Studies on the nanocellulose filled polylactide based biocomposites

Date

2024-3

Author

Sarı, Burcu

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In the first part of this dissertation, the main purpose of the first step was to obtain and characterize cellulose nanocrystal (CNC) particles by applying sulfuric acid hydrolysis method to the starting material of microcrystalline cellulose (MCC) fibrils. After obtaining CNC particles via acid hydrolysis procedure, various analyses conducted revealed that average size of round shaped CNC particles was 38 nm with -30.4 mV Zeta potential value. They have monoclinic Cellulose-I crystal structure with Crystallinity Index of 80.6% and Crystallite Size of 3.39 nm. Their maximum thermal degradation temperature was 307ºC with 23 wt% residue at 800ºC. In the second step, the main aim was to investigate contribution of these obtained CNC particles when they were used as nano-reinforcement in polylactide (PLA) matrix biocomposites produced by industrially compatible melt mixing and shaping techniques. Mechanical tests revealed that when only 1 wt% CNC particles were incorporated into PLA matrix, increases in flexural strength and modulus were 29% and 51%, respectively, while increases in fracture toughness values were as much as 105%. In the second part of this dissertation, the main purpose was to use “green materials” approach by investigating effects of only 1 wt% Cellulose Nanofibrils (CNF) on the strengthening and toughening of neat and blended polylactide (PLA) biopolymer matrix. For this purpose, first of all, effects of CNF were investigated in PLA/CNF biocomposite specimens. After blending of PLA with 10 phr bio-based thermoplastic polyester (b-TPE) elastomer, effects of CNF were investigated also for this PLA/b-TPE/CNF ternary biocomposite specimens. Mechanical tests revealed that due to the efficient strengthening and toughening mechanisms, CNF increased flexural strength of PLA by 33%, while b-TPE increased fracture toughness of PLA by 104%. When CNF and b-TPE were incorporated together, synergism in the strength and toughness values occurred. All bioblend and biocomposite specimens were produced by using the same “melt mixing” technique in a laboratory size twin-screw extruder, and their test specimens were shaped by conventional “compression molding”. Since shaping by “3D-printing” is frequently used in the biomedical sectors, another distinctive aim of this part was to reveal whether there were any differences in the strength and toughness values of specimens after their 3D-printing. It was observed that due to the “textured” structure of 3D-printed specimens, their flexural strength values were approximately 20% lower, while fracture toughness values were approximately 20% higher. In the third part of this dissertation, the main purpose was to investigate effects of various electrospinning parameters on the morphology and diameter of cellulose nanofibril (CNF) filled polylactide (PLA) nanofibers. For this purpose, first of all, effects of three important electrospinning parameters; polymer “Solution Concentration”, “Solution Feeding Rate” and “Collector Distance” to feeding tip were studied. Then, effects of using higher amount of CNF, effects of using cellulose nanocrystal (CNC) particles, and effects of adding potassium chloride salt were also investigated. It was observed that when optimum electrospinning parameters were determined, then it was possible to obtain almost “bead-free” morphology and “finest” average diameter of 232 nm for PLA/CNF electrospun fibers. Increasing values of Feeding Rate and Collector Distance parameters resulted in bead formation and thicker diameters. On the other hand, increasing CNF amount, using CNC particles and adding KCl salt, all resulted in further decreases in the diameter down to 152 nm; mainly due to increased charge density of the polymer solution. Moreover, in vitro degradation analysis of all types of electrospun nanofiber mats in a simulated body fluid revealed that increasing the immersion period increased their degradation rate in terms of “% weight loss”. It was also observed that mats with fine diameter fibers had higher degradation rate.

Subject Keywords

Cellulose Nanocrystals, Cellulose Nanofibrils, Polylactide, Sulfuric Acid Hydrolysis, 3D-Printing, Electrospinning

URI

https://hdl.handle.net/11511/109109

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Graduate School of Natural and Applied Sciences, Thesis