Characterization of the interphase in an aluminium/epoxy joint by using controlled pressure scanning electron microscopy coupled with an energy dispersive X-ray spectrometer

Sperandio, Caroline; Arnoult, Claire; Laachachi, Abdelghani; Martino, Jean Di; Ruch, David

doi:10.1016/j.micron.2009.10.006

Cited by 7 publications

(3 citation statements)

References 24 publications

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“…the art, the epoxy component of the mixture did not seem to react with metallic surfaces. XPS data also pointed out that the dissolution process of the metal surface upon contact with the amine strongly depended on the (hydr)oxidation of the surface [24 28], leading to direct evidence of metal compound (its state is not evidenced) within the adhesive layer [15,19]. The interphase formation however depends on many other parameters, such as the surface treatment [14], the nature of the amine (hardener) and the curing cycle [11 13], the thickness of the coating and its environment (thin coatings versus thick adhesive joint) [16], or the viscosity of the pre polymer mixture [28,29].…”

Section: Mixing Calorimetrymentioning

confidence: 99%

Direct evidence of amine-metal reaction in epoxy systems: An in situ calorimetry study of the interphase formation

Fritah

Drouet²,

Thouron³

et al. 2020

Progress in Organic Coatings

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Epoxy resins are ubiquitously encountered in industrial applications as in adhesives and composites. The properties of epoxy-amine networlcs are directly impacted by the presence of metal (bydr-oxidized) surfaces, leading to a modificati on of their glass transition temperature T 8 • We propose here an innovative experimental approach, investigating the interaction of DET A amine and DGEBA epoxy with Al and Cu powder substrates (partially (hydr)oxidized). We explored for the first tiine the formation of the amine-metal interphase by in situ mixing calorimetry to evaluate the energetics of interaction. While DGEBA interacted only sl ightly with Al-based surface, the reaction with OETA was associated with a high exothermic enthalpy of reaction. The enhancing role of surfaoe hydroxylation was also evidenced by comparing boehmited Al to a simply oxidired counterpart. An even larger exothermic effect was measured with copper, which was related to the high chelating power of Cu compared to Al. The possible underlying mechanism of amine-metal interphase formation was discussed with a generalized schematic.

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Section: Mixing Calorimetrymentioning

confidence: 99%

Direct evidence of amine-metal reaction in epoxy systems: An in situ calorimetry study of the interphase formation

Fritah

Drouet²,

Thouron³

et al. 2020

Progress in Organic Coatings

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show abstract

“…In the presence of metal substrates, however, the amine precursor was found to react with metal surfaces [4][5][6][7][8][9][10][11][12][13][14][15], leading to significant modifications in terms of degree of curing and glass transition temperature, T g . These modifications can in turn alter the expected behavior of the polymerized networks as well as their mechanical/thermal resistance over time and other properties upon use [6][7][8].…”

Section: Introductionmentioning

confidence: 99%

“…These techniques allowed observing the formation of metal-amine surface complexes [17][18][19][20] as well as of chelates in solution [6][7][8][17][18][19]. This was associated with partial dissolution of the metal surface on contact with the amine [17][18][19][20][21], leading to the presence of the metal element in the adhesive layer [10,14]. A molecular dynamics (MD) study has been reported to investigate an epoxy-amine-copper system and its curing kinetics [22]; also, another MD study investigated the DGEBA/DETA polymerization at the vicinity of a generic surface [23].…”

Section: Introductionmentioning

confidence: 99%

Further insight on amine-metal reaction in epoxy systems

Drouet

Salles

Fritah

et al. 2021

Surfaces and Interfaces

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Among thermosetting polymers, epoxy resins are major components of adhesives, sealants, paints and composites. Polymerization is often achieved by reaction of epoxy monomers like DGEBA with amine hardeners such as DETA. Previous works showed that polyamines interact with metal (hydr/oxide) substrates leading to the formation of an interphase involving the chelation of surface metal ions. In this work, we further explored the interaction between DETA and aluminum (hydr)oxide, denoted Al, via a combined experimental and modeling approach. We inspected in depth by DSC the modifications of glass transition temperature T g and change in heat capacity ΔC p after curing, allowing us quantifying the impact of Al amount on DGEBA/DETA degree of cure α. A new parameter, the "percentage of inhibition of cure" denoted α, was defined reaching up to ~4 % in our experimental conditions. In parallel, in situ mixing calorimetry confirmed the exothermic character of DETA interaction with Al with various degrees of division. DFT calculations were carried out to examine DETA/Al 3+ chelates. Among plausible chelate configurations, one was associated with a lower conformational energy and shorted Al-N bond lengths, suggesting greater stability. Calculated and experimental Raman spectra were additionally investigated, allowing us to discuss further about the DETA/Al 3+ chelates at play.

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Influence of plasma surface treatment on bond strength behaviour of an adhesively bonded aluminium-epoxy system

Sperandio

Bardon²,

Laachachi³

et al. 2010

International Journal of Adhesion and Adhesives

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Characterization of the interphase in an aluminium/epoxy joint by using controlled pressure scanning electron microscopy coupled with an energy dispersive X-ray spectrometer

Cited by 7 publications

References 24 publications

Direct evidence of amine-metal reaction in epoxy systems: An in situ calorimetry study of the interphase formation

Direct evidence of amine-metal reaction in epoxy systems: An in situ calorimetry study of the interphase formation

Further insight on amine-metal reaction in epoxy systems

Influence of plasma surface treatment on bond strength behaviour of an adhesively bonded aluminium-epoxy system

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