The Influence Of Charged Species On The Phase Behavior Self Assembly And Electrochemical Performance Of Block Copolymer Electrolytes
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The Influence Of Charged Species On The Phase Behavior Self Assembly And Electrochemical Performance Of Block Copolymer Electrolytes
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Author : Jacob Lloyd Thelen
language : en
Publisher:
Release Date : 2016
The Influence Of Charged Species On The Phase Behavior Self Assembly And Electrochemical Performance Of Block Copolymer Electrolytes written by Jacob Lloyd Thelen and has been published by this book supported file pdf, txt, epub, kindle and other format this book has been release on 2016 with categories.
One of the major barriers to expanding the capacity of large-scale electrochemical energy storage within batteries is the threat of a catastrophic failure. Catastrophic battery pack failure can be initiated by a defect within a single battery cell. If the failure of a defective battery cell is not contained, the damage can spread and subsequently compromise the integrity of the entire battery back, as well as the safety of those in its surroundings. Replacing the volatile, flammable liquid electrolyte components found in most current lithium ion batteries with a solid polymer electrolyte (SPE) would significantly improve the cell-level safety of batteries; however, poor ionic conductivity and restricted operating temperatures compared to liquid electrolytes have plagued the practical application of SPEs. Rather than competing with the performance of liquid electrolytes directly, our approach to developing SPEs relies on increasing electrolyte functionality through the use of block copolymer architectures. Block copolymers, wherein two or more chemically dissimilar polymer chains are covalently bound, have a propensity to microphase separate into nanoscale domains that have physical properties similar to those of each of the different polymer chains. For instance, the block copolymer, polystyrene-b-poly(ethylene oxide) (SEO), has often been employed as a solid polymer electrolyte because the nanoscale domains of polystyrene (PS) can provide mechanical reinforcement, while the poly(ethylene oxide) microphases can solvate and conduct lithium ions. Block copolymer electrolytes (BCEs) formed from SEO/salt mixtures result in a material with the bulk mechanical properties of a solid, but with the ion conducting properties of a viscoelastic fluid. The efficacy SEO-based BCEs has been demonstrated; the enhanced mechanical functionality provided by the PS domains resist the propagation of dendritic lithium structures during battery operation, thus enabling the use of a lithium metal anode. The increase in the specific energy of a battery upon replacing a graphite anode with lithium metal can offset the losses in performance due to the poor ion conduction of SPEs. However, BCEs that enable the use of a lithium anode and have improved performance would represent a major breakthrough for the development of high capacity batteries. The electrochemical performance of BCEs has a complex relationship with the nature of the microphase separated domains, which is not well-understood. The objective of this dissertation is to provide fundamental insight into the nature of microphase separation and self-assembly of block copolymer electrolytes. Specifically, I will focus on how the ion-polymer interactions within a diverse set of BCEs dictate nanostructure. Combining such insight with knowledge of how nanostructure influences ion motion will enable the rational design of new BCEs with enhanced performance and functionality. In order to facilitate the study of BCE nanostructure, synchrotron-based X-ray scattering techniques were used to study samples over a wide range of length-scales (i.e., from Angstroms to hundreds of nanometers) under conditions relevant to the battery environment. The development of the experimental aspects of the X-ray scattering techniques, as well as an improved treatment of scattering data, played a pivotal role in the success of this work. The dissemination of those developments will be the focus of the first section. The thermodynamic impact of adding salt to a neutral diblock copolymer was studied in a model BCE composed of a low molecular weight SEO diblock copolymer mixed with lithium bis(trifluoromethanesulfonyl)imide (LiTFSI), a common salt used in lithium batteries. In neutral block copolymers (BCPs), self-assembly is a thermodynamically driven process governed by a balance between unfavorable monomer contacts (i.e., the enthalpic contribution) and the entropy of mixing. When the enthalpic and entropic contributions to free energy are similar in magnitude, a block copolymer can undergo a thermally reversible phase transition from an ordered to a disordered nanostructure (i.e., the order-to-disorder transition (ODT). We used temperature-dependent small angle X-ray scattering (SAXS) to observe this transition in the model SEO/LiTFSI system. Unlike neutral BCPs, which to a first approximation are single component systems, the SEO/LiTFSI system demonstrated the thermodynamically stable coexistence phases of ordered lamellae and disordered polymer over a finite temperature window. Analysis of the lamellar domains revealed an increase in salt concentration during the ODT, indicating local salt partitioning due to the presence of nanostructure. While the Gibbs phase rule predicts this behavior, this was the first result demonstrating a direct connection between ion-polymer interactions and block copolymer nanostructure. We found evidence of salt redistribution in BCEs wherein self-assembly has been kinetically arrested. Through the structural analysis of BCEs formed from a high molecular weight SEO sample over a wide range of LiTFSI concentrations, it was revealed that in some cases, coexisting nanostructures were stable. While it is likely that the stability of these nanostructures was kinetic in nature, the relationship between nanostructure and salt partitioning revealed previously indicates that the salt could redistribute between the nanostructures to achieve the lowest energetic state. Unusual trends in the ionic conductivity with respect to salt concentration support this hypothesis. In some cases, high salt concentrations lead to significant improvements in ionic conductivity, representing a strong departure from the behavior of standard SPEs, and a possible route to improving the performance of BCEs. The performance of BCEs can also be improved by chemically functionalizing one of the polymer blocks by covalently attaching the salt anion. Since the cation is the only mobile species, these materials are coined single-ion conducting block copolymers. Single ion conduction can improve the efficiency of battery operation. In order for cation motion to occur in single-ion conducting block copolymers, it must dissociate from the backbone of the anion-containing polymer block. Through the structural and electrochemical characterization of poly(ethylene oxide)-b-poly[(styrene-4-sulfonyltrifluoromethylsulfonyl)imide] (PEO-P(STFSI))-based single-ion conductors, we found that ion dissociation significantly influences nanostructure: when a large amount of ions are dissociated, the polymer blocks tend to mix, thus precluding microphase separation and the formation of nanostructure. This direct coupling of ion dissociation (and hence conduction) and nanostructure has interesting implications for BCE performance. For instance, without discreet microphases, the single-ion conducting polymers cannot provide the enhanced mechanical properties like those obtained in SEO/LiTFSI electrolytes. Future development in single-ion conducting block copolymers should investigate polymer architectures where a third polymer block, such as PS, facilitates microphase separation and improved mechanical properties. Additional analysis of the single-ion conducting block copolymers revealed that ion dissociation from the charge-containing backbone (P(STFSI)) could also influence the crystallization of the neutral polymer block (PEO). Interestingly, ion dissociation did not disrupt PEO crystallization by directly interfering with the PEO chains, rather the homogeneity of the polymer melt prior to PEO crystallization led to differences in crystallization behavior. In the cases where ion dissociation lead to significant mixing of the polymer block, PEO crystallites grew unimpeded and formed well-ordered lamellar structures. When ion dissociation did not occur, fluctuations in concentration due to the demixing of PEO and P(STFSI) interrupted the growth of PEO crystallites, slowing the crystallization process and leading to less-ordered nanostructures. The final study in this work highlights the capability of utilizing in situ electrochemical characterization techniques while monitoring polymer microstructure using synchrotron X-ray scattering. We studied the electrochemical oxidation (doping) of poly(3-hexylthiophene) (P3HT) in a block copolymer of poly(3-hexylthiophene)-b-poly(ethylene oxide) (P3HT-PEO) mixed with LiTFSI. During the doping process, we monitored the charge mobility electrochemically and the crystalline structure of P3HT using wide angle X-ray scattering (WAXS). Combining the structural analysis with the transport measurements in situ allowed the observation of a clear correlation between doping-induced changes in the P3HT crystal lattice and improvements in charge mobility. Since the doping-induced structural changes involve the intercalation of a salt anion into the P3HT crystal lattice, tuning the nature of the anion present during electrochemical oxidation might provide a new route to improving hole mobility in P3HT.
Ionic Solvation
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Author : Gennadiĭ Alekseevich Krestov
language : en
Publisher: Prentice Hall
Release Date : 1994
Ionic Solvation written by Gennadiĭ Alekseevich Krestov and has been published by Prentice Hall this book supported file pdf, txt, epub, kindle and other format this book has been release on 1994 with Science categories.
This comprehensive, widely-read anthology presents cogent and provocativearticles from differing political perspectives on major issues in post-World WarII America. The fourth edition is considerably expanded to include newselections on the AIDS epidemic, gay rights, the women's movement, and theClinton-Gore administration. In addition to articles by leading historians theeditors have chosen first-person accounts by participants in each of the issuesunder discussion, from Martin Luther King, Jr.'s "Letter from the BirminghamJail" to Al Gore's speech on environmentalism. With lively introductions to eachsection providing a context for the articles, this book helps students makesense of the tumultuous world of our time.
Solution Self Assembly Of Block Copolymers
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Author : Nitin Sharma
language : en
Publisher:
Release Date : 2011
Solution Self Assembly Of Block Copolymers written by Nitin Sharma and has been published by this book supported file pdf, txt, epub, kindle and other format this book has been release on 2011 with categories.
Characterization Of Self Assembly And Charge Transport In Model Polymer Electrolyte Membranes
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Author : Keith Morgan Beers
language : en
Publisher:
Release Date : 2012
Characterization Of Self Assembly And Charge Transport In Model Polymer Electrolyte Membranes written by Keith Morgan Beers and has been published by this book supported file pdf, txt, epub, kindle and other format this book has been release on 2012 with categories.
There is broad interest in creating polymer electrolyte membranes (PEMs) that have a charged hydrophilic nanophase, where the size and geometry of the phase can be precisely controlled. The applications for such materials range from portable power generating devices to water purification. There is a need to better characterize the self-assembly, thermodynamics, and performance of both current and future PEMs. To this end a series of chapters is presented, that explore the development of techniques, equipment, methods, and materials to enable further progress in the field. The interaction of PEMs with external ionic solutions can be used to determine fundamental thermodynamic properties of the ions that reside within the membrane itself. Traditional techniques used to probe ions in PEMs, such as conductivity, can be greatly enhanced by knowing the number of dissociated ions and their activity coefficients. A technique is presented that provides one of the first methods able to quantify such properties in PEMs. The ionic species in PEMs are believed to reside in nanoscale ionic aggregates. Only recently have researchers begun to focus on the properties of this aggregation in regards to PEM performance. A summary of this phenomenon, as well as speculation on its effect on transport and thermodynamic properties is presented. In addition, evidence that suggests block copolymers offer a method of inhibiting aggregate formation is discussed. Characterization of PEM morphology is critical to properly understand structure-function relationships. Due to a lack of proper equipment, the morphological characterization of PEMs has been mostly limited to the dry state. The design and operation of a novel sample stage, used to simultaneously measure morphology and conductivity in humid air as a function of temperature and relative humidity is presented. Precise control over humidity and accurate determination of morphology and conductivity over a wide range of temperatures is shown. At present there is an incomplete understanding of the thermodynamic interaction between PEMs and water of varying activity. The morphology, water uptake, and proton conductivity of sulfonated polystyrene-block-polyethylene (PSS-PE) was studied under controlled relative humidity (RH) and in liquid water. Extrapolation of the domain size, water uptake, and conductivity in humid vapor to RH = 100% allowed for an accurate comparison between the properties of PSS-PE hydrated in saturated vapor and in liquid water. Absent from this system was Schroeder's Paradox, which expects the properties in saturated water vapor to be less than those obtained in liquid water. Polymers that are semi-crystalline are ubiquitous as commercial polymers because of their mechanical properties. Little is known about the effects of polymer crystallization on PEM structure and performance. The model system, PSS-PE, was synthesized at a variety of molecular weights to probe how crystallization affects performance for a variety of conducting domain sizes. Results are shown that indicate crystallization disrupts the self-assembly of low molecular weight PEMs, resulting in poor water uptake and proton conductivity in small domains. Increasing domain size results in less morphological disruption, leading to an improvement in performance at larger domain sizes. This work improves upon the ability of researchers to characterize and understand the relationship between the structure and performance of PEMs. The findings presented herein provide further understanding toward the goal of rational design of nanostructured membranes that show improved conductivity in a variety of conditions.
Dissertation Abstracts International
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Author :
language : en
Publisher:
Release Date : 2001
Dissertation Abstracts International written by and has been published by this book supported file pdf, txt, epub, kindle and other format this book has been release on 2001 with Dissertations, Academic categories.
Book Of Abstracts
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Author :
language : en
Publisher:
Release Date : 2000
Book Of Abstracts written by and has been published by this book supported file pdf, txt, epub, kindle and other format this book has been release on 2000 with Chemistry categories.
Thermodynamics And Ionic Conductivity Of Block Copolymer Electrolytes
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Author : Nisita Sidra Wanakule
language : en
Publisher:
Release Date : 2010
Thermodynamics And Ionic Conductivity Of Block Copolymer Electrolytes written by Nisita Sidra Wanakule and has been published by this book supported file pdf, txt, epub, kindle and other format this book has been release on 2010 with categories.
Solid electrolytes have been a long-standing goal of the battery industry since they have been considered safer than flammable liquid electrolytes and are capable of producing batteries with higher energy densities. The latter can be achieved by using a lithium metal anode, which is unstable against liquid electrolytes. Past attempts at polymer electrolytes for lithium-anode batteries have failed due to the formation of lithium dendrites after repeated cycling. To overcome this problem, we have proposed the use of microphase separated block copolymers. High ionic conductivity is obtained in soft polymers such as poly(ethylene oxide) (PEO) where rapid segmental motion, which is needed for ion transport, necessarily results in a decrease in the rigidity of the polymer. Block copolymers have the ability to decouple the requirements of high modulus, needed to prevent dendrite growth, and high ionic conductivity. Furthermore, the use of block copolymers may enable the creation of well-defined, optimized pathways for ion transport. This dissertation presents studies of a poly(styrene-block-ethylene oxide) (SEO) copolymer blended with the lithium salt LiTFSI for use as a polymer electrolyte. In this case, the PEO is the ionically conducting block whereas the PS provides mechanical rigidity. The polymers used for this study were synthesized via anionic polymerization to obtain copolymers with low polydispersity. The introduction of a nonconducting microphase undoubtedly decreases the overall conductivity of the block copolymer relative to that of the ionically conducting homopolymer. Furthermore, the addition of salts into the block copolymer can be viewed as adding a selective solvent to the system. This invariably changes the energetic interactions in the systems. It is our goal to determine the correlation between the salt concentration and polymer phase behavior, and determine the effects of phase behavior on the ionic conductivity. The polymer electrolyte system is designated as SEO (a-b)/LiTFSI where a = molecular weight of the PS block (kg/mol) and b = molecular weight of the PEO block (kg/mol). By varying the salt concentration, r = [Li]/[EO], and by varying a and b, several different morphologies such as alternating lamellae, hexagonally packed cylinders, and a cocontinuous network phase are obtained. Characterization of the electrolyte systems includes a combination of small-angle Xray scattering, optical birefringence measurements, and alternating current impedance spectroscopy. The phase behavior and thermodynamics of the block copolymers as a function of LiTFSI concentration are also explored. It is assumed that the LiTFSI resides mainly in the PEO phase, the polymer with the higher dielectric constant, which is known for solvating lithium salts very effectively. Upon addition of LiTFSI salts to SEO systems, we obtain a disorder-to-order transition at a particular salt concentration. Further increases in the salt concentration have been shown to lead to other phase transitions such as lamellar to gyroid, or gyroid to cylinders. Changes in morphology cannot be attributed to increases in volume fraction of the PEO/LiTFSI phase alone. It is hypothesized that the presence of salts increases the effective Flory Huggins chi parameter. Using six different SEO/LiTFSI mixtures with accessible order-to-disorder transitions, we can develop a relationship to estimate the change in the effective chi parameter with salt concentration. It was established that this relationship is a linear function, in good agreement with theoretical predictions. This relationship was also obtained for a mixture of SEO polymers with the ionic liquid imidizolium TFSI (ImTFSI). The effective chi parameter relationships were approximately the same, indicating that the large anion drives the thermodynamics of the polymer/salt systems. The slope of the effective chi vs. r line, m, is compared to theoretical calculations. The theoretically determined values were consistently higher than experimentally determined ones. In this study, ionic conductivity measurements through order-order and order-disorder phase transitions (OOTs and ODTs) in mixtures of SEO with LiTFSI were performed to determine the effect of morphology on conductivity. The molecular weight of the blocks and the salt concentration were adjusted to obtain OOTs and ODTs within the available experimental window. The normalized conductivity (normalized by the ionic conductivity of a 20 kg/mol homopolymer PEO sample at the salt concentration and temperature of interest), was also calculated to elucidate the effect of morphology. For samples with a major phase PEO block (e.g. volume fraction of PEO in SEO is greater than 0.5), no dramatic changes in conductivity were seen when transitioning through different morphologies. The well-known Vogel-Tamman- Fulcher (VTF) equation provides an excellent fit for the temperature dependence of the conductivities regardless of morphology. However, for samples with minor phase PEO block, the conductivity/structure relationship is more complex. Through in-situ conductivity/SAXS experiments, these samples show changes in conductivity with temperature, which are dependent upon the thermal history. The reason for these changes has not been established.
Synthesis And Characterization Of Simultaneous Electronic And Ionic Conducting Block Copolymers For Lithium Battery Electrodes
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Author : Shrayesh Patel
language : en
Publisher:
Release Date : 2013
Synthesis And Characterization Of Simultaneous Electronic And Ionic Conducting Block Copolymers For Lithium Battery Electrodes written by Shrayesh Patel and has been published by this book supported file pdf, txt, epub, kindle and other format this book has been release on 2013 with categories.
Materials with nanostructured conducting domains are essential for a wide range of applications related to alternative energy. Active materials in battery and fuel cell electrodes such as LiFePO4, graphite, and platinum, are either electronic or ionic insulators. Nanoscale electron- and ion-conducting domains are necessary for enabling redox reactions in these materials. For example, a traditional porous lithium battery electrode consists of a redox-active material, carbon black for electronic conduction, and non-conductive binder that holds the particles in place. The pores are backfilled filled with organic electrolyte for ionic conduction. In some cases such as LiFePO4, electronic and ionic conductivities are so low that the active materials must be in nanoparticle form, and addressing such particles requires the transport of both kinds of charges to occur on nanometer length scales. Materials such as block copolymers can self-assemble and form co-continuous nanoscale domains. In this study, poly(3-alkylthiophene)-block-poly(ethylene oxide) (P3AT-PEO) copolymers are used to conducts both electronic and ionic charges. P3AT-PEO block copolymer molecules self-assemble on the nanometer length scale to yield P3AT-domains that conduct electronic charges and PEO-domains that conduct ionic charges. We propose to create a unique battery electrode where the LiFePO4 active material is dispersed in a nanostructured P3AT-PEO block copolymer, which functions simultaneously as the conductor of lithium ions and electronic charge, as well as the binder material in the electrode. The first phase of this dissertation work involved the synthesis of P3AT-PEO block copolymers. Regioregular P3ATs were synthesized using the Grignard metathesis (GRIM) polymerization method where in-situ end-group functionalization was employed to obtain ethynyl-functionalized P3ATs. Azide-functionalized PEOs were obtained through end-group modification of PEO monomethyl ether. Ethynyl-functionalized P3ATs and azide-functionalized P3AT-PEO were coupled using 1,3-dipolar cycloaddition "click" reaction to obtain P3AT-PEO block copolymer. In particular, poly(3-hexylthiophene)-block-poly(ethylene oxide) (P3HT-b-PEO) copolymers and a poly(3-ethylhexylthiophene)-block-poly(ethylene oxide) (P3EHT-b-PEO) copolymer were synthesized in this study. Next, the morphology of the P3AT-b-PEO copolymer was characterized using small angle X-ray scattering (SAXS). The morphologies of P3HT-b-PEO copolymers, where the P3HT block is the major component, are dominated by nanofibrils due to the crystallization of P3HT. In contrast, the nearly symmetric P3HT-b-PEO copolymers self-assemble into a lamellar phase. In addition, we show that P3EHT-b-PEO chains self-assemble to produce traditional nanoscale morphologies such as lamellae and gyroid in the melt-state. The segregation strength between the two blocks is controlled through the addition of lithium bis(trifluromethanesulfonyl) imide (LiTFSI). Our approach enables estimation of the "effective" Flory-Huggins interaction parameter, $chieff, using the random phase approximation (RPA). The $chieff trends with salt concentration suggest that the TFSI anion preferentially segregates into the P3EHT phase while Li+ remains in the PEO phase. For the salt-free sample, the gyroid morphology, obtained in the melt-state, is transformed into lamellae when the P3EHT block is crystallized. This is due to the "breaking out" of the crystalline phase. At high salt concentrations, P3EHT-b-PEO has a lamellar morphology in both melt and crystalline states (confined crystallization). We present the first reported study on the relationship between morphology and electronic/ionic charge transport of P3HT-b-PEO/LiTFSI mixtures. Using ac impedance spectroscopy, we show that P3HT-b-PEO/LiTFSI mixtures can conduct electronic and ionic charges simultaneously. At 90 °C, the electronic conductivity of P3HT-b-PEO/LiTFSI mixtures ranged from 10-8 to 10-5 S/cm depending on the volume fraction of P3HT. The decoupled ionic conductivity is around ~10-4 S/cm. It was shown that LiTFSI partitions between P3HT and PEO microphases. In particular, LiTFSI only partitions between the microphases when the PEO block molecular weight is 2 kg/mol while we observe no partitioning when the PEO block molecular weight of 4.2 kg/mol. It thus appears that the chemical potential of LiTFSI in PEO is a function of the PEO block molecular weight. We propose that the higher chemical potential of LiTFSI for P3HT-b-PEO copolymers with PEO molecular weight of 2 kg/mol drives the LiTFSI into the P3HT rich microphase. The electronic conductivity can be further increased by electrochemically chemically doping the P3HT chains with LiTFSI. Therefore, we quantified the electronic conductivity P3HT-b-PEO copolymers electrochemically oxidized with LiTFSI. We use a novel solid-state three-terminal electrochemical cell that enables simultaneous conductivity measurements and control over electrochemical doping of P3HT. At low oxidation levels, the electronic conductivity increases from 10-8 S/cm to 10-4 S/cm. At high oxidation levels, the electronic conductivity approaches 10-2 S/cm. These values match or exceed the ionic conductivity, which is important for enabling redox reactions in a battery as they involve equal moles of lithium ions and electronic charges. A lithium metal battery was assembled where the positive electrode consisted of P3HT-b-PEO conductive binder and LiFePO4 active material. We were able to cycle batteries and obtain capacities approaching the theoretical limit of LiFePO4. Importantly, P3HT is electroactive within the voltage window of a charge/discharge cycle. The electronic conductivity of the P3HT-b-PEO copolymer binder is in the 10-4 to 10-2 S/cm range over most of the potential window of the charge/discharge cycle. This allows for efficient electronic conduction needed for the successful cycling of the batteries. However, at the end of the discharge cycle, the electronic conductivity decreases sharply to 10-7 S/cm, which means the "conductive" binder is now electronically insulating. The ability of our conductive binder to switch between electronically conducting and insulating states in the positive electrode provides an unprecedented route for automatic overdischarge protection in batteries.
Electrochemical Systems
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Author : John Newman
language : en
Publisher: John Wiley & Sons
Release Date : 2012-11-27
Electrochemical Systems written by John Newman and has been published by John Wiley & Sons this book supported file pdf, txt, epub, kindle and other format this book has been release on 2012-11-27 with Science categories.
The new edition of the cornerstone text on electrochemistry Spans all the areas of electrochemistry, from the basicsof thermodynamics and electrode kinetics to transport phenomena inelectrolytes, metals, and semiconductors. Newly updated andexpanded, the Third Edition covers important new treatments, ideas,and technologies while also increasing the book's accessibility forreaders in related fields. Rigorous and complete presentation of the fundamentalconcepts In-depth examples applying the concepts to real-life designproblems Homework problems ranging from the reinforcing to the highlythought-provoking Extensive bibliography giving both the historical developmentof the field and references for the practicing electrochemist.
Advances In Lithium Ion Batteries
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Author : Walter van Schalkwijk
language : en
Publisher: Springer Science & Business Media
Release Date : 2007-05-08
Advances In Lithium Ion Batteries written by Walter van Schalkwijk and has been published by Springer Science & Business Media this book supported file pdf, txt, epub, kindle and other format this book has been release on 2007-05-08 with Science categories.
In the decade since the introduction of the first commercial lithium-ion battery research and development on virtually every aspect of the chemistry and engineering of these systems has proceeded at unprecedented levels. This book is a snapshot of the state-of-the-art and where the work is going in the near future. The book is intended not only for researchers, but also for engineers and users of lithium-ion batteries which are found in virtually every type of portable electronic product.