P 45 ISSRNS 2012: Abstracts / Synchrotron Radiation in Natural Science Vol. 11, No 1 – 2 (2012)
CHARACTERIZATION OF POLYMER NANOCOMPOSITES BY MIKRO SR-FTIR SPECTROSCOPY
C. Paluszkiewicz1∗, W.M. Kwiatek2, and E. Stodolak1
1AGH — University of Science and Technology, Faculty of Materials Science and Ceramics, Al. Mickiewicza 30, 30-059 Krak´ow, Poland
2Institute of Nuclear Physics PAN, ul. Radzikowskiego 152, 31-342 Krak´ow, Poland
Keywords: bone defect, polymer-ceramic nanocomposites, SR-FTIR
∗e-mail : cpalusz@agh.edu.pl
Bone defect is one of the most frequent prob- lem in bone tissue reconstruction in which appli- cation of a biomaterial filling is necessary. It cre- ates a still rising demand of biomaterials for the bone surgery. Polymer-ceramic nanocomposites is a group of novel materials which properties such as strength, Young’s modulus, bioactivity and con- trolled degradation time make them suitable for fill- ing a bone defects.
The aim of this work was chemical characteri- zation of polymer nanocomposites. As a matrix for nanocomposite a natural polysaccharide — chitosan (CS) was used as well as a nanometric filler mont- morillonite (MMT). The applied biopolymer (CS) is a biocompatible and biodegradable material which mechanical properties are similar to the bone ones.
The ceramic nanofiller (MMT) was introduced in order to improve matching of mechanical properties of nanocomposite to a bone and to enable control of its degradation time.
The SR-FTIR (Synchrotron Radiation — Fourier Transform InfraRed) study was used to de- termine dispersion of MMT nanoparticles in the polymer matrix as well as chemical state of surface.
A correlation between the concentration of nanopar- ticles and physico-chemical properties (roughness and wettability) of nanocomposite surfaces was ob- served.
SR-FTIR measurements of the samples were car- ried out in the transmission mode. Spectra were measured at 4 cm−1 resolution in the region from 4000 cm−1to 900 cm−1using synchrotron radiation at Frascati, Italy. The SR-FTIR spectra were col- lected with Bruker system OPUS-65. Bruker spec- trometer was used with microscope (Hyperion-3000) equipped with MCT and FPA (64 × 64 pixel) detec- tors. The video camera enabled optical imaging of the investigated area. In case of FPA detector the analyzed area was 170 m × 170 m and thus the spatial resolution was about 3 µm.
Figure 1 : Optical and chemical images of CS/MMT foil analyzed in the region from 1208 cm−1 to 922 cm−1.
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The spectral data were baseline corrected. The band areas of the Si-O and COO- were calculated in the region from 1200 cm−1 to 900 cm−1 and from 1700 cm−1 to 1200 cm−1 respectively, which allow us to show chemical imaging of the samples.
As shown in Fig. 1 FTIR technique is a particu- larly efficient tool for the analysis of nanocomposite materials. This technique was used to determine dispersion of MMT nano-particles in polymer ma- trix (CS). We observed a correlation between the
concentration and distribution of nano-particles in nanocomposite samples. These results were con- firmed by SEM/EDS studies and PIXE measure- ments which have been done at AGH University of Science and Technology and at Institute of Nuclear Physics PAN respectively, both in Krak´ow, Poland.
Acknowledgments: This work was supported by The Polish Ministry of Science and Higher Education, grant No. N N507 370735.
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