li ion battery characterization

Capacity Studies of Li-ion Battery

Capacity Studies of Li-ion BatteryWith some cathodes1General Principle and Classification

PrincipleElectrons released at the negative electrode.These flow through the load and are accepted by the positive electrode. A voltage is measured due to the potential difference between the two electrodes of the cell.

http://spacepwr.jpl.nasa.gov/battery.htm#Lithium2

Lithium BatteriesIntroduced by Sony in 1991.Have been widely used to provide power for consumer products.Offer low safety risks, greater flexibility in battery configuration and energy densities exceeding 120 Wh/kg.Excellent pressure tolerance and neutral buoyancy.Make use of intercalant solids as electrodes.Host atoms or molecules within its lattice with very few structural changes.

Lithium batteries: New Materials, Developments and Perspectives, G. Pistoia, Elsevier 19943Intercalation

http://spacepwr.jpl.nasa.gov/lithumbgr.htm4Working Principles Electrochemical chain characterized by continued transport of lithium ions from a higher potential ( anode) to a lower potential (cathode).

Electrical energy liberated while discharging is equal to the change in lithium free energy due to the transfer.

Cell reactions in a Li/ Lix(cathode) system:

x Li x Li + + x e- (Li anode)x Li + + x e- + Lix(host) Lix + x (host cathode)Overall reaction:x Li + Lix(host) Lix + x (host)

Lithium batteries: New Materials, Developments and Perspectives, G. Pistoia, Elsevier 19945Lithium MicroBatteryMiniaturized power supply needed for micro-mechanical devices.Lithium microbatteries built using thin film technologies.

Substrate3 Intercalating electrode2 Electrolyte1 Lithium metal complexTypical lithium microgenerator

Hundreds of microcells on a four-inch diameter silicon wafer.

http://www.afrlhorizons.com/Briefs/Dec01/PR0104.html6Perform rate capability studies on cells cycled to different charge-discharge cycles.Perform half-cell studies to analyze causes for capacity decreaseUse impedance spectroscopy to analyze the change in cathode and anode resistance with SOC.Study structural and phase changes at both electrodes using XRD.7Characteristics of a Sony 18650 Li-ion cellCathode (positive electrode) - LiCoO2.Anode (negative electrode) - MCMB.Cell capacity 1.8 Ah

8Characteristics of a Sony 18650 Li-ion cellCharacteristics

Positive LiCoO2

Negative Carbon

Mass of the electrode material (g)

15.1

7.1

Geometric area (both sides) (cm2)

531

603

Loading on one side (mg/cm2)

28.4

11.9

Total Thickness of the Electrode (m)

183

193

Specific Capacity (mAh/g)

148

306

9Experimental Cycling StudiesCells cycled using Constant Current-Constant Potential (CC-CV) protocol. Cells were discharged at a constant current of 1 A.Batteries were cycled at 3 different temperatures 25oC, 45oC and 55oC. Experiments done on three cells for each temperature.Rate capability studies done after 150, 300 and 800 cycles - Cells charged at 1 A and discharged at currents of 0.2, 0.4, 0.6, 0.8 and 1.0 A.10Experimental - CharacterizationBatteries were cut open in a glove box after 150, 300 and 800 cycles.Cylindrical disk electrodes (1.2 cm dia) were punched from both the electrodes. Electrochemical characterization studies were done using a three electrode setup. Impedance analysis - 100 kHz ~ 1 mHz 5 mV.Material characterization - XRD studies and SEM, EPMA analysis.11Experimental - Characterization

12Discharge Curve Comparison of Sony 18650 Cells after 800 Cycles

13Capacity Fade as a Function of Cycle Life

14Capacity Fade as a Function of Cycle Life

15Charge Curves at Various Cycles

45 deg C55 deg C

Room Temperature

16Change in Charging Times with Cycling Constant Current

Constant Voltage

17Rate Capability after 150 and 800 Cycles

18Nyquist Plots of Sony Cell at RT and 55oC

19Nyquist Plots of Sony Cell at RT and 45oC

20Negative Electrode Resistance (Fully Lithiated)

21Positive Electrode Resistance (Fully Lithiated)

22Comparison of Electrode Resistances

150 Cycles300 Cycles23Possible Reasons for Rapid Capacity Fade at Elevated TemperaturesThe SEI layer formed on a graphite electrode changes in both morphology and chemical composition during cycling at elevated temperature.The R-OCO2Li phase is not stable on the surface and decomposes readily when cycled at elevated temperatures (55oC). This creates a more porous SEI layer and also partially exposes the graphite surface, causing loss of charge on continued cycling. The LiF content on the surface increases with increasing storage temperature mainly due to decomposition of the electrolyte salt.SEI and electrolyte (both solvents and salt) decomposition have a more significant influence than redox reactions on the electrochemical performance of graphite electrodes at elevated temperatures.24Nyquist Plot of Fresh LiCoO2 as a function of SOC at RT

25Nyquist Plot of Fully Delithiated LiCoO2 as a function of Storage Time at RT

26Nyquist Plot of Fully Lithiated LiCoO2 as a function of Storage Time at RT

27Specific Capacity of Positive and Negative Electrodes at Various Cycles and Temperature

Cell(Cycle No. Temperature)Specific capacity (mAh/g)

LiCoO2CarbonFresh147.81306.17150-RT144.292.38%299.552.16%150-45143.123.17%296.583.13%150-55141.254.44%290.565.10%300-RT139.175.84%283.957.26%300-45138.216.49%282.177.84%300-55125.1015.36%246.5819.46%28Comparison of Capacity Fade of Individual Electrodes with Full Cell LossCell(Cycle No. Temperature)Capacity Lost (mAh)Full Cell Capacity LossLiCoO2Carbon(mAh)150-RT53.06146.947107150-4570.74468.046125150-5598.996110.773168300-RT130.390157.719182300-45144.885170.379209300-55342.846423.04648129CVs of Sony Cell

Room Temperature30CVs of Sony Cell

31XRD Patterns of LiCoO2 after Different Charge-Discharge Cycles

Cellc/aFresh5.103150-RT5.077150-455.066150-554.995300-RT4.998300-454.995300-554.98532Variation of Lattice Constants with Cycling and Temperature

*G. Ting-Kuo Fey et al., Electrochemistry Comm. 3 (2001) 234Decrease in c/a ratio leads to decrease in Li stoichiometry*33Capacity FadeLoss of Li(Primary Active Material)Degradation of C, LiCoO2(Secondary Active Material)SEI FormationOvercharge

Salt Reduction

Solvent Reduction

Electrolyte OxidationStructural Degradation 34Physical Characteristics of Cellbatt Lithium Ion Battery Electrodes

Cellbatt is a Prismatic type cell35Electrode ReactionsAt anode

At cathode

Cell Reaction

Non-Stoichiometric Spinel36Charging ProtocolsConstant current - Constant voltageTotal charging time fixedConstant voltageCharging done completely at constant voltageConstant current - Constant voltageCharging stopped when the current reaches a value of 50 mA during the CV partCharging done to different cut-off potentials37Change in discharge capacity for Li-ion cells charged to different potentials

38ExperimentalFull Cell studies on CellBatt Li-ion CellsGalvanostatic charge-discharge 0.25 A, 0.5 A, 0.75 A, 1 A - (3.0-4.17 V)Cyclic Voltammograms - 0.05 mV/s, 2.5-4.2 VT-cell (half cell) studiesGlove Box - Disk electrodes 1.2 cm Counter, Reference electrodes Li metalCyclic Voltammograms - 0.05, 0.1 and 0.2 mV/s, 3-4.5 V vs. Li/Li+ for spinel and 0-1.2V vs. Li/Li+ for carbonImpedance Analysis - 100 kHz ~ 1 mHz 5 mV.XRD studies of spinel electrode at various cycles.

39Charge curves for CC-CV Protocol

40Charge and Discharge curves for Li-ion Cell at various CyclesCapacity Fade 15.4% for C/2 rate

C/2 RateC/2 Rate

Capacity Fade 19% for 1 C rate41Change in CC-CV Profiles with Cycling

42Nyquist plots for Cellbatt cell charged at 0.5 A at different states of charge

43Nyquist plots for Cellbatt cell charged at 0.5 A during different cycles

44Nyquist Plots for Spinel and Carbon Electrodes at Discharged state at Various Cycles

SpinelCarbon45Cyclic Voltammograms of Spinel Electrode after 800 Cycles at various Scan rates

46Cyclic Voltammograms of Carbon Electrode after 800 Cycles at various Scan rates

47Cyclic Voltammograms of Spinel and Carbon Electrodes at Different Cycles

SpinelCarbon

48XRD Patterns of Spinel after Different Charge-Discharge Cycles

P. G.. Bruce et al., J. Electrochem. Soc., 146, 3649 (1999). 49ConclusionsVarying the charging rate affects the overall capacity of the cell.Impedance studies reveal no significant increase in resistance at both electrodes after 800 cycles.XRD studies of Spinel electrode reveal the formation of an additional phase with cycling. Capacity fade in the case of Cellbatt cells can be summarized as50Capacity Fade in Cellbatt Li-ion cellsSecondary Active Material Degradation(C6 & LiMn2O4)Structural Degradation of LiMn2O4Mn Dissolution from SpinelSEI layer attack on Negative ElectrodeHF formationAccumulation of -MnO2 with Cycling

Electrolyte Oxidation(starts from 3.7 V)

Salt HydrolysisJ.C.Hunter et al.E. Wang et al.51Intercalation ElectrodesLithiated metal oxides-VOx, LiCoO2, LixMn2O4, LixNiO2, LixSnThin film deposition- CVD, RF Sputtering, Pulsed Laser Deposition.

Lithium batteries: New Materials, Developments and Perspectives, G. Pistoia, Elsevier 199452Advantages of Lithium Ion BatteriesStore 2-3 times more energy per unit weight and volume than lead-acid or Ni-Cd batteries.Long cycle lives (>1000 cycles)Low self-discharge and long shelf life.Widespread use in electronic devices.Potential applications promise in the areas of communications and remote sensing devices too!!!

Sides, C.R.; Li, N.; Patrissi, C.J.; Scrosati, B.; Martin, C.R. Nanoscale Materials for Li-ion Batteries, MRS Bulletin, 2002, 27, 604-607. 53LimitationsCritical area for improvement rate capabilityRate capability- ability to deliver large capacity when discharged at high C rates. ( rate of C/1 corresponds to the current required to completely discharge an electrode in 1 hour)Future applications require high-discharge-rate periods.

Sides, C.R.; Li, N.; Patrissi, C.J.; Scrosati, B.; Martin, C.R. Nanoscale Materials for Li-ion Batteries, MRS Bulletin, 2002, 27, 604-607. 54Motivation for use of Nano technologyLimitations in rate capabilities slow diffusion processShorter diffusion distance for Li+ ionIncreased surface areaPromise better rate capabilities.Smaller effective current density during discharge.Better cyclability due to smaller particles.Need for energy sources to power nano devicesMartin, C.R.; Li, N.; Scrosati, B. Nanomaterial-Based Li-Ion Battery Electrodes, J. Power Sources, 2001, 97-98, 240-243.

55Fabrication Technique

Template method-

General method to synthesize nanomaterials. Synthesis entails deposition of material of interest/ precursor, within cylindrical and monodisperse pores of a microporous template membrane. Cylindrical nanostructures with monodisperse diameters and lengths obtained. May be solid nanofibers or hollow nanotubes depending on membrane used.

C.R.Martin, Science, 266, 1961 (1994)56Electrode Fabrication

Precursor depositionGel formationTemplate removalThermal processing50 nm pores filled with triisopropoxyvanadium oxide.Gel formation after 12 hrs.Template removed with oxygen plasma(100mTorr O2, 2hrs)Processed at 400C for 10hrs in 150psi O2

Patrissi, C.J.; Martin, C.R. J. Electrochem. Soc. 1999, 146, 3176-3180.

57SEM micrographs

SEM images of the componenents of a nanostructured electrode: (A) low-magnification image of the V2O5 nanofibrils, (B) high-magnification image of the nanofibrils, and (C) the underlying V2O5 surface layer.

Patrissi, C.J.; Martin, C.R. J. Electrochem. Soc., 2001, 148, A1247-A1253.

58Sn-based anodesCan store twice as much lithium compared to carbon anodes.4Li+ + 4e- + SnO2 2Li2O + SnxLi + + xe - + Sn LixSnCan store upto 4.4 Li atoms per atom of Sn.Volume changes during alloying/dealloying cause internal damage to electrode lower cyclability.Nanostructure based designs can better accommodate for volume changes

Li, Naichao; Martin, C.R. J. Electrochem. Soc. 2001, 148, A164-A170.

59Sn- based anodesFabricated using template synthesis with a SnCl2 based precursor.Nanofibers heated at 440C to convert them to crystalline SnO2. Fiber dia. 110nmThin film electrode fabricated without template membrane.(550nm)

Li, Naichao; Martin, C.R. J. Electrochem. Soc. 2001, 148, A164-A170.

60Template based electrodesObserved improved rate capabilities Loss of volumetric energy density due to extremely low porosity of polycarbonate membranes(1.2%)Low number density of nanofibers protruding from current collector surface.Problem addressed by using alumina membranes (highly porous)Dissolution of membrane in aqueous acid or base; but this also dissolves the electrode materials.Chemical etching used to increase porosity of polycarbonate membranes.

Sides, C.R.; Li, N.; Patrissi, C.J.; Scrosati, B.; Martin, C.R. MRS Bulletin, 2002, 27, 604-607. 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