Sukanda Vaewbundit. Synthesis of chitosan/iron oxide nanocomposites by soft solution processing for medical application. Doctoral Degree(Applied Chemistry). King Mongkut's Institute of Technology Ladkrabang. Central Library. : King Mongkut's Institute of Technology Ladkrabang, 2022.
Synthesis of chitosan/iron oxide nanocomposites by soft solution processing for medical application
Abstract:
This research studied on synthesis of chitosan/iron oxide nanocomposites (CHI/IO) using two methods, i.e. the in-situ and adsorption systems, incorporating with the aqueous based systems at low reaction temperatures. In the in-situ synthesis, a chitosan solution was mixed with a mixture solution of iron(II) and iron(III), namely ammonium ferrous sulphate hexahydrate ((NH4)2S04FeS04.6H20) and ferric chloride hexahydrate (FeCl3.6H20), with an initial Fe2+: Fe3+ concentration of 0.625 : 1.25 M. After that, a solution of sodium tripolyphosphate (TPP) was added to the previous mixtures to crosslink chitosan, resulting in the chitosan network (cc) and the incorporation of Fe2+ and Fe3+ ions into the cc structure (CHI/Fe2+Fe3+). The TPP concentration was varied at 0.2, 0.3, 0.4, 0.5 and 0.6 %w/v. The CHI/Fe2+Fe3+ samples were then reacted in NaOH solution by hydrothermal and refluxing methods at 75, 100 and 125°c for 90 min, resulting in the CHI/IO nanocomposites. In the adsorption synthesis, the cc precipitates were soaked in the mixture solution of Fe2+Fe3+ with Fe2+: Fe3+ concentration of 0.625 : 1.25 M, resulting in the adsorption of Fe2+ and Fe3+ ions into the cc templates (CC/Fe2+Fe3+). The CC/Fe2+Fe3+ samples were reacted in NaOH solution by hydrothermal and refluxing methods at 100°c, yielding the CHI/IO nanocomposites. When the CHI/IO nanocomposites prepared using both synthesis systems were analyzed by various techniques, it was discovered that CHI/IO nanocomposites synthesized at temperatures higher than 100°c were primarily composed of magnetite-maghemite nanocrystals embedded in the cc network. The iron oxide nanocrystals prepared by in-situ method had an irregular spherical shape with sizes ranging from 3.9 to 4.3 nm, and the iron oxide fraction in the nanocomposites was in the range of 70-75%. While the iron oxide nanocrystals prepared by adsorption synthesis were quadrilateral in shape, with sizes ranging from 10.3 to 13.5 nm, and the iron oxide fractions in the nanocomposites ranging from 28 to 35%. The increase of initial TPP concentration promoted the formation of non-uniform cc network. The iron oxide nanocrystals with board particle size distribution were obtained in the nanocomposites when the non-uniform cc template was used as a template for crystal formation. The resultant CHI/IO nanocomposites exhibited superparamagnetic behavior, with maximum magnetization (Mmax) values ranging from 8.6 to 15.2 emu/g. The nanocomposites were found to be extremely safe, with cell viability in the range from 57-96% after exposure to the CHI/IO nanocomposites, indicating their suitability for medical applications, particularly the hybrid material for hyperthermia applications
King Mongkut's Institute of Technology Ladkrabang. Central Library