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Development of Attenuated Total Reflection Based Compression Modulation Step-Scan Fourier Transform Infrared Spectroscopy and its Applications to Rheo-Spectral Characterizations of Polymer Films

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Abstract:

Dynamic compression modulation attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopic methods have been developed in this paper for characterizing polymer films. To obtain dynamic compression polarized ATR spectra, internal reflection element (IRE) secure assemblies made of tungsten carbide with very high hardness (Knoop hardness of > 1000 kgf/mm2) have been designed. These assemblies are mounted on the Harrick SeagullĀ® ATR attachment and measured by step-scan FT-IR spectroscopy. The effect of static compression, air gaps, and refractive index changes were examined. Experimental and simulated results showed that the effect of air gaps between the sample and IRE and refractive index changes of the sample and IRE are negligible at values larger than a static torque of 40 cN m and good signal-to-noise ratios (SNR) and reproducible data can be obtained. Uniaxially and biaxially drawn poly(ethylene terephthalate) films were measured by the presented method. Both bipolar and unipolar bands were observed in the dynamic in-phase ATR spectra, which can be associated with their micro-structural environmental changes. This technique shows promise in evaluating various polymer film materials, including biaxially oriented films, multilayer coated film surfaces, and molecular interactions between polymer–polymer and polymer–additives at the film surface.

Keywords: ATTENUATED TOTAL REFLECTION; COMPRESSION MODULATION; DYNAMIC SPECTROSCOPY; FOURIER TRANSFORM; INFRARED SPECTROSCOPY; INTERNAL REFLECTION; POLARIZED ATR; POLY(ETHYLENE TEREPHTHALATE); STEP-SCAN FT-IR SPECTROSCOPY

Document Type: Research Article

DOI: http://dx.doi.org/10.1366/0003702041655322

Affiliations: 1: Material Analysis Division, Material Technology R&D Laboratories, Konica Minolta Technology Center Inc., No.1 Sakura-machi, Hino-shi, Tokyo, 191-8511, Japan 2: Thermo Electron K. K., C-2F, 3-9 Moriya-cho, Kanagawa-ku, Yokohama, 221-0022, Japan 3: Thermo Electron Corporation, 5225 Verona Road, Madison, Wisconsin 53711-4495

Publication date: August 1, 2004

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