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Physical and Electrochemical Investigations of Various PHYSICAL AND ELECTROCHEMICAL INVESTIGATIONS OF VARIOUS DINITRILE PLASTICIZERS IN HIGHLY CONDUCTIVE POLYMER ELECTROLYTE MEMBRANES FOR LITHIUM ION BATTERY APPLICATIONS A Thesis Presented to The Graduate Faculty of The University of Akron In Partial Fulfillment of the Requirements for the Degree Master of Science Chenrun Feng May, 2017 i PHYSICAL AND ELECTROCHEMICAL INVESTIGATIONS OF VARIOUS DINITRILE PLASTICIZERS IN HIGHLY CONDUCTIVE POLYMER ELECTROLYTE MEMBRANES FOR LITHIUM ION BATTERY APPLICATIONS Chenrun Feng Thesis Approved: Accepted: Advisor: Department Chair Dr. Thein Kyu Dr. Sadhan C. Jana Committee Member Dean of the College Dr. Xiong Gong Dr. Eric J. Amis Committee Member Dean of the Graduate School Dr. Zhenmeng Peng Dr. Chand Midha Date ii ABSTRACT To investigate physical and electrochemical properties of polymer electrolyte membranes (PEMs) containing various dinitriles such as succinonitrile (SCN), glutaronitrile (GLN) and adiponitrile (ADN), binary and ternary phase diagrams of poly(ethylene glycol) diacrylate (PEGDA), GLN and lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) blends were firstly established in this thesis. The binary phase diagram of PEGDA/GLN system was self-consistently solved based on the combined free energies of Flory-Huggins theory for liquid-liquid demixing and phase field theory for crystal solidification. Computed liquidus and solidus lines were compared with crystal melting temperatures of the binary pairs, obtained by differential scanning calorimetry (DSC) measurement. The binary phase diagram of LiTFSI/GLN system was drawn according to crystal melting temperatures of the binary pairs determined by DSC measurement. Then coexistence regions of each binary phase diagram were verified by polarized optical microscopy. Subsequently, the ternary phase diagram of PEGDA/GLN/LiTFSI at 25 oC were established. Guided by isotropic regions within ternary phase diagrams established in this thesis and previous studies, polymer electrolyte membranes (PEMs) plasticized by various dinitriles thus fabricated via photo-polymerization afforded transparent, homogeneous films. The ionic conductivity of these PEMs was determined by AC iii impendence spectrometer, which showed high ionic conductivity up to 10-3 S/cm at room temperature. Of particular interest is that GLN-PEM reveals the highest ion conductivity among the three PEMs tested. To analyze the electrochemical performance of PEMs used in lithium-ion batteries, SCN-PEM, GLN-PEM, and ADN-PEM were assembled into Li4Ti5O12/PEM/Li and LiFePO4/PEM/Li half-cells. The half-cell containing GLN-PEM exhibits the best charge-discharge cycling performance, which is consistent with the highest ionic conductivity of the GLN plasticized PEM. iv ACKNOWLEDGEMENTS First of all, I would like to give my sincere appreciation to my supervisor, Dr. Thein Kyu for his kind and patient indoctrination for my Master thesis. He not only teaches me as a master student, but also guides me how to think independently as a researcher. With his patient guidance, I have accomplished this thesis. I would also like to express my gratitude to my committee member: Dr. Gong Xiong and Dr. Zhenmeng Peng for their suggestions and comments. Secondly, I am very glad to study in the Department of Polymer Engineering at the University of Akron. Benefited from nice environment and facilities, I can focus on my researches and studies very well. My appreciation also goes to National Science Foundation (NSF) for providing financial support of this project(NSF-DMR 1502543). Thanks to all my group members, for their tolerance and understanding during my thesis. Without their helpful assistance, I cannot finish my thesis. Last but not least, I thank my parents in China for their love and support to me. v TABLE OF CONTENTS LIST OF TABLES ....................................................................................................... xx LIST OF FIGURES ....................................................................................................... x CHAPTER I. INTRODUCTION ...................................................................................................... 1 II. BACKGROUND ....................................................................................................... 3 2.1. Introduction of Batteries .................................................................................. 3 2.1.1. Basic concepts of batteries ..................................................................... 4 2.1.2. Battery operations .................................................................................. 4 2.2. Introduction to Lithium Ion Batteries. ............................................................. 8 2.2.1. Lithiumion battery operations ................................................................ 9 2.2.2. Basic concepts of lithiumion battery performance .............................. 12 2.2.3. The development of cathode in lithiumion batteries ............................ 15 2.2.4. The development of anode in lithiumion batteries .............................. 18 2.2.5. The development of electrolyte in lithium ion batteries ...................... 19 2.3. Polymer Electrolyte for Lithium Ion Batteries .............................................. 21 2.3.1. Development of polymer electrolyte ................................................... 22 2.3.2.Polymer electrolyte based on dinitrile solvents for high voltage applications .................................................................................................... 23 vi III. MATERIALS AND EXPERIMENTS ................................................................... 26 3.1. Materials ........................................................................................................ 26 3.1.1. Poly (ethylene glycol) diacrylate (PEGDA) ........................................ 26 3.1.2. Succinonitrile(SCN) ............................................................................. 26 3.1.3. Glutaronitrile (GLN) ............................................................................ 27 3.1.4. Adiponitrile (ADN) .............................................................................. 27 3.1.5. Lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) ........................ 27 3.1.6. 2,2-Dimethoxy-2-phenylacetophenone ................................................ 27 3.1.7. Materials used in thermal analysis of PEMs ........................................ 29 3.1.8. Materials used in battery preparation and electrochemical tests ......... 29 3.2 Experiment Techniques ................................................................................... 30 3.2.1. Polymer electrolyte preparation and membrane fabrication ................ 30 3.2.2. Thermal analysis of polymer electrolyte membranes .......................... 31 3.2.3.Electrochemical analysis of polymer electrolyte membranes ............... 32 IV. BINARY AND TERNARY PHASE DIAGRAMS OF VARIOUS DINITRILES PLASTICIZED POLYMER ELECTROLYTE SYSTEMS ......................................... 34 4.1. Introduction .................................................................................................... 34 4.2. Experimental Sections ................................................................................... 35 4.2.1. Solution Blending Method ................................................................... 35 4.2.2. Differential Scanning Calorimetry Analysis ........................................ 36 vii 4.2.3. Polarized optical microscopic characterization ................................... 37 4.3. Results and Discussion .................................................................................. 37 4.3.1. Binary phase diagram of PEGDA, GLN and LiTFSI blends............... 37 4.3.2. Ternary phase diagram ......................................................................... 42 4.4. Conclusions .................................................................................................... 43 V. IONIC CONDUCTIVITY OF UV-CROSSLINKED POLYMER ELECTROLYTE MEMBRANES CONTAINING VARIOUS PLASTICIZERS .................................... 44 5.1. Introduction .................................................................................................... 44 5.2. Experimental Sections ................................................................................... 45 5.2.1. Membrane fabrication and ionic conductivity measurement ............... 45 5.2.2. Thermal analysis for polymer electrolyte membranes (PEMs) ........... 46 5.3. Results and Discussion .................................................................................. 47 5.4. Conclusions .................................................................................................... 54 VI. EVALUATION OF ELECTROCHEMICAL STABILITY FOR PEMS IN LITHIUM ION BATTERY APPLICATIONS ............................................................. 56 6.1. Introduction .................................................................................................... 56 6.2. Experimental Sections ................................................................................... 57 6.3. Results and Discussion .................................................................................. 58 5.4 Conclusions ..................................................................................................... 68 VII. SUMMARY AND RECOMMENDATIONS ....................................................... 70 viii 7.1. Summary .......................................................................................................
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