Characterization of adhesive and coating constituents by time‐of‐flight secondary ion mass spectrometry (ToF‐SIMS). Part 1: Epoxy‐terminated diglycidyl polyethers of bisphenol‐A and propal‐2‐ol

Treverton, J. A.; Paul, A. J.; Vickerman, J. C.

doi:10.1002/sia.740200519

Cited by 23 publications

(18 citation statements)

References 21 publications

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“…The peaks for ToF‐SIMS data analysis were selected initially on the basis of reference libraries and previous assignments in the literature for DGEBA, DGEBF, IPD, Teta, and other amine molecules 21–24. Further peaks were assigned with the library and the exact mass calculator tool in Ionspec software (Ion‐TOF), including contaminant peaks, hydrocarbon peaks, and peaks likely to correspond to fragments of the resin/hardener that were not listed in the literature.…”

Section: Methodsmentioning

confidence: 99%

Investigation of the postcure reaction and surface energy of epoxy resins using time‐of‐flight secondary ion mass spectrometry and contact‐angle measurements

Awaja

Gilbert

Fox

et al. 2009

J of Applied Polymer Sci

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Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was used to investigate correlations between the molecular changes and postcuring reaction on the surface of a diglycidyl ether of bisphenol A and diglycidyl ether of bisphenol F based epoxy resin cured with two different amine-based hardeners. The aim of this work was to present a proof of concept that ToF-SIMS has the ability to provide information regarding the reaction steps, path, and mechanism for organic reactions in general and for epoxy resin curing and postcuring reactions in particular. Contact-angle measurements were taken for the cured and postcured epoxy resins to correlate changes in the surface energy with the molecular structure of the surface. Principal components analysis (PCA) of the ToF-SIMS positive spectra explained the variance in the molecular information, which was related to the resin curing and postcuring reactions with different hardeners and to the surface energy values. The first principal component captured information related to the chemical phenomena of the curing reaction path, branching, and network density based on changes in the relative ion density of the aliphatic hydrocarbon and the C 7 H 7 O þ positive ions. The second principal component captured information related to the difference in the surface energy, which was correlated to the difference in the relative intensity of the C x H y N z þ ions of the samples. PCA of the negative spectra provided insight into the extent of consumption of the hardener molecules in the curing and postcuring reactions of both systems based on the relative ion intensity of the nitrogen-containing negative ions and showed molecular correlations with the sample surface energy.

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Section: Methodsmentioning

confidence: 99%

Investigation of the postcure reaction and surface energy of epoxy resins using time‐of‐flight secondary ion mass spectrometry and contact‐angle measurements

Awaja

Gilbert

Fox

et al. 2009

J of Applied Polymer Sci

View full text Add to dashboard Cite

show abstract

“…The peaks for data analysis were selected initially based on reference libraries and previous assignments in the literature for DGEBA, DGEBF, and IPD molecules 20, 21, 24, 25. Further, peaks were assigned using the library and the exact mass calculator tool incorporated in the Ionspec software package (Ion‐TOF GmbH, Germany) to identify contaminant peaks, including the hydrocarbon peaks, and peaks that were likely to correspond to fragments of the resin/hardener not listed in the literature.…”

Section: Methodsmentioning

confidence: 99%

ToF‐SIMS investigation of epoxy resin curing reaction at different resin to hardener ratios

Awaja

Riessen

Kelly

et al. 2008

J of Applied Polymer Sci

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Time-of-flight secondary ion mass spectrometry (ToF-SIMS) and principal components analysis (PCA) were used to analyze diglycidyl ether of bisphenol A (DGEBA) and diglycidyl ether of bisphenol F (DGEBF) epoxy resin blend cured with isophorone diamine (IPD) hardener at different resin to hardener ratios. The aim was to establish correlations between the hardener concentration and the nature and progress of the crosslinking reaction. Insights into the cured resin structure revealed using ToF-SIMS are discussed. showed variance related to the completion of the curing reaction. Relative intensities of C x H y N z þ ions in the cured resin samples are indicative of the un-reacted and partially reacted hardener molecules, and are found to be proportional to the resin to hardener mixing ratio. The relative ion intensities of the aliphatic hydrocarbon ions are shown to relate to the cured resin crosslinking density.

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“…These observations are in agreement with previous work on commercial materials of this type. 10 Whilst these ions characterize the uncured adhesive, they may not be characteristic of the cured adhesive that will be present at the locus of failure of an adhesive joint. A comparison of the adhesive in its uncured and cured state was made by preparing specimens in which thin layers of polymer were smeared onto aluminium substrates; one specimen was then heated at 180°C for 30 min in air to simulate cure.…”

Section: Time-of-flight Sims Analysis Of Adhesive and Failure Surfacesmentioning

confidence: 98%

Adhesive bonding of hot-dipped galvanized steel: use of ToF-SIMS for forensic analysis of failed joints

Fitzpatrick¹,

Watts²

1999

Surf. Interface Anal.

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The interfacial chemistry of environmental failure of adhesively bonded hot‐dipped galvanized steel joints, fabricated using a structural epoxy in a lap configuration, has been investigated by time‐of‐flight (ToF) SIMS. The failed lap shear joints show areas of apparent interfacial failure but these regions are limited to thin strips at the ends of the overlap, termed initiation zones. An initial study highlighted the importance of small area surface analysis, using XPS, to demonstrate that electrochemical activity was responsible for the initial bond degradation and the formation of the initiation zones at the ends of the overlap. Despite having been employed successfully in a number of adhesion studies, XPS is unable to give the molecular level of specificity that is required for a full understanding of the mechanism of such an adhesively bonded system. A method has been developed, using ToF‐SIMS, for mapping the initiation zone of the adhesive joint. The images obtained support earlier evidence of electrochemical activity at the initiation zone showing the presence of cations (Mg2+), indicating that cathodic behaviour played a role in the formation of the initiation zone. The ToF‐SIMS line scans indicate residual polymer in the initiation zone, which supports the hypothesis of a dual effect of electrochemical behaviour and ingress of water being responsible for the formation of the initiation zone. This suggests weakening rather than the clear separation, prior to mechanical testing, observed in the case of classical cathodic delamination. The ToF‐SIMS images extend this model by showing corresponding cation‐rich and adhesive‐rich areas within the initiation zone, possibly demonstrating that the different processes dominate in different regions (a result of localized electrochemical activity), and enables cathode size to be estimated. Copyright © 1999 John Wiley & Sons, Ltd.

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Characterization of adhesive and coating constituents by time‐of‐flight secondary ion mass spectrometry (ToF‐SIMS). Part 1: Epoxy‐terminated diglycidyl polyethers of bisphenol‐A and propal‐2‐ol

Cited by 23 publications

References 21 publications

Investigation of the postcure reaction and surface energy of epoxy resins using time‐of‐flight secondary ion mass spectrometry and contact‐angle measurements

Investigation of the postcure reaction and surface energy of epoxy resins using time‐of‐flight secondary ion mass spectrometry and contact‐angle measurements

ToF‐SIMS investigation of epoxy resin curing reaction at different resin to hardener ratios

Adhesive bonding of hot-dipped galvanized steel: use of ToF-SIMS for forensic analysis of failed joints

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