Epoxy films spectroscopy

This paper reports the study of the aging behavior of ultra-thin epoxy films on PVD layers of Al, Au, and Cu under varying environmental conditions by FTIR external reflection absorption spectroscopy (ERAS), to reveal influences of interphase interactions on crosslinking and on chemical aging processes at moderate temperature. 

Transparent PVC plates were coated with a 70 pm thick film of an epoxy-acrylate resin containing 0.5 % of a benzotriazole UV absorber. They were first UV cured for one second and then exposed at 40°C to the low intensity radiations of a QUV accelerated weathering tester. The extent of the degradation was followed by Invisible spectroscopy, a very sensitive method that permits detec-... 

To evaluate the reactivity of model compounds III-VIII in photoinitiated cationic polymerization, we have employed real-time infrared spectroscopy (RTIR). Thin film samples of the model compounds containing 0.5 mol% of (4-n-octyloxyphenyl)phenyliodonium SbF - as a photoinitiator were irradiated in a FTIR spectrometer at a UV intensity of 20 mW/cm2. During irradiation, the decrease in the absorbance of the epoxy ether band at 860 cm-1 was monitored. 

Many investigations of the molecular structure of thin films formed by y-APS deposited onto inorganic substrates from aqueous solutions have been carried out. Ondrus and Boerio [2] used reflection-absorption infrared spectroscopy (RAIR) to determine the structure of y-APS films deposited on iron, 1100 aluminum, 2024 aluminum, and copper substrates from aqueous solutions at pH 10.4. They found that the as-formed films absorbed carbon dioxide and water vapor to form amine bicarbonate salts which were characterized by absorption bands near 1330, 1470, 1570, and 1640 cm-1. y-APS films had to be heated to temperatures above about 90°C in order to dissociate the bicarbonates, presumably to free amine, carbon dioxide, and water. Since the amine bicarbonates failed to react with epoxies, the strength of adhesive joints prepared... 

Abstract—The structure of films formed by a multicomponent silane primer applied to an aluminum adherend and the interactions of this primer with an amine-cured epoxy adhesive were studied using X-ray photoelectron spectroscopy, reflection-absorption infrared spectroscopy, and attenuated total reflectance infrared spectroscopy. The failure in joints prepared from primed adherends occurred extremely close to the adherend surface in a region that contained much interpenetrated primer and epoxy. IR spectra showed evidence of oxidation in the primer. Fracture occurred in a region of interpenetrated primer and adhesive with higher than normal crosslink density. The primer films have a stratified structure that is retained even after curing of the adhesive. 

Surface modification of LDPE film can also be brought about by chemical treatment [118] with an aqueous solution of ammoniacal ammonium persulphate in the presence of Ni+2 ions under variable reaction conditions. The investigation of treated surface showed the presence of polar groups (viz. carbonyl and hydroxyl) in the infrared (IR) spectroscopy, with characteristic bands at 1700, 1622 and 3450 cm-1. It is known that the persulphate ion attacks the double-bond-producing epoxy or diol group. However, the destructive oxidation of saturated hydrocarbons does not occur with persulphate alone, but requires the presence of the nickel (II) ion. The authors have proposed the following mechanism of chemical treatment ... 

Analysis of Cure. Infrared spectroscopy was utilized to examine film cure and the effect of stabilizers upon the cure of the epoxy acrylate. Pre-cured material has absorptions at 1635, 1410 and 810 cm-1 which clearly diminish after the resin is UV-irradiated (Figure 6). The 1635 cm-1 absorption can be assigned to the carbon-carbon stretch of an olefinic bond in conjugation with a carbonyl group the 1410 cm-1 can be assigned to the CH2 in-plane deformation of a vinylic group. The 810 cm-1 can also be assigned to some aspect of vinylic... 

J. Kanzow, F. Faupel, W. Egger, P. Sperr, G. Kogel, C. Wehlack, W. Possart, Depth-resolved analysis of the ageing behaviour of epoxy resin thin films by positron spectroscopy, Proc. oral pres., 7th European Adhesion Conference EURADH 2004, Ereiburg im Breisgau, September 5-9, 2004. 

Depth-Resolved Analysis of the Aging Behavior of Epoxy Thin Films by Positron Spectroscopy... 

In the polymer industry, packing material, laminates including multilayer films, pellets or molded products can be analyzed by NIR. Even polymer latex particles with up to 99 % water content may be analyzed. NIR provides information about reaction mechanisms, polymerization, crystallinity, orientation, water content and hydrogen bonding, even during the process of polymer manufacture. For example the disappearance of the double bonds in polyethylene and polypropylene can be monitored. In the NIR spectrum C=C bonds lead to a combination band at about 4740 cm and a first overtone at about 6170 cm NIR spectroscopy is applied to characterize ester-, nitrile-, or amide-based acrylic and methacrylic polymers. Other examples are the identification of polyvinylchloride, polyvinyl alcohol and polyvinyl acetates or the analysis of polymerization in epoxy and phenolic resins. 

FTIR spectroscopy was used for the analysis of ultrathin organic films on metals. FTIR in the reflection mode (IRRAS) was used to study the interaction of ultrathin films of dicyandiamide (hardener of most one-pack epoxy resins) with various substrates, model ones such as gold or zinc and industrial ones such as steel and zinc-coated steels. Pure zinc surfaces and, to a lesser extent, zinc-coated steels are shown to react with dicyandiamide after heating at 180 C, as evidenced by the frequency shift of the absorption band characteristic for nitrile groups. Some mechanically tested specimens are then analysed, after failure, by FTIR microspectrometry. The spectra obtained, corresponding to the fracture initiation zone which is about 100 micrometers in diameter, indicate the presence of an ultrathin layer of modified polymer still covering the substrate. 28 refs. 

The hardening of the boundary layer of epoxy and polyester compositions was studied by IR spectroscopy (of repeatedly disturbed total internal reflection—RDTIR) on a UR-20 spectrometer. A KRS-5 prism N =18, C = 45°) and a germanium prism N =14, C = 45°) were used for simulation of the substrate surface. The thickness of a polymer layer was 0.5-1 nm for the element made of germanium and 2-3 nm for KRS-5. Inhibition of polyester resin polymerization by atmospheric oxygen was eliminated by applying a polyethylene film to the surface of a system to be hardened. The thickness of the applied epoxy and polyester composition was up to 20-30 nm. To evaluate the glass-transition temperature and the polymer-solvent interaction parameter, we used reversed-phase gas chromatography. Basalt-1 and basalt-2 (see below) served as fillers and as a model substrate. The... 

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