Polymerization monitoring using ultrasound (original) (raw)
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High temperature polymerization monitoring of an epoxy resin using ultrasound
IOP Conference Series: Materials Science and Engineering
In this study, the real time ultrasonic monitoring is investigated to quantify changes in physical and mechanical properties during the manufacture of composite structures. In this context, an experimental transmission was developed with the aim of characterizing a high temperature polymerization reaction and post-curing properties using an ultrasonic method. First, the monitoring of ultrasonic parameters of a thermosetting resin is carried out in a device reproducing the experimental conditions for manufacturing a composite material with a process known as RTM, that is to say an isothermal polymerization at T = 160°C. During this curing, the resin is changing from its initial viscous liquid state to its final viscous solid state. Between those states, a glassy transition stage is observed, during which the physical properties are strongly changing, i.e. an increase of the ultrasonic velocity up to its steady value and a transient increase of the ultrasonic attenuation. Second, the ultrasonic inspection of the thermosetting resin is performed during a heating and cooling process to study the temperature sensitivity after curing. This type of characterization leads to identifying the ultrasonic properties dependence before, during and after the glassy transition temperature Tg. Eventually, this study is composed of two complementary parts: the first is useful for the curing optimization, while the second one is fruitful for the post-processing characterization in a temperature range including the glassy transition temperature Tg.
Polymerization monitoring and porosities detection in composites materials during manufacturing
The polymerization of a resin is of the main interest during the fabrication of a composite material. In the case of a Resin Transfer Molding (RTM) process, the monitoring of resin polymerization can inform about the evolution of the process parameters. In this work, ultrasonic velocity and attenuation in the resin are monitored using a broadband ultrasonic transducer. Using this method, the time dependence of the characterized parameters allows determining the polymerization characteristics such as the beginning, the end or the inflexion point of the studied parameter. Through these measurements, the evolution of polymerization, could be related to the process and environmental conditions (such as temperature) in order to consider improvements to the RTM technique.
In this paper the monitoring of ultrasonic parameters of a thermosetting resin during an isothermal curing process is described. The ultrasonic properties are studied within the context of the monitoring of composite plate production by resin transfer molding (RTM). These ultrasonic characteristics can be related directly to cure kinetic models. An ultrasonic method, based on the measurement of the elastic constant and associated mechanical loss has been developed to identify the variations of the phase transformation. To study the reaction kinetics, the time dependence of the elastic coefficient is modeled using a Weibull distribution. The approximate time derivative form of this Weibull model makes it possible to find the relationship between ultrasonic parameters and the chemical Kamal model. The ultrasonic monitoring of a cooling process was also performed to study the temperature sensitivity after curing. Thanks to experimental measurements of the ultrasonic velocity and attenuation, the power law coefficient variations and their temperature sensitivity can be examined. The resulting viscoelastic Cole-Cole parameters were estimated and a frequency-temperature (f, T) model was proposed.
Monitoring the Cure State of Thermosetting Resins by Ultrasound
Materials, 2013
The propagation of low intensity ultrasound in a curing resin, acting as a high frequency oscillatory excitation, has been recently proposed as an ultrasonic dynamic mechanical analysis (UDMA) for cure monitoring. The technique measures sound velocity and attenuation, which are very sensitive to changes in the viscoelastic characteristics of the curing resin, since the velocity is related to the resin storage modulus and density, while the attenuation is related to the energy dissipation and scattering in the curing resin. The paper reviews the results obtained by the authors' research group in the last decade by means of in-house made ultrasonic set-ups for both contact and air-coupled ultrasonic experiments. The basics of the ultrasonic wave propagation in polymers and examples of measurements of the time-evolution of ultrasonic longitudinal modulus and chemical conversion of different thermosetting resins are presented. The effect of temperature on the cure kinetics, the comparison with rheological, low frequency dynamic mechanical and calorimetric results, and the correlation between ultrasonic modulus and crosslinking density will be also discussed. The paper highlights the reliability of ultrasonic wave propagation for monitoring the physical changes taking place during curing and the potential for online monitoring during polymer and polymer matrix composite processing.
Air-Coupled Ultrasonic Cure Monitoring of Unsaturated Polyester Resins
Macromolecular Symposia, 2007
Air-coupled ultrasound in one-side transmission mode has been applied to monitor the curing process of an unsaturated polyester resin, commonly used as a matrix in glass reinforced composites. The evolution of the resin mechanical properties during cure has been measured from the variation of longitudinal velocity. The technique has demonstrated to be a very powerful tool for detecting the structural changes occurring at gelation and vitrification. The no-contact ultrasonic results have been compared with those obtained using conventional contact ultrasonic measurements, characterized by direct coupling between the transducer and the resin, and with the rheological measurements. The good agreement among the results of the different techniques demonstrates the reliability of air-coupled ultrasound in monitoring the changes of viscoelastic properties occurring during the cure of thermosetting polymers. A further advantage of the proposed one-side ultrasonic technique is the absence of physical contact between the transducers and the sample, which is relevant during composite manufacturing, where probe contact could adversely affect the part quality or access from both sides is not practicable. No-contact ultrasonic cure monitoring is suitable for both stationary and moving liquid or solid samples in several process conditions such as moulding, filament winding, etc., opening the way to new applications of ultrasound in the composite industry.
The Journal of the Acoustical Society of America, 2016
Real-time ultrasonic monitoring is investigated to quantify changes in physical and mechanical properties during the manufacture of composite structures. In this context, an experimental transmission was developed with the aim of characterizing a high temperature polymerization reaction and post-curing properties using an ultrasonic method. First, the monitoring of ultrasonic parameters of a thermosetting resin is carried out in an isothermal polymerization process at 160°C. During this curing, the resin is changing from its initial viscous liquid state to its final viscous solid state. Between those states, a glassy transition stage is observed, during which the physical properties are strongly changing, i.e. an increase of the ultrasonic velocity up to its steady value and a transient increase of the ultrasonic attenuation. Secondly, the ultrasonic inspection of the thermosetting resin is performed during a heating and cooling process to study the temperature sensitivity after curing. This type of characterization lead to identifying the ultrasonic properties dependence before, during and after the glassy transition temperature T g. This study is composed of two complementary parts: the first is useful for the curing optimization, while the second one is fruitful for the post-processing characterization in a temperature range including the glassy transition temperature.
Polymer characterization by ultrasonic wave propagation
Advances in Polymer Technology, 2009
The propagation of low-intensity ultrasound in polymers, acting as a high-frequency dynamic mechanical deformation, can be successfully used to monitor changes in the modulus of polymers associated with glass transition, crystallization, cross-linking, and other chemical and physical phenomena related to changes in viscoelastic behavior, such as gelation phenomena. The velocity of sound is related to the polymer storage modulus and density, whereas the absorption of ultrasonic waves is related to the energy dissipation in the material and, therefore, to the loss modulus. Accordingly, ultrasonic measurements have been used by several authors to monitor the evolution of the viscoelastic moduli of polymers as a function of time or temperature and, recently, become a characterization technique of its own right, generally known as ultrasonic dynamic mechanical analysis (UDMA). Often the technique is used in conjunction with rheological methods as a means of providing a better insight into the viscoelastic behavior of polymer systems. As yet UDMA is underutilized-primarily because of the low-operating temperatures (usually below 100 • C)-of commercially available ultrasonic transducers, and also due to the requirement of a coupling medium to ensure an efficient energy transfer mechanism between the transducer and the test material. Despite these limitations, this paper shows that the use of ultrasonics is potentially a powerful method for the characterization of polymers, particularly as a tool for online monitoring of events occurring during polymer processing and in the manufacture of polymer matrix composites. The aim of this paper is to review the progress made in recent years, highlighting the potential and reliability of UDMA for monitoring physical transitions in polymers such as glass transition, melting, crystallization, as well as physical changes taking place during curing of Q2
Materials Research Innovations, 2011
A non-destructive ultrasonic attenuation measurement is adopted to characterise the state of polymers in the cavity during injection moulding. According to the relationship between ultrasonic attenuation behaviours and polymer viscosity, elasticity transition as well as crystallisation, the evolution of ultrasonic attenuations for an amorphous polymer (general purpose polystyrene) and a crystalline polymer (polypropylene) were discussed. Experimental results show that the ultrasonic attenuation measurement can not only provide information of the amorphous polymer on filling start, filling stop, elasticity transition and detachment from the mould, but can also extract information of crystallisation for the crystalline polymer throughout the injection moulding process. The ultrasonic attenuation measurement is a potential candidate technology to characterise the state of polymers in the cavity and thereby optimise the injection moulding process for perfect products.