New evaluation method for the curing degree of rubber and its nanocomposites using ATR-FTIR spectroscopy

Muroga, Shun; Takahashi, Yasuhiro; Hikima, Yuta; Ata, Seisuke; Ohshima, Masahiro; Okazaki, Toshiya; Hata, Kenji

doi:10.1016/j.polymertesting.2020.106993

Cited by 24 publications

(14 citation statements)

References 30 publications

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“…Figure 1 b shows a series of ATR-FTIR spectra of FKM samples at different measurement times. In the spectra, two distinct absorption bands were observed: one is the C=O stretching at 1699 cm −1 and the other is C=C stretching band at 1656 cm −1 [ 34 , 39 , 40 , 41 ]. The evolution of the spectra was observed via the broadening of the C=O stretching band.…”

Section: Resultsmentioning

confidence: 99%

“…In our previous work, the C=O stretching of TAIC was related to the degree of cure in FKM prepared by different molding conditions regardless of fillers [34]. Here, we determined the degree of cure at the surface of rubber measured by in situ ATR-FTIR, α surf , as follows:…”

Section: Methodsmentioning

confidence: 99%

“…Each ATR-FTIR spectrum was subjected to the baseline correction and subsequently normalized by the absorbance of C–F stretching in FKM at 1396 cm −1 , whose intensity was not changed during the curing process. The change in the TAIC concentration can be evaluated by the integrated absorbance of the C=O stretching band using Simpson’s rule in a similar manner of our previous work [ 34 ]. The penetration depth of evanescent waves is approximately 0.93 μm at 1700 cm −1 (C=O stretching region), and the refractive index is 2.42 (fluorine rubber matrix), which is sufficiently smaller than the sample thickness.…”

Section: Methodsmentioning

confidence: 99%

“…In our previous work, the C=O stretching of TAIC was related to the degree of cure in FKM prepared by different molding conditions regardless of fillers [ 34 ]. Here, we determined the degree of cure at the surface of rubber measured by in situ ATR-FTIR,

, as follows:

where

is the full width at half maximum (FWHM) of C=O stretching at each time

is the maximum FWHM of C=O stretching, and

is the minimum FWHM of C=O stretching.…”

Section: Methodsmentioning

confidence: 99%

“…TAIC is widely used as a trifunctional curing agent for radical curing (heat or electron beam) of plastics and rubbers for toughening and improving thermal stability [ 29 , 30 , 31 , 32 , 33 ]. Our previous work reported that the broadening of the peak of C=O in triallyl isocyanurate rather than that of cleaved C=C was highly correlated with the degree of cure due to the steric hindrance induced by the curing reaction [ 34 ]. The changes in the C=O by steric hindrance was quantitatively validated by the relationship between the crosslinking density and the Young’s modulus and the robustness of the approach against curing temperature, curing time, filler kind, and filler content was clearly demonstrated.…”

Section: Introductionmentioning

confidence: 99%

See 4 more Smart Citations

Novel Approaches to In-Situ ATR-FTIR Spectroscopy and Spectroscopic Imaging for Real-Time Simultaneous Monitoring Curing Reaction and Diffusion of the Curing Agent at Rubber Nanocomposite Surface

et al. 2021

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Here, we propose a novel attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy method for simultaneously monitoring the curing reaction and the diffusion behavior of curing agents at the surface of rubber in real-time. The proposed scheme was demonstrated by fluorine rubber (FKM) and FKM/carbon nanotube (CNT) nanocomposites with a target curing agent of triallyl-isocyanurate (TAIC). The broadening and the evolution of the C=O stretching of TAIC were quantitatively analyzed to characterize the reaction and the diffusion. Changes in the width of the C=O stretching indicated the reaction rate at the surface was even faster than that of the bulk as measured by a curemeter. The diffusion coefficient of the curing agent in the course of heating was newly calculated by the initial increase in the absorbance and our model based on Fickian diffusion. The diffusion coefficients of TAIC during curing were evaluated, and its temperature and filler dependency were identified. Cross-sectional ATR-FTIR imaging and in situ ATR-FTIR imaging measurements supported the hypothesis of the unidirectional diffusion of the curing agent towards the heated surface. It was shown that our method of in situ ATR-FTIR can monitor the degrees of cure and the diffusion coefficients of curing agents simultaneously, which cannot be achieved by conventional methods, e.g., rheological measurements.

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Section: Resultsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

“…In our previous work, the C=O stretching of TAIC was related to the degree of cure in FKM prepared by different molding conditions regardless of fillers [ 34 ]. Here, we determined the degree of cure at the surface of rubber measured by in situ ATR-FTIR,

, as follows:

where

is the full width at half maximum (FWHM) of C=O stretching at each time

is the maximum FWHM of C=O stretching, and

is the minimum FWHM of C=O stretching.…”

Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

Novel Approaches to In-Situ ATR-FTIR Spectroscopy and Spectroscopic Imaging for Real-Time Simultaneous Monitoring Curing Reaction and Diffusion of the Curing Agent at Rubber Nanocomposite Surface

et al. 2021

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Effects of composite reinforcing filler, vulcanizing temperature, and pressure on mechanical properties of gasket material for proton exchange membrane fuel cells

Hou

Yin

et al. 2022

J of Applied Polymer Sci

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Gasket is one of the key components in proton exchange membrane fuel cells (PEMFCs), and the performance of the gasket can directly affect the durability and electrochemical performance of the PEMFCs. In this paper, the silicone rubber material, which is being considered as gasket material for PEMFC, was fabricated with different composite reinforcing fillers at different vulcanizing temperatures under different vulcanizing pressures. Effects of the composite reinforcing fillers (i.e., gas-phase SiO 2 and nano-CaCO 3 ), vulcanizing temperatures, and pressures on mechanical properties of the silicone rubber material were investigated. The tensile, hardness measurement, compression set, and compression stress relaxation experimental results show that the mass ratios of the gas-phase SiO 2 to nano-CaCO 3 , curing temperatures, and pressures had a significant impact on the mechanical properties of PEMFC gasket materials. It is found that the silicone rubber material cured at a vulcanization temperature of 160 C and a vulcanization pressure of 10 MPa had good compression mechanical properties compared to the materials cured at the other curing temperatures and curing pressures. Orthogonal test results show that, when mass ratio of the gas-phase SiO 2 to nano-CaCO 3 was 25:20, the silicone rubber material cured at the curing temperature of 160 C and under the curing pressure of 10 MPa had good compressive stress relaxation performance in this work.

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Vulcanization behavior and thermal performance of peroxide‐curable fluoroelastomer

Wang

Zheng-tao

2022

J of Applied Polymer Sci

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Different coagents including triallyl isocyanurate (TAIC) and trimethallyl isocyanurate (TMAIC) were applicated on peroxide curable fluoroelastomer (FKM). The cure efficiency for TAIC has found to be higher than TMAIC using rubber process analyzing (RPA). Moreover, TAIC also creates extra exothermal peak and greater enthalpy in Differential scanning calorimetry test. In addition, X‐ray photoelectron spectra further demonstrated that TMAIC expresses low tendency on crosslinking with cure sites and homopolymerization, the network formed by TMAIC expressed more prominent degradation under thermo‐oxidative aging which also supported by mechanical properties. In the end, different network modes were purposed corresponding to vulcanizates using TAIC and TMAIC, and the network consisting relatively long segments of TAIC polymer exhibits better stability during thermo‐oxidative aging.

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New evaluation method for the curing degree of rubber and its nanocomposites using ATR-FTIR spectroscopy

Cited by 24 publications

References 30 publications

Novel Approaches to In-Situ ATR-FTIR Spectroscopy and Spectroscopic Imaging for Real-Time Simultaneous Monitoring Curing Reaction and Diffusion of the Curing Agent at Rubber Nanocomposite Surface

Novel Approaches to In-Situ ATR-FTIR Spectroscopy and Spectroscopic Imaging for Real-Time Simultaneous Monitoring Curing Reaction and Diffusion of the Curing Agent at Rubber Nanocomposite Surface

Effects of composite reinforcing filler, vulcanizing temperature, and pressure on mechanical properties of gasket material for proton exchange membrane fuel cells

Vulcanization behavior and thermal performance of peroxide‐curable fluoroelastomer

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