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Effects of Temperature and Dissolved Lithium Perchlorate on the Viscoelastic and Dynamic Properties of Poly(Ethylene Oxide), (Peo) Melts

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Effects of Temperature and Dissolved Lithium Perchlorate on the Viscoelastic and Dynamic Properties of Poly(Ethylene Oxide), (Peo) Melts UNLV Retrospective Theses & Dissertations 1-1-2005 Effects of temperature and dissolved lithium perchlorate on the viscoelastic and dynamic properties of poly(ethylene oxide), (Peo) melts Radoslav B Bogoslovov University of Nevada, Las Vegas Follow this and additional works at: https://digitalscholarship.unlv.edu/rtds Repository Citation Bogoslovov, Radoslav B, "Effects of temperature and dissolved lithium perchlorate on the viscoelastic and dynamic properties of poly(ethylene oxide), (Peo) melts" (2005). UNLV Retrospective Theses & Dissertations. 2627. http://dx.doi.org/10.25669/4bxr-m28d This Dissertation is protected by copyright and/or related rights. It has been brought to you by Digital Scholarship@UNLV with permission from the rights-holder(s). You are free to use this Dissertation in any way that is permitted by the copyright and related rights legislation that applies to your use. For other uses you need to obtain permission from the rights-holder(s) directly, unless additional rights are indicated by a Creative Commons license in the record and/or on the work itself. This Dissertation has been accepted for inclusion in UNLV Retrospective Theses & Dissertations by an authorized administrator of Digital Scholarship@UNLV. For more information, please contact [email protected]. EFFECTS OF TEMPERATURE AND DISSOLVED LiC104 ON THE VISCOELASTIC AND DYNAMIC PROPERTIES OF POLY(ETHYLENE OXIDE), (PEO) MELTS by Radoslav B. Bogoslovov Master of Science in Physics University of Nevada, Las Vegas, Las Vegas, Nevada 2003 Master of Science in Engineering Physics Sofia University, Sofia, Bulgaria 1996 A dissertation submitted in partial fulfillment of the requirements for the Doctor of Philosophy Degree in Physics Department of Physics College of Sciences Graduate College University of Nevada, Las Vegas December 2005 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. UMI Number: 3215869 INFORMATION TO USERS The quality of this reproduction is dependent upon the quality of the copy submitted. Broken or indistinct print, colored or poor quality illustrations and photographs, print bleed-through, substandard margins, and improper alignment can adversely affect reproduction. In the unlikely event that the author did not send a complete manuscript and there are missing pages, these will be noted. Also, if unauthorized copyright material had to be removed, a note will indicate the deletion. UMI UMI Microform 3215869 Copyright 2006 by ProQuest Information and Learning Company. All rights reserved. This microform edition is protected against unauthorized copying under Title 17, United States Code. ProQuest Information and Learning Company 300 North Zeeb Road P.O. Box 1346 Ann Arbor, Ml 48106-1346 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Dissertation Approval IINTV The Graduate College University of Nevada, Las Vegas November 15 20D5_ The Dissertation prepared by __________________ Radoslav Boykov Bogoslovov Entitled Effects of Temperature and Dissolved LICIO/, on the Viscoelastic and Dynamic Properties of Polyfethylene Oxide). (PEOl Melts______________ is approved in partial fulfillment of the requirements for the degree of Doctor of Philosophy In Physics Examination Committee Chair Dean of the Graduate College Examination Conpniitee Member Examination Committee Member Graduate College Faculty Representative PR/1017-52/1-00 11 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. ABSTRACT Effects of Temperature and Dissolved LIC104 on the Viscoelastic and Dynamic Properties of Poiy(ethylene Oxide), (PEO) Melts by Radoslav B. Bogoslovov Dr. James Selser, Examination Committee Chair Professor of Physics University of Nevada, Las Vegas Poly(ethylene oxide)/lithium perchlorate (PEO/LiC 104) complexes are widely studied as a prototype solid polymer electrolyte in rechargeable lithium-polymer batteries. Characterizing the structure and dynamics of the system in its molten state is important for understanding the role of the polymer environment in lithium ion transport and conductivity. A fiber-optic coupled Fabry-Perot interferometer is employed in the investigation of the electrolyte viscoelastic and dynamic properties, which are both related to the intrachain local mobility and therefore to ion diffusion. The properties of the system are studied as a function of composition, temperature, and fi-equency. Structural relaxation processes are observed both in the neat polymer melt and in the salt containing electrolytes. For the neat PEO-IK melt the relaxation is identified as Maxwell-Debye single-exponential relaxation (>0 = 1). The relaxation time follows Arrhenius temperature dependence with activation energy of the order of 10-11 kJ/mol. I l l Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Upon addition of salt, the character of the relaxation persists with y0 = l, while the characteristic relaxation time slows down and the activation energy increases slightly. The slowdown of the dynamics is more pronounced at lower temperatures. In addition, with increasing salt concentration the elastic modulus increases significantly making the system stiffer at all temperatures, while the maximum of the storage modulus is shifted to higher temperatures. These effects result in a decrease in polymer segmental mobility and consequently in reduction of lithium ion diffusivity, with increased salt concentration. A unique ^-dependent measurement is performed, allowing the investigation of the Brillouin frequency and linewidth as a function of fi-equency. It revealed a double-step relaxation in the electrolyte. The two relaxations are identified as secondary relaxations with Maxwell-Debye character (>0 = 1). The lower-frequency relaxation is stronger and has Arrhenius temperature behavior of the relaxation time. It is attributed to conformai fluctuations of the chain segments between transient crosslinks formed by the EO-Li^ complexation in the melt. The higher-ffequency relaxation is weaker, especially at higher temperatures and more difficult to resolve. It is possible it results fi-om librational motions or conformai rearrangements of the uncomplexed polymer dihedrals and seems to be strongly affected by the specifics of the local chain conformation and the EO-Li^ complexation in the melt. IV Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. TABLE OF CONTENTS ABSTRACT.............................................................................................................................iii LIST OF FIGURES................................................................................................................vii ACKNOWLEGMENTS.......................................................................................................viii CHAPTER 1 INTRODUCTION.......................................................................................... 1 CHAPTER 2 EXPERIMENTAL SETUP............................................................................ 9 2.1. Experiment layout ................................................................................. 9 2.2. The Fabry-Perot interferometer ........................................................ 13 2.3. Light collection: scattering geometry and alignment ...................... 20 CHAPTER 3 THEORY AND BACKGROUND .............................................................28 3.1. Viscoelasticity of liquids and the light-scattering spectra ..............28 3.2. Generalized hydrodynamics (Mountain’s theory) ...........................33 3.3. Structural relaxation in polymeric liquids (Wang’s theory) ...........36 3.4. Generalization of the Brillouin spectrum ......................................... 38 3.5. Relaxation strength ............................................................................46 CHAPTER 4 DYNAMIC AND THERMODYNAMIC PROPERTIES OF POLYMER ELECTROLYTES...................................................................50 4.1. Glass-forming liquids - dynamics and relaxation phenomena 50 4.2. Literature results for PEO and PEO/salt electrolytes ...................... 56 CHAPTER 5 EXPERIMENTAL.......................................................................................61 5.1. Samples and sample preparation .......................................................61 5.2. Data collection and analysis .............................................................. 62 5.3. Error analysis ..................................................................................... 68 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. CHAPTER 6 RESULTS AND DISCUSSION ..................................................................73 6.1. Results for PEO melt and PE 0 -melt/LiC104 - temperature dependence ................................................................................................. 73 6.2. Frequency dependence of cOg and F g ..............................................83 6.3. Discussion of the experimental results .............................................92 CHAPTER 7 SUMMARY AND CONCLUSIONS .......................................................... 98 REFERENCES .................................................................................................................... 104 VITA.....................................................................................................................................
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