Simultaneous DSC-FTIR spectroscopy: Comparison of cross-linking kinetics of an epoxy/amine resin system

Pandita, Surya D.; Wang, Liwei; Mahendran, Ramani S.; Machavaram, Venkata R.; Irfan, Muhammad Shafiq; Harris, Don; Fernando, Gerard Franklyn

doi:10.1016/j.tca.2012.04.024

Cited by 53 publications

(44 citation statements)

References 29 publications

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“…The epoxy conversion can also be measured directly by structural changes using spectroscopic methods like near-infrared (NIR) [4,[22][23][24][25], mid-infrared (MIR) [26][27][28][29] or Raman [30][31][32] spectroscopy. In the NIR region bands are often difficult to evaluate due to mode coupling and overtones, hence MIR spectroscopy is often preferred to analyse chemical composition.…”

Section: Introductionmentioning

confidence: 99%

Analyzing the network formation and curing kinetics of epoxy resins by in situ near-infrared measurements with variable heating rates

et al. 2015

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Section: Introductionmentioning

confidence: 99%

Analyzing the network formation and curing kinetics of epoxy resins by in situ near-infrared measurements with variable heating rates

et al. 2015

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“…The discrepancy between the measured and predicted rate of depletion is generally attributed to: (i) a change in the reaction mechanism from chemical-controlled to diffusion-controlled reactions towards the latter stages [10]; (ii) the fact that the rate constants for the primary and secondary amine reaction rates may be different (a single rate Table 2 Rate constant k for the EPO-TEK ® 310M resin system when using transmission and evanescent wave Fourier transform infrared spectroscopy at specified processing temperatures. constant is assumed in the auto-catalytic model) [21]; (iii) the sum of the reaction orders, m and n, being forced to equate to an integer (2 in the current case) in the curve fitting routine; (iv) the observation that when the epoxy conversions are greater than 80%, the signal-to-noise decreases progressively. In contrast to Fig.…”

Section: Discussionmentioning

confidence: 99%

“…In a previous study [21], the authors used ii-demountable 1 mm path length quartz cuvette; iii-SMA connector enabling optical connection to the spectrometer; iv-impregnated E-glass bundle attached to a pair of SMA connectors; v-thermocouple; and vi-purpose-built oven.…”

Section: Cross-linking Kineticsmentioning

confidence: 99%

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In-situ monitoring of cross-linking reactions using E-glass fibres and evanescent wave spectroscopy

Wang

Tomlin

Pandita

et al. 2016

Sensors and Actuators B: Chemical

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a b s t r a c t E-glass fibres are used in products such as printed circuit boards, wind turbine blades, pipes, marine vehicles and pressure vessels. With reference to the production of fibre reinforced composites, the reinforcement (E-glass) is impregnated with a resin system, consolidated and generally processed by the application of heat. This results in the resin system being converted from a liquid or semi-solid to a highly cross-linked and infusible solid. There is significant interest in monitoring the progression of these crosslinking or chemical reactions and a number of optical and electrical, ultrasonic-based techniques have been developed and demonstrated. The current paper reports on the use of the reinforcing E-glass fibres to track the cross-linking of commercially available epoxy/amine resin systems. The mode of interrogation was based on using the E-glass fibres as evanescent wave sensors thus enabling Fourier transform infrared spectroscopy to be conducted. This enabled the cross-linking reactions at the glass/resin interface to be monitored. Conventional transmission Fourier transform infrared spectroscopy experiments were also conducted. The cross-linking kinetic data from the two methods were modelled and compared. A good correlation was obtained between the experimental and predicted data using a single rate constant.

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“…7,8 Such flexibility of FTIR has been employed also for simultaneous measurement with differential scanning calorimetry (DSC). 9,10 In this study, we tried to establish the simultaneous SANS/ FTIR measurement protocol. For this purpose, a device consisting of a portable FTIR spectrometer and an optical system, which allows a sample to be irradiated with neutron and infrared beams simultaneously, was developed and installed on a smallangle neutron diffractometer.…”

mentioning

confidence: 99%

Development of a Simultaneous SANS/FTIR Measuring System

et al. 2015

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A novel method for the simultaneous measurement of smallangle neutron scattering and Fourier transform infrared spectroscopy (SANS/FTIR) has been developed. The method was realized by building a device consisting of a portable FTIR spectrometer and an optical system that allows both a neutron beam and an infrared beam to pass through a sample coaxially. The device was installed on a small-angle neutron diffractometer, KWS2 of the Jülich Centre for Neutron Science (JCNS) outstation at Heinz Maier-Leibnitz Center (MLZ) in Garching, Germany. In order to check the performance of this measuring system, the structural changes in a cocrystal of syndiotactic polystyrene with triethylene glycol dimethyl ether, were followed during the course of heating.Small-angle neutron scattering (SANS) is a powerful and convenient method to investigate the higher-order structure of static polymer systems. Owing to technological developments in instruments such as detectors and neutron guides, SANS has extended its presence, even to research concerning timedependent structural evolution.The scattering pattern of SANS is determined by the scattering length density (SLD) profile of the object under study, and therefore, it is of great difficulty to derive the sole solution for the arrangement of constituent components from the scattering pattern of SANS. Accordingly, if a system of interest is a multicomponent one, the interpretation of the time-dependent changes in SANS profile is not easy. There are usually several alternatives to explain the variations in the SANS profile, and it is laborious to select an option from them. 1,2 It is desirable to obtain two or more different kinds of structural information simultaneously from the same sample, which would drastically reduce ambiguities in interpretation. Vibrational spectroscopy has been employed as a complementary tool to X-ray and neutron diffractometry for investigating the structure of polymer systems. Simultaneous analyzes by X-ray scattering and Fourier transform infrared spectroscopy (FTIR) have been developed so far. 36 We expect that the combination of SANS with FTIR would also produce a fruitful methodology for such a simultaneous measurement system. Owing to a high-throughput optical system, a highly sensitive detector, and advanced hardware and software design, it is easy to follow the time-evolution of infrared spectra with a compact FTIR spectrometer. 7,8 Such flexibility of FTIR has been employed also for simultaneous measurement with differential scanning calorimetry (DSC). 9,10 In this study, we tried to establish the simultaneous SANS/ FTIR measurement protocol. For this purpose, a device consisting of a portable FTIR spectrometer and an optical system, which allows a sample to be irradiated with neutron and infrared beams simultaneously, was developed and installed on a smallangle neutron diffractometer. In the proof-of-concept experiment described here, we followed the structural changes on heating a crystalline complex system of syndiotactic polystyrene (sPS) with...

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Simultaneous DSC-FTIR spectroscopy: Comparison of cross-linking kinetics of an epoxy/amine resin system

Cited by 53 publications

References 29 publications

Analyzing the network formation and curing kinetics of epoxy resins by in situ near-infrared measurements with variable heating rates

Analyzing the network formation and curing kinetics of epoxy resins by in situ near-infrared measurements with variable heating rates

In-situ monitoring of cross-linking reactions using E-glass fibres and evanescent wave spectroscopy

Development of a Simultaneous SANS/FTIR Measuring System

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