Application of FTIR technique in study on polymer - ceramic nanocomposites
Czesław Paluszkiewicz, Ewa Stodolak, Piotr Jeleń
Quarterly No. 1, 2010 pages 64-69
DOI:
keywords: nanocomposite, nanoparticles, FTIR spectroscopy
abstract The nanocomposites from renewable sources are considered to be a group of perspective materials. The main advantage of the nanocomposite materials based on natural biopolymers such as polysaccharides e.g. alginates or chitosane is their simple utilization and safe products of degradation. The additional advantage of nanocomposites based on chitosane and montmorylonite (MMT) is availability and low cost of the component materials. However, successful preparation of the nanocomposites still encounters many problems mainly related to proper dispersion of nano-fillers. High surface area, and high free surface energy are the cause of agglomeration of the nanoparticles, which then lose ability to create first-, and second-order interactions with a polymer matrix. In the result, the nano-filler becomes submicron or micron phase which because of its low fraction, not exceeding 10% (volume or weight), act as a defect weakening the polymer matrix. The situation between nanofillier and polymer matrix can be observed used the most popular measurement technique: thermal analyses (DSC, TG, DTA), microscopic methods such as: AFM, SEM, TEM, and spectroscopic methods; FTIR, Raman, XPS. In order to follow the structural changes in the nanocomposites materials a variety of investigative methods suitable for verification of complex phenomena taking place in the materials is utilized. The spectroscopy techniques FTIR can be relatively easily applied both to powder and foil samples on nanocomposite materials. Obtained result can be averaged in the case of transmission techniques or it may describe an area of a sample in the case of ATR technique. FTIR techniques enables better observation and interpretation of subtle changes taking place in the polymer matrix than XRD and SEM/EDS methods, especially when the investigated material is a nanocomposite polymer foil. In the work efforts of production of a series of nanocomposites based on natural chitosane and nano-clay (MMT) were taken. The nanocomposites materials was obtaining by casting method. Mechanical and ultrasound stirrer was used to better homogenization between nanoclay particles and biopolymer matrix. Two types of MMT (MMT-K5 and MMT-K10) with different particle size (DLS) and specific surface area (BET) were used. The nanoparticles morphology was examined with transmission electron microscopy (TEM). In each nanocomposite, the nano-filler amount was 3% wt. Dispersion of the nano-filler within the polymer matrix was investigated with the use of FTIR method (transmission mode, FTIR microscopy). FTIR measurements of the samples were carried out on the transmission mode in the region from 400 to 4000 cm–1 and ATR method in the region from 700 to 4000 cm–1. For the transmission mode powder samples were prepared in the form of potassium bromide (KBr), whereas the foils of the polymer samples were placed directly in the spectrometer. In the ATR method which allow to analyze the deep of penetration of the samples two different crystals were used: german and diament. In this way were observed how the clay (MMT-K5 or MMT-K10) influenced on the chemical structure of biopolymer chain.