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Electrochemical performance of the reaction of recovered limn1 / 3ni1 / 3co1 / 3O2 with molybdenite in lithium ion battery

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https://www.eduzhai.net International Journal of M aterials and Chemistry 2013, 3(5): 85-90 DOI: 10.5923/j.ijmc.20130305.01 Electrochemical Performance of Recycled LiMn1/3Ni1/3Co1/3O2 Reacted with Molybdenite in Lithium-ion Battery Oluwatosin Emmanuel Bankole1,2,*, Chunxia Gong1, Lixu Lei1 1School of Chemistry and Chemical Engineering, Southeast University, Nanjing 211189, China 2Department of Chemistry, College of Natural Science, Crawford University, P.M .B 2001, Atan-Agbara Road, O gun State, Nigeria Abstract The electrochemical performance of as-recovered LiNi1/3Co1/3Mn1/3O2 containing varying percentage weights of MoS2 and effect of preparing the powder obtained with dimethyl sulfo xide (DM SO) was investigated. All the powders were calcined at 650 oC. The SEM images and XRD patterns analysis showed that the powders have well-crystallized particles. Fro m the results, highest electrochemical performance was recorded for powder with 0.4 wt. % MoS2. Samp le pressed before fabrication delivered discharge capacity of 201 mAhg-1 in the first cycle before sudden drop to 172 mAhg-1 in the second cycle at a discharge rate of 0.1 C (27.5 mAg-1). After t wenty cycles, it delivered 146 mAhg-1 with efficiency ratio of 96.6%. For samp le fabricated without pressing the slurry after drying, the capacities delivered revealed similar trends as recorded in pressed slurries. Highest charge-transfer resistance was recorded for powder with 0.4 wt. % MoS2 during AC impedance analysis. The performance recorded revealed that relatively cheap and environmentally co mpatible DMSO could replace N-methylpyrro lidone in lithiu m-ion battery formulat ion. Keywords Recycled LiNi1/3Co1/3Mn1/3O2, MoS2, Dimethyl Sulfo xide, Electrochemical Performance, Lithiu m-ion Battery 1. Introduction Mo lybd en ite (Mo S2) wh ich h as d ist inct merits ov er traditional silicon and even graphene used in electronic has been uncovered by researchers as having many applicat ions. However, study on its applications in electronic has not been exp loit as a sign of oversight with the recent researches revealing its potential as a very effective semiconductor[1]. The various ap p licat ions o f Mo S2 in clu de so lid state lubrication[2], catalysis[3-6], hydrogen storage[7] and as an anode[8-11] o r cathode material fo r lithiu m-ion batteries because of the free energy o f lith iat ion and the vo ltage profile. However, energy density fro m its cathodes has been considered limited due to its relatively low average voltage (0.01 V o r 0.02 V)[12-18]. Feng et al inv estigated the preparation and application of MoS2 as a promising anode material exhib iting h igher specific capacity with very high cycling stability over a wide voltage range. After 20 cycles, the reversible capacity remained 840 mAh/g (84% o f the initial reversible capacity) for lithiu m-ion battery[8]. Zhang et al also p repared M o S2 ano de and so lid elect ro ly te * Corresponding author: bantosinemma@yahoo.co.uk (Oluwatosin Emmanuel Bankole) Published online at https://www.eduzhai.net Copyright © 2013 Scientific & Academic Publishing. All Rights Reserved polyvinylidene fluoride (PVDF) for three-d imensional lithiu m-ion microbattery in silicon MCP and recorded better initial charge-discharge performance capacity of MoS2[9]. The use of MoS2 and Pt as anode catalyst in H2S-O2 fuel was investigated at 800 oC[10]. The MoS2/ G co mposite with Mo: C (mo lar rat io of 1:2) used as higher performance anode materials in lith iu m-ion battery delivered the highest specific capacity of about 1100mAh/g at a cu rrent of 100 mA/g with an excellent cycling stability and high rate capability. The electrochemical performance recorded was attributed to the robust composite and synergistic effect between the layered MoS2 and graphene[11]. As a cathode, Wu et al prepared and tested FeF3/MoS2 with in itial discharge capacity of about 170 mAhg-1 in the voltage range 2.0-4.5 V at roo m temperature and charge-discharge rate of 0.1 C. The capacity retention was 83.1% after 30 cycles[13]. Liang et al used graphene-like MoS2 cathode and ultra small Mg nanoparticle anode in a rechargeable Mg battery. The Mg storage capacity of MoS2 single layer was about 223 mAhg − 1[14]. Preparat ion of MoS2 cathode in three-dimensional lithiu m-ion microbattery in silicon MCP has also been investigated[15]. Julien also investigated the disordered MoS2 as a cathode material in lith iu m-ion battery[16]. Miki et al synthesized amorphous MoS2 (a-MoS2) as a cathode materia l by therma l decomposition of (NH4)2MoS4 in hydrogen gas flow at 86 Oluwatosin Emmanuel Bankole et al.: Electrochemical Performance of Recycled LiM n1/3Ni1/3Co1/3O2 Reacted with M olybdenite in Lithium-ion Battery temperatures fro m 150 to 300 oC. The discharge-charge cycling measurements revealed that sample prepared at 150°C showed the highest cycle capacity (100 Ah/kg) in the 100th cycle[17]. In this study, we report the electrochemical performance of reacting as-recovered LiMn1/3Ni1/3Co1/3O2 with varying ratios of MoS2 and preparation of the powders with dimethyl sulfoxide (DMSO) as a solvent instead of N-methylpyrro lid one. 2. Experiment 2.1. Separation of Electrode Materials The cylindrical lo w quality LiBs used in this study were provided by a company in China, wh ich used LiNi1/3Mn1/3Co1/3O2 and carbon on Al and Cu fo ils as the positive and negative electrodes respectively. The flo w-sheet for the experimental procedures used for the separation of cathode active materials fro m the alu min iu m fo ils is shown in Figure 1. 2.3. XRD and Electrochemical Anal ysis of the Samples The powder X-ray diffraction characterization was carried out by a Bruker-A XS, X-ray diffracto meter D8 with Cu Kα radiation with a g raphite monochromator and Cu Kα1 radiation operated at 5~90° and 0.015 °/s. The electrochemical characterization of the powder was performed using a CR2032 coin cell. The cathode fabrication was prepared by mixing thoroughly the mixtu re of 85 % of MoS2 /LiNi1/3Co1/3Mn1/3O2, 10 % of acetylene b lack, 5 % polyvinylidene fluoride (PVDF) with one drop of dimethyl sulfoxide (Lingpeng ≥ 99.0%) instead of NMP until homogeneous slurry was obtained. The blended slurries were pasted onto aluminiu m co in current collectors, and the electrode was dried at 100 o C fo r 12 h in vacuu m and then pressed at 10 MPa before assembling the cells in a dry argon-filled glove box for cell testing. The test cell consists of the cathode prepared, lith iu m metal anode and Cellgard 2300 film as the separator and the solution of electrolytes consisting of 1 M LiPF6 dissolved in ratio 1:1 (v/v) mixtu re of dimethyl carbonate (DMC) and ethylene carbonate (EC). Capacity measurements and cycling tests of the coin-type cells were performed in LA ND2001CT battery cycler over a voltage range 2-4.5 V at current density 0.2 mA and 0.1 C rate (27.5 mAg-1) at room temperature. 3. Results and Discussions 3.1. XRD and Lattice Parameters Figure 2 shows the XRD patterns of the powder obtained fro m the extractions after calcined at 650 oC for 10 h. Except for the sample obtained fro m 1.2 wt % MoS2, it is ev ident that all the patterns are similar to the standard patterns of LiNi1/3Co1/3Mn1/3O2 obtained from the software used for comparison. Samp le with 1.2 wt % MoS2 shows the difference with small peak d iffraction at 14.36 degree which corresponds to the high peak for the pure samp le of MoS2 reacted with LiNi1/3Co1/3Mn1/3O2 recovered. This shows that the sample contains traces of MoS2. Figure 1. Flow-sheet for the recycling and preparation of MoS2-LiNi1/3Mn1/3Co1/3O2 powders 2.2. Pre par ati on of MoS2/ Li Mn1/3Ni1/3Co1/3O2 The preparation of the MoS2-LiNi1/3Co1/3Mn1/3O2 was done by mechano-thermal technique[18]. The d ispersion of nanoparticles of MoS2 in 50 cm3 ethanol (Yazheng ≤ 95%) was done for 1 h by sonication (KH-50B) fo llo wed by addition of dried LiNi1/3Co1/3Mn1/3O2 to dispersed MoS2 at varying weight rat ios of 99.80:0.20, 99.60:0.40, 99.20:0.80 and 98.80:1.20 respectively and then sonicated for 1 h. The mixtu re was heated to boiling for 2 h 30mins before filtration. The powder obtained was then dried at 60 oC fo llo wed by sintering at 650 oC for 10 h. The powder obtained was then characterized by X-ray diffraction (XRD). Figure 2. X-ray diffraction patterns of as-recovered LiNi1/3Co1/3Mn1/3O2 containing varying percentage weights of MoS2 calcined at 650 oC for 10 h and pure MoS2. The pattern marked ‘x’ is the LiNi1/3Co1/3Mn1/3O2 standard from the PDF number 87-1561 of the crystallographic search-match so ft ware International Journal of M aterials and Chemistry 2013, 3(5): 85-90 87 Table 1 shows the lattice parameters indexed on cells of α-NaFeO2 type hexagonal structure with a space group of R-3M fro m the XRD patterns (Figure 2). It is ev ident that samples M1, M 2, M3 and M4 for powders reacted with 0.2, 0.4, 0.8 and 1.2 wt % MoS2 respectively have the same patterns in spite of the appearance of sma ll pea k for powder labelled “M4” as mentioned above. The c/a ratios of the powders are around 4.96, which co mply with the value preferred for the material having well-defined hexagonal layered characteristics[19, 20]. Samp le M 4 has the smallest particle sizes followed by M1, wh ile M2 has the largest particle sizes. The particle sizes were calcu lated by Scherrer equation according to the peak at about 19°. Table 1. Latt ice paramet ers of the powders cont aining MoS2 Sample a (Å) M1 2.886 M2 2.888 M3 2.881 M4 2.875 c (Å) 14.30 14.30 14.31 14.29 c/a 4.960 4.952 4.967 4.970 Particle size (nm) 64.30 66.80 65.70 64.20 3.2. Electrochemical Performance of the Powders Containing wi th MoS2 cycle at the same rate. However, the value delivered in sixth cycle is still lower than that of sample reacted with 1.2 wt % MoS2. Apart from poor electrical contact during charging, the sudden drop in capacities fro m the third to the tenth cycles could be attributed to the loss of active materials and parasitic side reactions occurring during charging processes, specifically deposition of LiF[21, 22]. All other powders obtained do not exh ibit good rate capacities during cycle tests despite being the same. 3.3. XRD Analysis of New Powders with MoS2 Figure 4 shows the XRD patterns of the new powders obtained after calcined at 650 o C for 10 h. It is ev ident that all the patterns are similar to the initial patterns obtained in Figure 2 above. The lattice parameters shown in Table 2 were also indexed on cells of α-NaFeO2 type hexagonal structure with a space group of R-3M fro m the XRD patterns as in Table 1. Table 2 shows that the c/a ratios of the powders still remain 4.96 as obtained in the first set of samples (Tab le 1) for material having well-defined hexagonal layered characteristics[19, 20]. A mongst all the samples, powder reacted with 0.8 wt. % MoS2 labelled M 33 has the smallest particles size of about 66.0 n m, wh ile powder reacted with 0.2 wt. % MoS2 (M11) has the largest value of 71.30 n m. Figure 3. Discharge-capacity vs cycle number plots of 0.4, 0.8 and 1.2 wt. % MoS2 calcined at 650 oC, prepared with DMSO and charged with the voltage range 2.5-4.5V at current density of 0.2mA at the rate of 0.1 C (27.5 mAg-1) Figure 4. X-ray diffraction patterns of new LiNi1/3Co1/3Mn1/3O2 with (a) 0.2 (b) 0.4 (c) 0.8 wt. % MoS2 calcined at 650 oC for 10 h and labelled as M11, M22 and M33 respectively. Figure 3 shows the electrochemical performance of the powders obtained after sintering LiNi1/3Co1/3Mn1/3O2 reacted with various percentage weights of MoS2 at 650 oC fo r 10 h. Among all the powders prepared, the powder reacted with 0.4 wt. % MoS2 has the highest cyclic conductivity. It delivers discharge capacity of 201 in the first cycle befo re undergoing sudden drop to deliver capacity of about 172 mAhg-1 in the second cycle at a discharge rate of 0.1C. After the twenty cycles, it delivers 146 mAhg-1 with efficiency ratio of 96.6%. Samp le reacted with 1.2 wt % MoS2 undergoes rise in discharge capacity from 131 to 156 mAhg-1 and almost maintains the capacities discharged without significant capacity fading. The capacity delivered by sample reacted with 0.8 wt % MoS2 also rises from 142 mAhg-1 in the first cycle to about 147 mAhg-1 in the sixth Table 2. Lattice parameters of the powders different new powders containing MoS2 Sample a (Å) c (Å) c/a Particle size (nm) M11 2.888 M22 2.880 M33 2.883 14.30 14.28 14.31 4.952 4.960 4.964 71.30 66.10 66.00 3.4. Structure and Morpholog y Analysis of New Powders wi th MoS2 Figure 5 shows the morphologies and particle sizes of the all three powders. The larger aggregate particles are composed of smaller particles with the size of 100~200 n m. The images show that all the powders consist of 88 Oluwatosin Emmanuel Bankole et al.: Electrochemical Performance of Recycled LiM n1/3Ni1/3Co1/3O2 Reacted with M olybdenite in Lithium-ion Battery well-crystallized particles. In co mparison, sample ‘b2’ has the smallest particles size on the larger aggregate particles. Although sample M 33 has the smallest particle size of the all powders (Table 2), the larger aggregate spherical part icles of b3 shows that sample with 0.4 wt % MoS2 is the most homogeneous as evident in the image. The difference in particle sizes observed in all the samples could be attributed to varying percentage weight of MoS2 used in the as-recovered LiNi1/3Co1/3Mn1/3O2. discharge capacities of about 126 mAhg-1 in the first-fifth cycles at a discharge rate of 0.1 C (27.5 mAg-1) and 114 mAhg-1 in seven-eleventh cycles at a discharge rate of 0.2 C (55 mAg-1) with corresponding efficiency rat ios of about 94 and 98 % respectively. This electrochemical performance can be attributed to the homogeneous particles appearance of b3 (Figure 5). According to reports, uniform part icles contribution of cathode materials causes uniform depth of charge (DOC) of each particle, wh ich increases the utilizat ion of the material to enhance the overall battery performance[23, 24]. Samp le with 0.8 wt % MoS2 delivers the lowest capacities. In comparison with the capacities delivered by the sa mples whose slurries were pressed (Figure 3), fabricat ion without pressing the slurry has no significant effects on the performance of the battery if we ll prepared. Figure 5. SEM micrographs at different magnifications for as-recovered LiNi1/3Co1/3Mn1/3O2 reacted with (a) 0.2 (b) 0.4 (c) 0.8 wt. % MoS2 calcined at 650 oC for 10 h 3.5. Electrochemical Anal ysis of the Powders Fabricated wi thout Pressing 3.6. Cyclic Voltammetry Performance of LiNi1/3Co1/3Mn1/3O2 Contai ning MoS2 Figure 7 shows the cyclic voltammogram of the as-recovered LiNi1/3Co1/3Mn1/3O2 containing varying percentages weights of MoS2 conducted at scan rate of 1 mVs−1 in 1 M LiPF6 dissolved in ratio 1:1 (v/v) mixture of dimethyl carbonate and ethylene carbonate as electrolyte mixtu re against Li metal as counter and reference electrodes. It is evident that the cyclic voltammograms measurement shows no reversible lithiation and de-lithiat ion processes of a typical LiNi1/3Co1/3Mn1/3O2 reported[25]. The presence of MoS2 could affect the structure of the electrode materials reported by Luo et al, making it difficu lt for the lith iu m ion to reversibly intercalate into a lithiu m-accepting anode and deintercalate fro m a cathode active material during the processes[26]. A ll the samples show only cathodic peaks. It shows that the lithiathion at the cathode during discharging processes occurs easily during the analysis. A mongst all the samples, sample with 0.2 wt % MoS2 shows the highest cathodic peak at 3.51 V. Figure 6. Discharge-capacity vs cycle number plots of 0.2, 0.4 and 0.8 wt. % MoS2 calcined at 650 oC, prepared with DMSO and charged with the voltage range 2.5-4.5V between 0.12-1.2 mA at different rates Figure 6 shows the electrochemical performance of LiNi1/3Co1/3Mn1/3O2 powder reacted with varying weights percentage of MoS2 and fabricated without pressing the slurry after drying at 100 oC. Similar to the electrochemical performance shown in Figure 3, the powder with 0.4 wt. % MoS2 has the highest cyclic conductivity. It delivers average Fi gure 7. Current vs potent ial plot s of LiNi1/3Co1/3Mn1/3O2 cont aining 0.2, 0.4 and 0.8 wt % MoS2 calcined at 650 oC for 10 h 3.7. Electrochemical Impedance Analysis Figure 8 shows the Nyquist plots of as-recovered LiNi1/3Co1/3Mn1/3O2 containing varying percentage weights International Journal of M aterials and Chemistry 2013, 3(5): 85-90 89 of MoS2 tested between the frequency ranges from 100 kHz to 0.1 Hz. Similar electrochemical impedance spectroscopy (EIS) patterns were observed for all three samples system. AC impedance is a strong function of state-of-charge. The spectra consist of one semicircle each in higher frequency region related to a charge-transfer assigned to the ionic condition in the Li+ electrolyte film as well as its migration through the interface between the surface layer of the particles and the electrolyte [27, 28]. The low frequency tails resulted fro m the d iffusion of lithiu m ions in the bulk active mass. Also, except for samp le with 0.2 wt.% MoS2 which has a distorted tail, both samples with 0.4 and 0.8 wt.% MoS2 have a nearly 45o line in the complex-plane impedance plot ascribed to a Warburg region of semi-infinite diffusion of species in the modified electrode[29]. Although it is ev ident that the total impedance of the battery with 0.8 wt. % MoS2 is largest, powder with 0.4 wt. % MoS2 has greatest charge-transfer resistances considering its spectrum. Charge transfer resistance shows a greater dependence on the Li+ ion intercalation and deintercalation levels, which influences the electrochemical conductivity and improve the Li+ kinetic behavior. Thus, as observed in Figure 6 above, powder with 0.4 wt. % MoS2 has the highest Li+ ion migration through the interface between the surface layers. This contributes to its highest discharge capacities. the first cycle before sudden drop to deliver capacity of 172 mAhg-1 in the second cycle at a discharge rate of 0.1 C (27.5 mAg-1). After the twenty cycles, it delivered 146 mAhg-1 with efficiency ratio of about 97 %. The capacity delivered by sample with 1.2 wt % MoS2 rose from about 131 to 156 mAhg-1 at the same rate. For samp le fabricated without pressing the slurry, the capacities delivered revealed similar trends as in pressed slurry. Sample with 0.4 wt. % MoS2 delivered the h ighest capacity of about 127 mAhg-1 in first-fifth cycles at the same rate of 0.1 C (27.5 mAg-1), wh ile sample with 0.8 wt % MoS2 has the least discharge capacities. The sudden drop in capacities observed can be attributed to loss of active materials due to parasitic side react ions of LiF according to reports. All the powders obtained do not exh ibit good rate capacities during cyclic tests. However, the electrochemical performances and the AC impedance analysis for the first set of samples prepared show that DMSO that is considered relatively cheaper and environmentally co mpatible than NMP could be used instead of the latter solvent (NMP) in battery formu lation. ACKNOWLEDGMENTS We appreciate the company that supplied the lith iu m-ion batteries used for the study. The support received from the School of Chemistry and Chemical Eng ineering, Southeast University, China is gratefully acknowledged. 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