Transcription of THE CRYSTALLIZATION BEHAVIOUR OF ISOTACTIC …
1 I THE CRYSTALLIZATION BEHAVIOUR OF ISOTACTIC polybutene -1 A THESIS SUBMITTED TO THE DEPARTMENT OF CHEMISTRY AND THE INSTITUTE OF ENGINEERING AND SCIENCE OF BILKENT UNIVERSITY IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE DEGREE OF MASTER OF SCIENCE BY HACI BAYRAM ERDEM AUGUST 2002 ii I certify that I read this thesis and that in my opinion it is fully adequate, in scope and in quality, as a thesis for the degree of Master of Science. _____ Asst.
2 Prof. Dr. G rhan Kalay (Supervisor) I certify that I read this thesis and that in my opinion it is fully adequate, in scope and in quality, as a thesis for the degree of Master of Science. _____ Prof. Dr. efik S zer I certify that I read this thesis and that in my opinion it is fully adequate, in scope and in quality, as a thesis for the degree of Master of Science. _____ Assoc.
3 Prof. Dr. C. Hakan G r Approved for Institute of Engineering and Science. _____ Prof. Dr. Mehmet Baray Director of Institute of Engineering and Science iiiABSTRACT THE CRYSTALLIZATION BEHAVIOUR OF ISOTACTIC polybutene -1 Haci Bayram Erdem in Chemistry Supervisor: Assist. Prof. Dr. G rhan Kalay August 2002 The CRYSTALLIZATION BEHAVIOUR of different commercial grades of ISOTACTIC polybutene -1 was investigated and an experimental set-up was designed for this research study.
4 The experimental set-up constructed provides both fast-cooling of the sample and the recording of the growth of spherulites as a real time movie. The radial growth rate of the spherulites were observed to be higher for the grades with higher molecular weights. The results were found to fit to the Lauritzenn-Hoffman CRYSTALLIZATION theory, and this theory is used to calculate the lateral surface free energy, , and fold surface free energy, e. The lateral surface free energy was found to be erg/cm2 for all the grades investigated.
5 The fold surface free energy calculated to be between to erg/cm2. The fold surface free energies and the CRYSTALLIZATION rates do not exhibit any dependence on the molecular weight of the polymer. The polymer containing nucleating agents has the highest CRYSTALLIZATION rate. It was observed that the likelihood of deviation from spherical shape is greater for the grades with lower molecular weights. Key-words : polybutene -1, Lauritzen-Hoffman theory, spherulite growth rate, nucleating agent, CRYSTALLIZATION rate, polymer CRYSTALLIZATION iv ZET ZOTAKT K POL B TEN-1 N KR STALLE ME DAVRANI I Hac Bayram Erdem Kimya Y ksek Lisans Tez Y neticisi: Assist.
6 Prof. Dr. G rhan Kalay A ustos 2002 Polibuten-1 in d rt farkl ticari t r n n kristalle me davran incelendi ve bu inceleme i in bir deney d zene i haz rland . Haz rlanan deney d zene i, ayn zamanda numunelerin h zl -so utulmas n ve k resel kristal yap lar n b y mesini ger ek zamanl bir film olarak kaydedilmesini sa lad . Yar apsal b y me h zlar n n, b y k molek l a rl kl s n flar i in daha b y k oldu u g zlemlendi. Bulunan sonu lar n Lauritzen-Hoffman kristalle me teorisine uygunlu u g sterildi ve bu teori yanal y zey serbest enerjisi, , ile katlanma y zeyi serbest enerjisi, e, de erlerini hesaplamada kullan ld.
7 Yanal y zey serbest enerjisi n n b t n incelenen t rler i in de eri 10,4 erg/cm2 olarak bulundu. Katlanma y zeyi serbest enerjisi de erlerinin 15,5 erg/cm2 ile 17,4 erg/cm2 aras nda de i ti i hesapland . Katlanma y zeyi serbest enerjisi, e, ile kristalle me h z n n molek ler a rl a ba l olmad g r ld . ekirdekle me katk maddeleri i eren t r n kristalle me h z n n incelenen t rler i inde en y ksek oldu u bulundu. K resel yap dan sapma olas l n n, daha k k molek l a rl kl s n flar i in daha y ksek oldu u g zlendi.
8 Anahtar Kelimeler : polib ten-1, Lauritzen-Hoffman teorisi, yar apsal b y me h z , ekirdekle me katk maddesi, kristalle me h z , polimer kristalle mesi v ACKNOWLEDGEMENT I warmly thank Asst. Prof. Dr. Gurhan Kalay, for his great help and supervision throughout my studies. vi TABLE OF CONTENTS SIGNATURE TABLE OF LIST OF LIST OF LIST OF MOVIES INCLUDED IN THE CHAPTER-1. CHAPTER-2. LITERATURE Introduction ..3 Synthesis of ISOTACTIC Properties of Monomer.
9 3 Synthesis of Polymorphmism of ISOTACTIC Form-II to Form-1 Crystal The Rate of Transformation from Form-II to Polymer CRYSTALLIZATION During Strain Induced from Solutions under CRYSTALLIZATION from Melts under CRYSTALLIZATION under Quiescent from Quiescent from Quiescent vii Fringed Micelle Kinetics of Lateral Crystal Lauritzen-Hoffman secondary Nucleation Regimes of Spherulite Growth rate vs
10 Bulk CRYSTALLIZATION Kinetics and Avrami Supermolecular Structure of iPB-1 ..32 Applications of ISOTACTIC CHAPTER-3. EXPERIMENTAL PROCEDURE AND THE DESCRIPTION OF THE CRYSTALLIZATION DSC FT-IR Spherulite Growth Rate CRYSTALLIZATION Spherulite Growth Rate (SGR) The Measurement of Spherulite Growth Preperation of the L-H Plots and Calculation of the Regime Calculation of the Overall CRYSTALLIZATION and Avrami CHAPTER-4.
