollo de una mezcla para elaborar un compuesto con un uso final específico es una tarea complicada en el ámbito de la tecnología del caucho. Por esto el desarrollo exitoso de un compuesto requiere de un trabajo sistemático siendo clave el uso de un diseño experimental estadístico (DoE). Al implementar el DoE, deberán seleccionarse las variables para el sistema bajo investigación; las variables observadas o medidas (respuesta, propiedades del compuesto que desean controlarse) y las variables independientes que describen al sistema (los ingredientes y cantidades en la formulación del compuesto). El propósito del DoE es especificar el valor de las variables independientes, como también seleccionar la respuesta apropiada. La estrategia DoE se ensayó anteriormente al utilizar dos grados de cauchos E-SBR (estireno-butadieno en emulsión), E-SBR 1712 y E-SBR 1721 y un caucho BR (polibutadieno) alto cis, con la finalidad de encontrar una mezcla de éstos que posea propiedades comparables a las de un neumático de alto rendimiento. En este trabajo se muestra el uso de la estrategia DoE para optimizar el agregado de un aceite extendedor al compuesto. Se utiliza una mezcla de tres tipos de aceites, dos aceites petroquímicos (Pq1 y Pq2) y un aceite vegetal de soja, buscando maximizar la cantidad de este último. Las propiedades a ensayar se relacionan con características requeridas para la banda de rodamiento de un neumático: temperatura de transición vítrea (Tg); relación entre módulo viscoso y módulo elástico (tanδ@60°C); Viscosidad Mooney y propiedades de tracción-elongación. Los valores obtenidos de cada propiedad se intentaron ajustar a modelos estadísticamente significativos, obteniéndose superficies de repuesta para cada una de ellas. Las superficies se combinan en la función deseabilidad, bajo ciertos criterios tanto para las propiedades buscadas, como también para la cantidad a usar de cada tipo de aceite en el compuesto óptimo deseable. Aplicando la función deseabilidad se logró predecir la composición óptima de aceites en el compuesto para alcanzar las propiedades deseadas, (3,17 pHR de aceite Pq1, 5,90 pHR de aceite Pq2 y 7,86 pHR de aceite de soja). La validación satisfactoria de los modelos propuestos muestra la capacidad del DoE como estrategia útil para la optimización de propiedades en un compuesto de caucho de formulación compleja.
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