Heat of Fusion, Crystallization Kinetics Analyses and Morphology of Poly[(ethylene)-co-(trimethylene terephthalate)]s

• Main Authors: Chuan-Liang Wang, 王傳樑
• Other Authors: Chen, Ming
• Format: Others
• Language: zh-TW
• Published: 2003
• Online Access: http://ndltd.ncl.edu.tw/handle/35562037169547062975

碩士 === 國立中山大學 === 材料科學研究所 === 91 === These developmental grade samples were supplied by the Union Chemical Laboratories of Industrial Technology Research Institute(ITRI). The compositions of a series of copolyesters were identified by C1-NMR and H1-NMR. The ethylene terephthalate(ET) units are 8.9、33.7、37.9% and trimethylene terephthalate(PT) units are 91.1、66.3、62.1% in the copolyesters with sample codes of C2、C3、C4. Differential scanning calorimeter(DSC) was used to study the isothermal crystallization kinetics and melting behaviors and Polarizing Microscope(PLM) was used to study the spherulite growth rates and spherulite patterns. The Hoffman-Weeks linear plot and M-X nonlinear plot gave an equilibrium meiting temperature(Tmo ) oC of C2、C3、C4 are (240.6、275.5)、(208.8、247.0)、(194.3、229.4). The growth rates (μm/s )of different samples in the different crystallination temperature(Tc) oC are C2(0.614~0.061, 180~207)、C3(0.112~0.021, 130~166)、C4(0.0213~0.003, 120~160). From the different equilibrium meiting temperature(Tmo ) and different T∞ = ( Tg-30, Tg-51.6 oC) to analysis the regime transition temperature (TⅡ→Ⅲ) in units of oC are C2(234.0、237.1、240.6、275.5，195.9±0.3, 196.2±0.4)、C3(193.1、198.9、208.8、247.0，147.5±0.2, 147.5±0.1)、C4(184.1、187.9、194.3、229.4，133.3±0.4, 133.6±0.2). Compare the results with the results that using the half-time of crystallization(t1/2) from DSC (C2(193.6 oC)、C3(147.3 oC)、C4(1140.4 oC)). It can find that C2 is over 2.3 and 2.6 oC and C3 is the same and C4 is under 6.8 and 7.1 oC. From the morphology of spherulite patterns and regime transition temperature (TⅡ→Ⅲ) oC, the results indicated that the change from the morphology is closed to regime transition temperature. Regular spherlites were exhibited at temperature(Tc) between 180 and 196 oC and banded spherulites were observed between 197 and 208 oC in the C2. The band spacing increase with increasing crystallization temperature. Regular spherlites were exhibited at temperature(Tc) between 130 and 147 oC and banded spherulites were observed between 148 and 172 oC in the C3. The band spacing increase with increasing crystallization temperature. Regular spherlites were exhibited at temperature(Tc) between 120 and 134 oC and banded spherulites were observed between 135 and 160 oC in the C4. The band spacing increase with increasing crystallization temperature. Combine the results of M-X plot and spherulites pattern and melting behaviors at a heating rate of 80 oC/min . It indicated that the regime transition temperature (TⅠ→Ⅱ) oC are in the range of crystallization temperature of C2、C3、C4 are (210~213、174~178、160~164 oC). The heat of fusion (△Hu) of C3 is 4.88±0.06 kcal/mol and B is 1.47±0.05 cal/c.c from the experimental. The heat of fusion(△Hu) of C4 is 2.56±0.22 kcal/mol and B is 4.45±0.36 cal/c.c from the experimental. Compare the results with PET(△Hu = 5.6 kcal/mol) and PTT(△Hu = 7.2 kcal/mol). It indicated that PTT > PET > C3 > C4.