Degradation Phenomena of Lithium-rich Lithium-Nickel-Cobalt- Manganese-Oxide in Lithium-Ion-Batteries

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1 Degradation Phenomena of Lithium-rich Lithium-Nickel-Cobalt- Manganese-Oxide in Lithium-Ion-Batteries Der Naturwissenschaftlichen Fakultät / Dem Fachbereich Chemie und Pharmazie der Friedrich-Alexander-Universität Erlangen-Nürnberg zur Erlangung des Doktorgrades Dr. rer. nat. vorgelegt von Linda Brinkhaus aus Rheda-Wiedenbrück

2 Als Dissertation genehmigt von der Naturwissenschaftlichen Fakultät / vom Fachbereich Chemie und Pharmazie der Friedrich-Alexander-Universität Erlangen-Nürnberg Tag der mündlichen Prüfung: Vorsitzender des Promotionsorgans: Prof. Dr. Jörn Wilms Gutachter: Prof. Dr. Dirk M. Guldi Prof. Dr. Rainer Fink

3 Die vorliegende Arbeit wurde in der Zeit von Juli 2011 bis April 2014 im Technologiezentrum Isenbüttel der Volkswagen AG, in der VOLKSWAGEN VARTA Microbattery Forschungsgesellschaft mbh & Co. KG. in Ellwangen und am Department Chemie und Pharmazie am Lehrstuhl für Physikalische Chemie I der Friedrich-Alexander-Universität Erlangen-Nürnberg unter der Leitung von Prof. Dr. Dirk M. Guldi angefertigt. Die Ergebnisse, Meinungen und Schlüsse dieser Dissertation sind nicht notwendigerweise die der Volkswagen AG. Ich versichere hiermit eidesstattlich, dass ich die vorliegende Arbeit selbständig und nur mit Hilfe der angegebenen Hilfsmittel angefertigt habe. Linda Brinkhaus

4 "You will never understand the battery unless you make it. You will never understand it even though you make it." Takeshi Akamatsu (2000)

5 Zusammenfassung Die Energiedichte von Lithium-Ionen-Batteriezellen ist von entscheidender Bedeutung für die Reichweite von elektrischen und hybridischen Fahrzeugen, sowie für Geräte der Unterhaltungselektronik und der stationären Energiespeicherung. Zur signifikanten Erhöhung der Energiedichte sind neue Aktivmaterialien für die Kathode und Anode in Lithium-Ionen-Batterien unabdingbar. Ein vielversprechendes Aktivmaterial für die Kathode ist Lithium-reiches Lithium-Nickel-Cobalt-Mangan-Oxid (Li-reiches NCM), da dieses eine deutlich höhere theoretische spezifische Kapazität von 380 mahg 1 besitzt und damit um 35 % höher ist als die Kapazität von Standard Lithium-Nickel-Cobalt- Mangan-Oxid (Standard NCM), welches derzeit in kommerziellen Lithium-Ionen-Batteriezellen verwendet wird. Für kommerzielle Anwendungen muss dieses Material eine zufriedenstellende Langzeitstabilität in Lithium-Ionen-Zellen besitzen. Die wird nach momentanem Stand nicht erreicht. Diese Arbeit ist daher darauf ausgelegt, ein tieferes Verständnis über die Degradationsmechanismen, wie fundamentale physikalische, chemische und elektrochemische Prozesse, sowie Alterungsprozesse, die aufgrund der Prozesskette, anfallen, zu generieren, um Gründe für die geringe Langzeitstabilität zu identifizieren. Die zentrale Frage zielt darauf ab, ob und mit welchem Beitrag verschiedene Degradationsmechanismen zur Alterung des Materials beitragen. Weiterhin werden in dieser Arbeit Möglichkeiten aufgezeigt, diese Mechanismen teilweise zu umgehen oder zu minimieren, um für eine verbesserte Langzeitstabilität zu sorgen. Zunächst wird der theoretische elektrochemische Hintergrund dieses Materials für die weitere Analyse geschaffen. Wichtige elektrochemische Beziehungen, sowie spezifische Parameter werden diskutiert und für die nachfolgenden Messungen festgelegt. Als Anode wird stets Lithiummetall verwendet. Während der ersten 100 Zyklen verlieren entsprechende Batteriezellen ungefähr 30 % der Ursprungskapazität. Dies dient als Grundlage für die weitere Diskussion. 15 % dieses Verlusts wird der Alterung der Lithiumanode zugeschrieben, 10 % den strukturellen Umordnungen im Kristallgitter der Kathode, und 3 % dem Verlust an Übergangsmetall- V

6 ionen aus dem Kristallgitter und somit dem Verlust an aktivem Material. Übergangsmetallionen können weitere Mechanismen der Alterung, wie Anodenblockierung oder Elektrolytzersetzung induzieren und katalysieren. Es wird gezeigt, dass der Zusatz des Elektrolytadditivs Lithium (bis)oxalatoborat (LiBOB) die Metallauflösung zwar nicht vermindert, aber den Anteil auf der Anode minimiert. Diese Zellen zeigen eine bessere Langzeitstabilität und einen geringeren Abfall der Ursprungskapazität. Hieraus wird geschlussfolgert, dass der Einfluss von Übergangsmetallen kritisch ist. Die restlichen 2 % werden verschiedensten anderen Effekten zugesprochen. Auf der Basis dieser Degradationsmechanismen, werden Methoden erprobt, die die genannten Mechanismen kompensieren oder verhindern sollen. Um Strukturänderungen zu minimieren, wurde eine neue Zyklisierungsprozedur entwickelt. Diese beinhaltet die Idee, Übergangsmetallionen im Kristallgitter zu stabilisieren oder sogar bereits gewanderte Metallionen auf ihre Ursprungsplätze zurückzudrängen. Dies geschieht durch sogenannte Regenerationszyklen, die in die Standard Zyklisierungsprozedur eingefügt werden. Im Detail wird hier Manganmigration durch hohe C-Raten (> 0.5 C) und einer hohen Anzahl an diesen Regenerationszyken (> 5) im Bereich der Manganaktivität ( V) verringert. Weiterhin wurde durch eine Beschichtung der Ausgangspartikel die Metallauflösung reduziert. Elektrolytadditive verringern die Menge an Metallionen auf der Anode und stabilisieren zusätzlich die Kathodenoberfläche durch eine Schichtbildung und verhindern somit Elektrolytzersetzung. Zukünftig sollte der katalytische Effekt dieser Metallionen genauer hinsichtlich der Art des Metallions, der Konzentration im Elektrolyt und in metallischer Form auf der Anode, des Oxidationszustands und der elektrochemischen Zyklisierungsparametern untersucht werden, um diesen Effekt besser zu verstehen und Gegenmaßnahmen treffen zu können. VI

7 Abstract Increasing the energy density in lithium-ion-batteries is crucial for the widespread of electric or partly electrified vehicles, consumer electronics, or stationary energy storage systems. One feasible way to achieve this aim is to change the cell chemistry of a lithiumion-battery cell by substituting the existing anode and cathode active materials. One possible cathode material, that has the capability to increase the energy densities in future lithium-ion-batteries is lithium-rich lithium-nickel-cobalt-manganese-oxide (Li-rich- NCM) due to its high theoretical gravimetric capacity of 380 mahg 1, which is nearly 35 % higher than the theoretical capacity of standard lithium-nickel-cobalt-manganeseoxide (standard NCM), which is currently used for lithium-ion-batteries. The energy density impacts the energy storage property of a battery and, finally, the electrical range. An overall aim concerning Li-rich-NCM is the long-term-cycling-stability of the cells, that is not yet reached. As such, this thesis should provide a better understanding of possible degradation processes, namely fundamental physical, chemical, electrochemical, and processing phenomena, taking place in Li-rich-NCM, leading to the worse long-term-cycling-stability. The central question is whether and to what extent different deterioration mechanisms change the effectiveness of Li-rich-NCM active material. The thesis includes approaches, which prevent or minimize these degradation mechanisms. Therefore, the theoretical background needed to follow this thesis is provided. At the beginning, important electrochemical relationships and battery specific parameters are discussed. Lithium is used as anode. Concerning Li-rich-NCM, a capacity fading of 30 % during the first 100 cycles is measured. This fact is used as the basis for the discussion. 15 and 10 % capacity loss are ascribed to the anode and to structural transformation of Li-rich-NCM, respectively, while 3 % relates to transition metal ion loss, and, thus, a loss of active mass. Transition metal ions could induce a blocking of the anode or catalyze electrolyte decomposition. It was shown that the addition of lithium (bis)oxalatoborate (LiBOB) decreases the amount of transition metal ions on the anode. Simultaneously, cells with LiBOB show VII

8 a better capacity retention. Therefore, the impact of transition metals on the anode is critical. The residual 2 % are ascribed to different ageing effects. On the basis of these degradation mechanisms, methods are probed, which partly inhibit the aforementioned mechanisms. To minimize structural rearrangements, a cycling procedure was developed. The idea was to stabilize transition metal ions in their environment or to push transition metal ions back into the transition metal layers. As such, so-called regeneration cycles were inserted during the standard cycling procedure of Li-rich-NCM-cells. In detail, manganese migration was reduced by high current rates (> 0.5 C) and a high number of regeneration cycles (> 5), which cover the range between 2.5 and 3.7 V, namely the range of manganese activity. Furthermore, a coating of Lirich-NCM particles resulted in a lower transition metal dissolution. Electrolyte additives reduced the amount of transition metals on the anode and stabilized the Li-rich-NCM surface due to surface layer formation, which thus prevents electrolyte decomposition. Finally, a big topic in the future should be the investigation of the catalytical effect of transition metals regarding the type of the transition metal, its concentration in the electrolyte and in metallic form on the anode, the oxidation state, and the electrochemical parameters in order to understand this effect and initiate countermeasures. VIII

9 Table of Contents 1 Introduction and Motivation 1 2 Theoretical Concepts Thermodynamic and Electrochemical Aspects of Lithium-Ion-Batteries Overpotentials of Half Cells and Internal Resistance The Voltage Plateau Theory of Lithium-rich Lithium-Nickel-Cobalt-Manganese-Oxide as Cathode Material for Lithium-Ion-Batteries History of the Development of Li-rich Lithium-Nickel-Cobalt-Manganese- Oxide Cathode Materials Structure of Li-rich Lithium-Nickel-Cobalt-Manganese-Oxide Intercalation and Deintercalation Mechanism of Lithium-rich Lithium- Nickel-Cobalt-Manganese-Oxide Structural Changes in Lithium-rich Lithium-Nickel-Cobalt-Manganese- Oxide Challenges of Lithium-rich Lithium-Nickel-Cobalt-Manganese-Oxide Electrochemical Methods Galvanostatic Cycling Cyclic Voltammetry Alternating Current Methods - Electrochemical Impedance Spectroscopy Principles of Optical Spectroscopy Raman Spectroscopy and Microscopy X-ray Diffraction Inductively-Coupled Plasma Optical-Emission-Spectroscopy Microscopy Scanning Electron Microscopy Transmission Electron Microscopy IX

10 Table of Contents 3 Objective 58 4 Experimental Instruments Chemicals and Materials Sample Preparation and Measuring Conditions Results and Discussion SEM/TEM Investigations of Li-rich Lithium-Nickel-Cobalt-Manganese- Oxide as Active Material in Lithium-Ion-Cells Estimation of the Degradation Impact of the Lithium Anode and the Electrolyte in Li-rich Lithium-Nickel-Cobalt-Manganese-Oxide Cells Electrochemical, Spectroscopic and Microscopic Characterization of Lirich Lithium-Nickel-Cobalt-Manganese-Oxide Manganese Activity in Li-rich Lithium-Nickel-Cobalt-Manganese- Oxide - Electrochemical Investigation Structural Transformation of Li-rich Lithium-Nickel-Cobalt-Manganese- Oxide during Charge and Discharge - Spectroscopic Investigation Regeneration of Li-rich Lithium-Nickel-Cobalt-Manganese-Oxide Electrolyte Decomposition in Li-rich Lithium-Nickel-Cobalt-Manganese- Oxide-Cells Transition Metal Dissolution and Deposition Macroscopic Degradation of Li-rich Lithium-Nickel-Cobalt-Manganese- Oxide Global Discussion of the Impact of Degradation Phenomena on Capacity Retention Conclusion and Outlook Appendix Raman Spectra Standard deviation of ICP-OES data References Curriculum Vitae IX XX X

11 Nomenclature A AE ac α BET C CV c cc cv D DEMS DFT DMC DSC d ΔG E EC EDX EMC F FEC GC HOMO HR-TEM I ICP-OES i.e. η j k λ area Auger electron alternating current symmetry factor, polarizability Brunauer-Emmett-Teller number of components, capacitance cyclic voltammetry concentration constant current constant voltage diffusion constant differential electrochemical mass spectrometry discrete fourier transform dimethylcarbonate differential scanning calorimetry diameter free energy difference of a galvanic reaction voltage ethylenecarbonate energy dispersive X-ray ethylmethylcarbonate Faraday constant, degree of freedom fluroethylene carbonate gas chromatography highest occupied molecular orbital high-resolution transmission electron microscopy current inductively-coupled plasma optical-emission-spectroscopy that is overpotential current density reaction rate wavelength XI

12 Nomenclature L LCO LFP LIB LMO LUMO LiBOB Li-rich-NCM M MS m μ N N A NCA NEP Ni-Cd Ni-MH OSSE ω P PVDF p ppb ppm ϕ Q Q th q R SEI SEM SOC Si/C standard NCM σ T TEM TG TGA TM t VP XRD Z z inductance lithium cobalt oxide lithium iron phosphate lithium-ion-battery lithium manganese oxide lowest unoccupied molecular orbital lithium bis(oxalato)borate lithium-rich lithium-nickel-cobalt-manganese-oxide molar mass mass spectrometry mass chemical potential, induced dipole, magnetic permeability number of intensive variables Avogadro constant nickel cobalt aluminum oxide N-ethyl-pyrrolidon nickel-cadmium nickel-metalhydride octahedra site stabilization energy frequency number of phases, power poly(vinylidene difluoride) pressure parts per billion parts per million potential amount of charge; specific capacity, group of all individual normal modes q galvanostatic current rate efficiency, normal coordinate universal gas constant solid electrolyte interphase scanning electron microscopy state-of-charge silicon/carbon composite standard lithium-nickel-cobalt-manganese-oxide electronic conductivity temperature transmission electron microscopy thermogravimetry thermogravimetric analysis transition metal time vinylpyridine X-ray diffraction atomic number valence number of ions XII

13 1 Introduction and Motivation Global warming and finite supply of fossil fuels are reasons requiring renewable energies and sustainable mobility. Even today, half of the population worldwide lives in urban areas. People are highly impacted by smog, noise, and traffic jams due to plants, power plants, and vehicles. The development of renewable energies in the federal republic of Germany, especially in the area of power generation by wind energy and photovoltaics, demands the research of suitable storage technologies, which store the non-projectable generated excess of energy and provide it if required. Even when they are plugged into the grid, a storage device is required to smooth the output [1 3]. Batteries, composed of battery-cells, are from an environmentally point-of-view the first choice because they store and provide electrical energy nearly without loss. Alternatives are: pumped-storage power station implying an intervention into nature and locally generated energy has to be transported over long distances. storage technologies including the conversion of electrical energy in, for example, hydrogen and generation of electrical energy by fuel cells. The maximum efficiency is 60 % [4]. Another advantage of batteries is that they are employable in mobile applications, i.e. in homes (4-20 kwh) and in electrical vehicles (18-50 kwh). By now, the lithium-ion rechargeable battery has enabled the wireless revolution of cell phones, lap-top computers, digital cameras, and i-pads as means to transform global communication. The adaptation of electric vehicles, which are powered by renewable energies, is a much needed milestone towards a neutral CO 2 and, thus, sustainable mobility. Range extension, costs, quick-charge, optimization of an electric engine are emerging topics concerning the improvement of electric vehicles suited for daily use. Establishing Germany as a lead market and a lead provider in the area of electric mobility is a top priority of the federal government and German industry. Together, they share 1

14 Introduction and Motivation the vision of putting at least one million electric vehicles on Germany s roads by Currently, 10,000 battery electric vehicles are registered in Germany. In 2013, 0.2 % and 0.9 % of newly registered cars were battery electric and hybrid electric vehicles, respectively [5]. However, to fully exploit the huge CO 2 emissions reduction potential of electric vehicles, the electricity required has to come from renewable energy sources [6]. The efficiency of an electric motor is > 90 %, which is more than twice the efficiency of a modern gasoline or diesel engine. The positive balance is downgraded by the low energy density of batteries. An automotive battery capacity of 25 kwh corresponds to about 10 L fuel assuming similar mechanical efficiency (without recuperation energy) [7], but the acceptance of an electrochemical energy accumulator for its application in electric vehicles depends on a number of technological, economical, and ecological aspects. Energy density, power density, cycle life, safety, and costs are key criteria regarding battery development [8]. The energy density impacts the energy storage property of a battery and, finally, the electrical range. The product of energy density (Ah kg 1 ) and the cell voltage (V) defines the energy content per mass of a battery (Wh kg 1 ). An increase of the accumulator dimension leads to an increase of energy consumption due to higher weight of the accumulator. In addition, space in vehicles is limited. Inactive materials like separators, electrolyte, current collectors, and cell housing need to be considered with respect to overall weight and volume [9]. Important vehicle parameters like acceleration and speed depend on the power of the electric engine and on the power density of the accumulator. The energy density represents the maximum available battery power. It describes the power provided by the battery mass (W kg 1 ). The dynamic provision and admission of energy is important, especially for hybrid vehicles and battery electric vehicles concerning acceleration and quick charging [9]. Over the years, energy, and power of batteries degrade due to mechanical and thermal loads. In an ideal case, a lifetime of a battery should comply with the lifetime of the vehicle, namely ten years. The cycle life represents the number of charge and discharge processes until the capacity drops below 80 % of the original capacity [9]. Costs of electric vehicles have a high impact on the market acceptance. Depending on the cell chemistry, manufacturing and battery system costs can exceed 500 and 1000 e kwh 1, respectively. Volume production and the development of manufacturing technologies should lower the overall costs. Several studies predict costs between 200 and 600 e kwh 1 in 2020 [7]. 2

15 Introduction and Motivation Large-sized automotive batteries contain a high amount of energy. Several of the chemicals are highly flammable and may generate explosive mixtures upon leakage. Short circuits, overcharge, high temperature exposure, and possible collisions and accidents of cars are high risk factors [10]. Successive improvements in battery technology concerning the aforementioned issues triggered major electrical breakthroughs, from early scientific studies to the advent of telegraphs and telephones, leading eventually to portable computers, mobile phones, electric cars and multitudes of other electrical devices. The first battery was invented by Volta in 1800 consisting of alternating discs of zinc and copper separated by a cardboard and using a brine solution (NaCl). In 1866, Léclanché developed a battery with a zinc-amalgam bar anode and a cathode comprising of manganese dioxide. Here, some small amounts of carbon powders and an ammonium chloride electrolyte are critical. The electrolyte in today s applications is zinc chloride mixed with a minor amount of ammonium chloride. Disadvantages in zinc/carbon batteries arise from the fact that electrolytes are an active part of the cell reaction. This results in a decreasing electrolyte concentration during cell operation. Present cells with improved shelf-life and power density use an alkaline electrolyte (aqueous KOH), a zinc anode, and a manganese oxide cathode. Their energy density reaches 150 Wh kg 1 [11]. Alkaline cells are all primary cells, and not rechargeable [12]. Rechargeable batteries, better known as secondary batteries, have evolved over the years from lead acid in 1859 via nickel cadmium (Ni-Cd) in 1899 and nickel metal hydride (Ni-MH) in the mid-1980s to lithium-ion in Lead-acid batteries are used in battery power applications in energy storage, emergency power, and electric and hybrid vehicles. A limited energy density, typically between 30 and 50 Wh kg 1, and a relatively low cycle life of 350 cycles are disadvantages concerning the application in electric vehicles [13]. Lead-acid batteries are, however, irrelevant regarding the prospective electromobility [7]. The components of a Ni-Cd battery are a cadmium metal anode, a nickel oxide hydroxide or nickel oxide cathode, and a potassium hydroxide electrolyte solution. The gravimetric energy of these batteries ranges from 40 to 60 Wh kg 1. Ni-Cd batteries are mostly used in portable devices such as mobile phones, digital cameras, and power tools. The drawback of Ni-Cd rechargeable batteries is the "memory effect", that is, upon charging the voltage, at which discharge ceased, will be attained rather than of the maximum voltage [12]. Consequently, energy is lost. In the 1970s, a surge of interest, lead to developing new rechargeable batteries. In 1967, 3

16 Introduction and Motivation scientists discovered that sodium beta alumina features an exceptionally high ionic conductivity [14]. This discovery was the prelude to a revolution in solid-state electrochemistry. It resulted in the use of solid compounds that could reversibly store lithium, like TiS 2, or hydrogen, like LaNi 5, which became the basis for rechargeable Li-ion batteries and the Ni-MH batteries, respectively [15]. Ni-MH batteries contain a nickel electrode similar to that used in Ni-Cd batteries as positive electrode. The anode is composed of alloys expressed in the form of AB 5, where A is an alloy of La, Ce, Nd, and Pr, while B is an alloy of Ni, Co, Mn, and Al. Ni-MH batteries were commercialized in The high capacity of Ni-MH batteries, which is approximately twice that of a Ni-Cd battery, is based on a hydrogen-absorbing alloy as negative electrode. This alloy absorbs a large amount of hydrogen and features excellent reversibility in terms of hydrogen absorption and desorption. Notably, the typical specific energy for Ni-MH cells is between 70 and 80 Wh kg 1. The memory effect of Ni-MH is similar to that described for Ni-Cd battery [12]. The Ni-MH technology was implemented in the first generation of hybrid electric cars. It is highly reliable in cycling throughout several thousand times. Still, they have been displaced by lithium-ion because of its higher energy storage capability and lower costs [16]. The potential of Ni-MH batteries for electric vehicles is, however, disregarded due to already exhausted battery capacities [7]. It did not take long for researchers to realize that lithium-based cells were promising candidates for secondary batteries as well. Due to its low density, lithium has a specific capacity of 3680 Ah kg 1. Li is the most electropositive metal and gives rise to very high electrode potentials. Extensive research on rechargeable lithium batteries, which operate around room temperature, began in the early 1970s. Back then, it was discovered that intercalation and insertion reactions into a host lattice were ideal for storing energy. Today, essentially all secondary lithium batteries use intercalation or insertion reactions for both electrodes. In other words, the basis for storing energy has not changed in almost 40 years [12, 16]. Lithium-ion-batteries are generally composed of lithium containing transition-metal oxides as the positive electrode material and a carbon material as the negative electrode material [17]. Carbon-based anodes have been used in essentially all lithium batteries since 1990 [18]. Carbon reacts with lithium to form the intercalation compound LiC 6 very readily at room temperature. To this end, purified natural graphites have recently replaced expensive synthetic carbons, such as mesocarbon microbeads (MCMB). This was probably the most important breakthrough to render Li-ion battery commercially viable. A carbon anode takes up as much space as the cathode, because of its low gravimetric density. 4

17 Introduction and Motivation Its energy storage capability is 340 Ah kg 1 and 740 Ah L 1. Silicon has received much more attention in the last five years than any other host metal for anodes. It is readily available, low cost, and reacts readily with lithium under ambient conditions. As with tin, it needs to be nanosized to be effective. In addition, smart nanostructures need to be developed to allow for the huge expansion on lithium reaction and to attain of high volumetric capacities. Numerous announcements have been made about commercializing silicon anodes, but none are available yet. NEC has developed a new silicon oxide anode that uses carbon nanohorns as conductive agent. Here, an energy density of 271 Wh kg 1 is proposed [19]. In contrast, Amprius is developing a silicon anode consisting of silicon nanowires using a chemical vapour deposition technique [20]. Panasonic delayed its exciting round cell until This cell has specifications showing a volumetric energy density 60 % higher than today s cells [7]. Not only anode materials but also cathode materials were developed during the last decades. The first commercial secondary Li cells were manufactured by Exxon Company in 1970 with a LiT is 2 cathode. After the announcement and brief commercialization of Li/TiS 2 cells, there was a hiatus until 1990, when SONY brought the C/LiCoO 2 cell onto the market [16]. The successful commercialization of the lithium secondary battery took less than 17 years. Although the lithium cobalt oxide (LCO) cathode has dominated for well over a decade, there has been much effort to replace the cobalt. Cobalt is too expensive and the battery market is driven by the price of cobalt. A wide range of metals may replace either totally or in part cobalt. Lithium cobalt oxide offers a high energy density, but presents safety risks, especially when damaged. The more common compositions are LiNi 1/3 Co 1/3 Mn 1/3 O 2 and LiNi 0.8 Co 0.15 Al 0.05 O 2, which are commonly known as NCM and NCA, respectively [16, 21]. In addition, olivine lithium iron phosphate (LFP), spinel lithium manganese oxide (LMO), and the aforementioned NCM offer lower energy density, but longer lifetimes and inherent safety. Such batteries are widely used for electric tools and medical equipment. NCM in particular is a leading contender for automotive applications. On the other hand, LiMn 2 O 4 and LiF ep O 4 electrodes are significantly more stable under lithium extraction conditions than layered Co- and Ni-based electrodes, both structurally and thermally. But, they deliver relatively low practical capacities above 3 V in a lithium cell, typically Ah kg 1 at moderate current rates [22]. The energy density of commercial cells using LiCoO 2 have far more than tripled since their introduction in In just a few years from 1999 the volumetric energy density increased from 250 to over to 570 Wh L 1 in The actual specific energy density 5

18 Introduction and Motivation achieved by a Li-ion battery is in the region of Wh kg 1. However, the rechargeable capacity for all of these materials approaches their limits ( Ah kg 1 ). In light of the aforementioned cathode materials associated with higher specific capacity are needed to meet the demand for further energy density enhancement. Researchers continue to probe variations of the above layered materials to increase the capacity and to decrease costs. It is widely expected that with a considerable amount of research and development the maximum specific energy density that can be achieved within the next 5 years could be 300 Wh kg 1 [23]. To reach this goal, one example is increasing the lithium content as exemplified by the formula 0.5 Li 2 MnO LiMO 2, where M = Ni, Co, Mn, which researchers at Argonne National Laboratory report can achieve capacities exceeding 250 Ah kg 1 [22]. Although researchers have put forth much effort in studying these so-called lithium-rich lithium-nickel-cobalt-manganese-oxide (Li-rich-NCM) materials in the past, many debates and issues over these materials still exist. These need to be clarified and solved in the future. The electrochemical properties associated with the low initial columbic efficiency, slow Li + diffusion speed, and voltage degradation during cycling are the main problems preventing the utilization in lithium-ion-batteries. Thus, the lifetime requirements of a battery cell with Li-rich-NCM as cathode material cannot be fulfilled yet [24]. Nevertheless, it is aimed that new cathode and anode materials like Li-rich-NCM and silicon, respectively, are combined to yield a maximized cell voltage and energy density of up to 300 Wh kg 1. A change of one component in a lithium-ion-cell influences the whole cell chemistry and can provoke different ageing mechanisms. Thus, research activities need to be concentrated on developing the complete full cell system. If all five issues (energy density, power density, cycle life, safety and costs) are fulfilled, a new cell chemistry may be ready to enter the market. With a higher driving range, lower costs, and a higher input of renewable energies, the market acceptance of electric engines will be undoubtfully improved. They can power vehicles in the near future leading to a sustainable mobility. 6

19 2 Theoretical Concepts 2.1 Thermodynamic and Electrochemical Aspects of Lithium-Ion-Batteries Scientifically, battery cells and also lithium-ion-cells are referred to as electrochemical or galvanic cells. This is due to the fact that they store electrical energy in the form of chemical energy. In addition, the electrochemical reactions that take place are also termed galvanic. Galvanic reactions are thermodynamically favorable (the free energy difference, ΔG, is negative) and occur spontaneously when two materials of different standard reduction potentials are connected by an electronic load (meaning that a voltage E is derived). When a current is flowing through the external circuit, the electrochemical processes occur and the amount of charge Q is determined by [12]: Q = I t (2.1) During the time t, a specific number of ions react. Thus m z N M A electrons are transported. Then Q is: Q = m M z N A e (2.2) with F = N A e the Faraday constant and e the electric charge of an electron. Therefore, the current I is be expressed by: I = m M z F 1 t (2.3) The quantitative correlation between ΔG and E results, when the reaction work is expressed by the electric energy produced by the cell per formula unit [25]: ΔG = zfe (2.4) 7

20 Theoretical Background The electrochemical series indicates how easily a metal is oxidized or its ions are reduced. On the one hand, the material with the lower standard reduction potential, called E 0, undergoes oxidation providing electrons into the external circuit. On the other hand, the material with the higher standard reduction potential, undergoes reduction. Both reactions occur concurrently and enable for the conversion of chemical energy into electrical energy by means of electron transfer through the external circuit. The material with the lower standard reduction potential is the negative electrode or anode on discharge (since it provides electrons), while the material with the higher standard reduction is the positive electrode or cathode on discharge (since it accepts electrons). Potential differences are only be determined as a difference between two potentials, while it is impossible to determine the absolute potential of a single electrode. For this reason, the potential of the hydrogen electrode in a 1 M acidic solution is set to 0 V at 25 C and kpa. These conditions are called standard conditions [25]. The cell voltage is therefore given by ΔE 0 = E 0 cathode E 0 anode (2.5) A negative ΔE 0 means that the electrochemical reaction proceeds in the reverse direction. Anodic and cathodic sides are exchanged. In addition, an electrolyte and a separator are required for a practically usable electrochemical conversion. The electrolyte is an ion conducting material, which can be in the form of an aqueous, molten or solid solution. The separator is a membrane that physically prevents a direct contact between the two electrodes and allows ions but not electrons to pass through [12]. As far as the maximum electric energy, which might be delivered by chemicals that are stored within or supplied to the electrodes in the cell, depends on the change in free energy ΔG of the electrochemical couple. The sum of chemical potentials μ i of the compounds ν i involved in the reaction is equal to the reaction free energy. ΔG = ν i μ i (2.6) As a result of combinating Eqs. 2.4 and 2.6 the free reaction enthalpy ΔG and the equilibrium cell voltage ΔE 0 under standard conditions are related to the sum of the chemical potentials μ i of ν i. 8

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