Fourier-Transform Infrared Analysis of a Linear, Anhydride-Cured Epoxy

Tadros, R M; Timm, D. C.

doi:10.1021/ma00126a024

Cited by 17 publications

(21 citation statements)

References 8 publications

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“…Both the mid‐IR15 and near‐IR16–19 regions of the spectra have been explored for finding the degree of conversion of the epoxy resin. The small‐ring epoxy compounds usually absorb at three positions in the mid‐IR region: a medium‐intensity symmetric stretching vibration in the range 1280–1230 cm −1 , a strong asymmetric band between 950 and 815 cm −1 , and a strong band20 between 880 and 750 cm −1 .…”

Section: Resultsmentioning

confidence: 99%

Cationic electron‐beam curing of a high‐functionality epoxy: effect of post‐curing on glass transition and conversion

Rath¹,

Boey²,

Abadie³

2004

Polymer International

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This paper reports on the cationic electron‐beam curing of a high‐functionality SU8 epoxy resin, which is extensively used as a UV‐curing negative photoresist for micro‐electronics machine systems (MEMS) applications. Results show that elevated post‐curing treatment significantly increased both the conversion and the glass transition. The degree of conversion and the glass transition temperature were measured by using Fourier‐transform infrared (FTIR) spectroscopy and modulated differential scanning calorimetry (MDSC®), respectively. The glass transition temperature (Tg), which has been observed to be dependent on the degree of conversion, reaches a maximum of 162 °C at 50 Mrad and post‐curing at 90 °C. The degradation pattern of the cured resin does not show much variation for exposure at 5 Mrad, but does show significant variation for 50 Mrad exposure at various post‐curing temperatures. A degree of conversion of more than 0.8 was achieved at a dosage of 30 Mrad with post curing at 80 °C, for the epoxy resin with an average functionality of 8 a feature simply not achievable when using UV‐curing. Copyright © 2004 Society of Chemical Industry

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Section: Resultsmentioning

confidence: 99%

Cationic electron‐beam curing of a high‐functionality epoxy: effect of post‐curing on glass transition and conversion

Rath¹,

Boey²,

Abadie³

2004

Polymer International

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“…The direct methods allow the evaluation of the concentration of one or more reactive groups as a function of time. They include gel permeation chromatography (GPC), 8 nuclear magnetic resonance (NMR), 9 electron paramagnetic resonance, 10 Fourier transform infrared spectroscopy (FTIR), [11][12][13] and Raman spectroscopy. 14 Indirect analysis gives only an assessment of the degree of cure by monitoring, as a function of time, a physical property directly correlated with the reactants' conversion.…”

Section: Introductionmentioning

confidence: 99%

Tetrafunctional epoxy resins: Modeling the curing kinetics based on FTIR spectroscopy data

Musto

Martuscelli

Ragosta

et al. 1999

J. Appl. Polym. Sci.

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ABSTRACT:The curing kinetics of two thermosetting systems based on a tetrafunctional epoxy resin was investigated by Fourier transform infrared spectroscopy. Two formulations were studied, in which the hardener was an aromatic diamine and a carboxylic dianhydride, respectively. The quantitative evaluation of the epoxy conversion was based on spectra collected in the near-infrared range (8000 -4000 cm Ϫ1) as well as in the medium infrared range (4000 -400 cm Ϫ1 ). The kinetic parameters evaluated in the above frequency intervals were significantly different. The reasons for such a discrepancy are discussed critically. Several kinetic models, based on the widely employed Kamal approach, were applied to verify their predictive capability. Satisfactory results were obtained for the amine-cured system, particularly with a modified equation taking into account the autocatalytic nature of the process as well as a limiting diffusional effect. Less accurate results were achieved for the anhydride-cured system.

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“…Samples (Ӎ0.1 g) were analyzed through end-group analysis and gel permeation chromatography (GPC). 15,16 The reactor apparatus consisted of a 100-cc round, Pyrex glass flask. A glass tube about 10 cm long was used to admit a stream of nitrogen to bubble through the molten resin.…”

Section: Thermoplastic Resinmentioning

confidence: 99%

Z‐protected glutamic acid‐based biodegradable thermoplastic and thermosetting polyesters: Synthesis and characterization

Tadros

Noureddini

Timm

1999

J. Appl. Polym. Sci.

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Biodegradable polymers were formed from N-benzyloxycarbonyl-L-glutamic acid with the comonomers ethylene glycol, diglycidyl ether of 1,4-butanediol, and diglycidyl ether of bisphenol A. The three polymers were a linear and a crosslinked heterochain polyester and a crosslinked polyester that contained aromatic units within its network chains. The thermoplastic resin and the soluble fractions for the thermosetting resins were characterized by gel permeation chromatography. Conversions for carboxylic acid were determined by titrations. A quality, 22,000 molecular weight thermoplastic resin was formed. The two thermosets were cured past their gel points. Gelation analysis revealed that the relative rate constants for the sequential oxirane/ acid and alcohol/acid reactions were distinct. With diglycidyl ether of 1,4-butanediol, the ratio of the respective rate constants was 3; with diglycidyl ether of bisphenol A, the ratio approached 200. The resins hydrolyzed to monomers in the presence of lipase, but in the presence of a mixed microbial culture, only the first two resins decayed to biomass, respiratory gases, and water. The third resin was inert during the period of observation.

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Fourier-Transform Infrared Analysis of a Linear, Anhydride-Cured Epoxy

Cited by 17 publications

References 8 publications

Cationic electron‐beam curing of a high‐functionality epoxy: effect of post‐curing on glass transition and conversion

Cationic electron‐beam curing of a high‐functionality epoxy: effect of post‐curing on glass transition and conversion

Tetrafunctional epoxy resins: Modeling the curing kinetics based on FTIR spectroscopy data

Z‐protected glutamic acid‐based biodegradable thermoplastic and thermosetting polyesters: Synthesis and characterization

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