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Synthesis and Study of Zirconium Doped Lithium Titanate Ceramics
Available online at www.sciencedirect.com
ScienceDirect Materials Today: Proceedings 18 (2019) 1459–1464
www.materialstoday.com/proceedings
ICN3I-2017
Synthesis And Study of Zirconium Doped Lithium Titanate Ceramics
Neha Balaa, Swati Raaj, Deep Shikha Kumaria, Firdaus Alia, Anjali Singha, P.Koura, & S.K. Sinhaa a
Department of Physics, Birla Institute of Technology, P.O:B.V. College, Patna, India-800014
Abstract Lithium titanate has been used as anode materials for litium batteries. Lithium titanate with stoichiometric formula (Li4Ti5O12) was prepared by the solid state method followed by sintering of the material. Lithium oxide (Li2O) and Titanium Oxide (TiO2) were taken as a base material to prepare the sample. The anode materials should have better ionic mobility. To enhance the ionic mobility of Lithium Titanate, Zr+4 is incorporated in the titanum site of Lithium Titanate. Incorporated Zr+4 with stoichiometries formula Li4Ti5-xAxO12, with x = 0.1, 0.2 and 0.3 weight percent respectively was prepared. Differential thermal analyses (DTA) of the prepared green sample had shown that the reaction completes at around 500°C. Thus, calcinations of the sample was done at temperatures greater than 500°C for an hour to get the proper phase of Lithium Titanate. X-ray diffraction (XRD) of the pure sample was carried out. Monoclinic phase was found in the material . Crystallite size was found in nm. Pellets were sintered at varying temperature rang e.g. 900°C, 950°C, 1000°C, 1050°C and 1100°C with soaking time of one hour. The measurement of mobility of charge carrier was measured using impedance analyser. The electrical properties of the sample were correlated with microstructure. Scanning Electron Microscopy (SEM) of the sintered sample shown the clear grain and grain boundaries with grains are in μm size. Frequency dependent resistance of Li4Ti5-xZrxO12, where x= 0.1, 0.2 & 0.3 weight percent has been studied. © 2019 Elsevier Ltd. All rights reserved. Selection and/or Peer-review under responsibility of International Conference on Nanotechnology: Ideas, Innovations & Initiatives-2017 (ICN:3i2017). Keywords: Lithium titanate, DTA; TGA; XRD
1. Introduction The storage of electrical energy has become far more important at the present time than it was in the earlier. Lithium ion battery is found to have good potential in meeting this objective [1-2]. Whether to supply power the portable consumer electronic devices (cell phones, PDAs, laptops, or for implantable medical applications, such as artificial 2214-7853 © 2019 Elsevier Ltd. All rights reserved. Selection and/or Peer-review under responsibility of International Conference on Nanotechnology: Ideas, Innovations & Initiatives-2017 (ICN:3i2017).
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hearts, or to address global warming (hybrid electric vehicles, storage of wind/solar power), the need for clean and efficient energy storage will be need of time. Nanomaterials have vast potential to play in achieving this change in the way we store energy. Rechargeable lithium batteries have revolutionized handy electronic devices. They have become the dominant power source for cell phones, digital cameras, laptops, etc., because of their superior energy density (capability to store 2– 3 times the energy per unit weight and volume compared with conventional rechargeable batteries). This technology may be useful for future hybrid electric vehicles, which are central to the reduction of CO2 emissions arising from transportation. The rechargeable lithium battery does not contain lithium metal. It is a lithium-ion device, comprising a graphite negative electrode (anode), a non-aqueous liquid electrolyte, and a positive electrode (cathode) formed from layered LiCoO2. On charging, lithium ions start emitting from the layered LiCoO2 pass across the electrolyte, and are intercalated between the graphite layers in the anode. Discharge reverses this process. The electrons, of course, pass around the external circuit. Lithium titanate (Li4Ti5O12) is a material for battery applications in automotive vehicles due to its long lifetime and its suggested zero-strain ability. The zero-strain ability, meaning no volume changes in the material during cycling, would allow for the high charge/discharge rates required in electric vehicles. [3-5] The rechargeable lithium battery is a supreme representation of solid-state chemistry in action. The first-generation lithium-ion battery has electrodes that are composed of powders containing millimetre-sized particles, and the electrolyte is trapped within the millimeter sized pores of a polypropylene separator. This battery has a high energy density, but it is a low-power device (slow charge/discharge). This slow action limitation exists because of the intrinsic diffusivity of the lithium ion in the solid state (e.g. 10 -8 cm2 s-1), which limits the rate of intercalation/deintercalation, and hence results in slow charge/ discharge. However, an increase in the charge/discharge rate of lithium-ion batteries of more than one order of magnitude is required to meet the future demands of hybrid electric vehicles and clean energy storage [6-9]. To enhance the electrical conductivity of Li4Ti5O12, dope with other metal ions [10-11]. Various metal ions were employed to doped at Li+ or Ti4+ side to improve the electronic conductivity [12-14]. In the present work for better ionic mobility in Lithium Titanate anode Zr+4 in varying concentrations were incorporated in the lattice site of Lithium Titanate. Incorporation of Zr+4 was done based on the following stoichiometry formula; Li4Ti5-xAxO12, where A (Zr+4) represents the dopant having x = 0.1, 0.2 and 0.3 weight percent respectively. The method for preparation of the material was by solid state reaction method [15-16]. Impedance analyzer was used to measure the change in resistance at different frequency ranges for prepared sample to judge the suitability as cathode material of lithium cell. The objective of this work is to study the effect of Zr+4 ion doping of Lithium Titanate on microstructure and electrical properties such as grain size and impedance. A further objective of this work is to enhance the Li-ion mobility by decreasing its resistance at a frequency of 50Hz. 2. Experimental Base chemicals taken for preparation of lithium titanate (LT) ceramic cathode were Li2O (AR grade Loba Chemi), Ti2O (AR grade Loba Chemi) and ZrO2 (AR Grade Loba Chemi). Chemicals were taken as per stoichiometries formula Li4Ti5-xZrxO12, where x= 0.1, 0.2 & 0.3 weight percent. Flow chart for preparation of material is shown in Fig.1.Chemicals in powder form were mixed in a ball miller for an hour for better mixing. Differential Thermal analysis (DTA) characterization of green powder was done to know the thermal changes in powder as well as to determine the calcinations temperature. Mixed powder were calcined at 800oC for one hour in a muffle furnace in an air environment to get the proper phase of LT. Calcined powder was tested for phase analysis by using X-ray diffractometer (Philips make). Particle size calculation of the prepared material was carried out by using Scherer’s formula [17]. Small pellets of calcined powder of 10 mm diameter were made by applying a pressure of 2.5 ton in a cold press. Pellets were further sintered at 11000 C for two hours for optimum densification. For testing of the suitability of prepared materials as a cathode of lithium battery cell, frequency Vs resistance Z was tested for sintered pellets by using an impedance analyzer. Scanning Electron Microscopy test of sintered pellet was carried out to obtain the grain size of prepared material at a particular sintering temperature.
N. Bala et al. / Materials Today: Proceedings 18 (2019) 1459–1464
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Fig.1 Flow chart for preparation and characterization of LT by solid state reaction method 3. Result and Discussion 3.1 DTA Analysis
Thermal Analysis Result
TGA % 100.00
DSC3.tad
TGA
80.00
60.00
40.00 0.00
200.00
400.00
600.00 Temp [C]
800.00
1000.00
Fig.2: Differential Thermal Analysis (DTA) micrograph of green Li4Ti5O12 (LT) Differential Thermal Analysis (DTA) micrograph of green prepared powder of Li4Ti5O12 (LT) is shown in Fig.2. Major exothermic peaks were observed in 220oC and 280o C. These are the indication of release of present volatile impurities in the prepared sample. DTA micrograph also indicates about completion of solid state reaction at 510o C.
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N. Bala et al. / Materials Today: Proceedings 18 (2019) 1459–1464
It means the phase of LT is achieved at 510o C. After this particular temperature no exothermic or endothermic reaction was observed in the DTA micrograph [18]. 3.2 XRD Analysis
Fig 3: X-ray diffraction analysis test micrograph for Li4Ti5O12 calcined at 800O C X-Ray Diffraction test report (XRD) of calcined powder of Li4Ti5O12 (LT) is displayed as fig 3. Different intensity peaks were observed at 2θ values at 37.50 (FWHM β: 0.1994), 43.56 (FWHM β: 0.1865), 63.36 (FWHM β: 0.1270) and 63.54 (FWHM β: 0.0772). These peaks indicate presence of monoclinic phase in prepared LT. This confirms the formation of Li4Ti5O12 as reported in other works [19]. Crystallite size analysis was done by using Scherer‘s formula as given below-
With k ~ 0.89, β is full width at half maximum (FWHM). The average crystallite size was found in nm range. 3.3 Impedance analysis Measurement of resistance at varying frequency of unmodified Li4Ti5O12 ceramics and modified with Zr ions at different weight percent is shown in Fig.4. It was observed that resistance decreases with the incorporation of Zr+4 ions in the lattice site of Li4Ti5O12. It was found from the graph that with increase in frequency, the resistance increases and the maximum resistance were observed at 1000 Hz and then it started decreasing with further increases of frequency. Maximum decrease in resistance in prepared material was observed in the case of 0.2 weight percent of Zr- ion. Lowering of resistance due to incorporation of Zr–ion in lattice site of LT indicates better Li-ion mobility during the electrolytic reaction. As a result the performing capacity of Li ion cell will be enhanced [20]. There was a decrease of 28% in resistance observed in the ambient frequency range of 50 Hz in the case of 0.2 weight percent of Zr – ion [21-22].
N. Bala et al. / Materials Today: Proceedings 18 (2019) 1459–1464
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Fig 4: Variation of Resistance (ohm) with Frequency (Hz) for Li4-xZr xTi5O12, where X= 0.0, 0.1, 0.2 & 0.3 weight percent 3.4 SEM Analysis
Fig.5: SEM micrograph of 0.2 weight percent doped Li4Ti5O12 sintered at 11000 C Scanning electron microscopy (SEM) micrograph of 0.2 weight percent incorporated Li4Ti5O12 is shown in Fig.5. Spherical distinct grains can be clearly observed in the micrograph. The average grain size was observed as 10μm. Small pore channels can also be observed in the micrograph. This pores or channel formation was due to grain boundary strain due to Zr incorporation in lattice site [23]. This pore helps in increase in Li mobility during the electrolysis reaction of lithium battery.
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4. Conclusion Lithium Titanate anode material Li4Ti5O12 incorporated with Zr-ion at varying weight percent was successfully prepared by the solid state reaction method. Presence of monoclinic phase was observed in prepared material.. Crystallaite size are found nm range. DTA test results reveal low calcination temperature in the prepared Li cathode i.e. 500 degree centigrade. SEM test had clearly shown spherical grains having average size 10μm. Impedance analysis of prepared material was shown that 0.2 weight % doping of Zr-ion in Li4Ti5O12 is most appropriate as it results in a decrease of the cathode resistance by 28 %. References [1]. [2]. [3]. [4]. [5]. [6]. [7]. [8]. [9]. [10]. [11]. [12]. [13]. [14]. [15]. [16]. [17]. [18]. [19]. [20]. [21]. [22]. [23].
R. Yuan, Cai, P. Gu,Z. Shao, J. of Power Sources 195(2010)2883-2887. L. Zhao, Y.S. Hu, H. Li, Z. Wang, L. Chen, Adv. Mat. 23(2011)1385-1388. M.M. Rahman, J.-Z.Wang, M. F.Hassan, D.Wexler, and H. K.Liu, Adv. Energy Mat.l(2011)212-220. Y. Wang, H. Liu, K. Wang, H. Eiji, Y. Wang, H. Zhou,J. of Mat. Chem.19(2009)6789. K. Amine, I. Belharouak, Z. Chen et al., Adv.Mat. 22(2010)3052-3057 S.Goriparti,E.Miele,F.De Angelis,E.Di Fabrizio,R.P.Zaccaria,C.Capiglia,J.Pow.Sources 257(2014) 421-443 A.V. Chadwick, M. J. Pooley and S. L. P. Savin Physica. Status Solidi 2(2015) 302-305 J. Lee, O. Nam, B.H. Cho,J. Power Sources, 174(2007)1-348 S.Arico,P. Bruce, B.Scrosati,J.M. Tarascon,V.Schalkwijk,Nat.Mater 4(2005) 366-77. X.Li,M.Qu,Z.Yu,J. of Alloys and Comp. 487(2009)13 J. Wolfenstine and J. L. Allen, J. of PowerSources, 180(2008) 582–585. S. Huang, Z. Wen, X. Zhu, and Z. Lin, J. of PowerSources1(2007). 408–412. A. D. Robertson, L. Trevino, H. Tukamoto, and J. T. S. Irvine, J. of PowerSources1Sources, 81(1999)352–357. S. Shi, C. Ouyang, M. Lei, and W. Tang, Journal of Power Sources 171(2007) 908–912. P. Kubiak, A. Garcia, M.Womes et al., Journal of Power Sources, 119–121(2003) 626–630. Y.Lu,M.Pang,S.Shi,Q.Ye,Z Tian,T Wang, NCBI Literature,8(2014) 2981 P. Kour, Pawan Kumar, S. K. Sinha, Manoranjan Kar, Solid StateCommunications 190(2014) 33–39. I. A. Leonidov,O. N. Leonidova,L. A. Perelyaeva, R. F. Samigullina,S. A. Kovyazina,M. V. Patrakeev, Physics of the Solid State 45 (2003)2183-2188. Z.Wang,H.Xie, G.Guowei, Lijun. J.of Nanomaterials(2012). 10.1155/2012/876197. D.Juarez-Robles,C.Chen,Y.Barsukov,P.Partha,Mukherjee,.J.of the electro.soc.164(2007)A837-A847. L.Wang,Z Wang,Q.Ju,We Wang,Z.Wang,,The 8th International Conference on Applied Energy- ICAE(2016) 4444- 4449 N.Bala, S.K.Sinha, International Journal of Interdisciplinary Research Centre (IJIRC) 1(2016), ISSN: 2455-2275(E) B.Scrosati,J.Garche,J.Power Sorces195(2005)2419-2430
ScienceDirect Materials Today: Proceedings 18 (2019) 1459–1464
www.materialstoday.com/proceedings
ICN3I-2017
Synthesis And Study of Zirconium Doped Lithium Titanate Ceramics
Neha Balaa, Swati Raaj, Deep Shikha Kumaria, Firdaus Alia, Anjali Singha, P.Koura, & S.K. Sinhaa a
Department of Physics, Birla Institute of Technology, P.O:B.V. College, Patna, India-800014
Abstract Lithium titanate has been used as anode materials for litium batteries. Lithium titanate with stoichiometric formula (Li4Ti5O12) was prepared by the solid state method followed by sintering of the material. Lithium oxide (Li2O) and Titanium Oxide (TiO2) were taken as a base material to prepare the sample. The anode materials should have better ionic mobility. To enhance the ionic mobility of Lithium Titanate, Zr+4 is incorporated in the titanum site of Lithium Titanate. Incorporated Zr+4 with stoichiometries formula Li4Ti5-xAxO12, with x = 0.1, 0.2 and 0.3 weight percent respectively was prepared. Differential thermal analyses (DTA) of the prepared green sample had shown that the reaction completes at around 500°C. Thus, calcinations of the sample was done at temperatures greater than 500°C for an hour to get the proper phase of Lithium Titanate. X-ray diffraction (XRD) of the pure sample was carried out. Monoclinic phase was found in the material . Crystallite size was found in nm. Pellets were sintered at varying temperature rang e.g. 900°C, 950°C, 1000°C, 1050°C and 1100°C with soaking time of one hour. The measurement of mobility of charge carrier was measured using impedance analyser. The electrical properties of the sample were correlated with microstructure. Scanning Electron Microscopy (SEM) of the sintered sample shown the clear grain and grain boundaries with grains are in μm size. Frequency dependent resistance of Li4Ti5-xZrxO12, where x= 0.1, 0.2 & 0.3 weight percent has been studied. © 2019 Elsevier Ltd. All rights reserved. Selection and/or Peer-review under responsibility of International Conference on Nanotechnology: Ideas, Innovations & Initiatives-2017 (ICN:3i2017). Keywords: Lithium titanate, DTA; TGA; XRD
1. Introduction The storage of electrical energy has become far more important at the present time than it was in the earlier. Lithium ion battery is found to have good potential in meeting this objective [1-2]. Whether to supply power the portable consumer electronic devices (cell phones, PDAs, laptops, or for implantable medical applications, such as artificial 2214-7853 © 2019 Elsevier Ltd. All rights reserved. Selection and/or Peer-review under responsibility of International Conference on Nanotechnology: Ideas, Innovations & Initiatives-2017 (ICN:3i2017).
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N. Bala et al. / Materials Today: Proceedings 18 (2019) 1459–1464
hearts, or to address global warming (hybrid electric vehicles, storage of wind/solar power), the need for clean and efficient energy storage will be need of time. Nanomaterials have vast potential to play in achieving this change in the way we store energy. Rechargeable lithium batteries have revolutionized handy electronic devices. They have become the dominant power source for cell phones, digital cameras, laptops, etc., because of their superior energy density (capability to store 2– 3 times the energy per unit weight and volume compared with conventional rechargeable batteries). This technology may be useful for future hybrid electric vehicles, which are central to the reduction of CO2 emissions arising from transportation. The rechargeable lithium battery does not contain lithium metal. It is a lithium-ion device, comprising a graphite negative electrode (anode), a non-aqueous liquid electrolyte, and a positive electrode (cathode) formed from layered LiCoO2. On charging, lithium ions start emitting from the layered LiCoO2 pass across the electrolyte, and are intercalated between the graphite layers in the anode. Discharge reverses this process. The electrons, of course, pass around the external circuit. Lithium titanate (Li4Ti5O12) is a material for battery applications in automotive vehicles due to its long lifetime and its suggested zero-strain ability. The zero-strain ability, meaning no volume changes in the material during cycling, would allow for the high charge/discharge rates required in electric vehicles. [3-5] The rechargeable lithium battery is a supreme representation of solid-state chemistry in action. The first-generation lithium-ion battery has electrodes that are composed of powders containing millimetre-sized particles, and the electrolyte is trapped within the millimeter sized pores of a polypropylene separator. This battery has a high energy density, but it is a low-power device (slow charge/discharge). This slow action limitation exists because of the intrinsic diffusivity of the lithium ion in the solid state (e.g. 10 -8 cm2 s-1), which limits the rate of intercalation/deintercalation, and hence results in slow charge/ discharge. However, an increase in the charge/discharge rate of lithium-ion batteries of more than one order of magnitude is required to meet the future demands of hybrid electric vehicles and clean energy storage [6-9]. To enhance the electrical conductivity of Li4Ti5O12, dope with other metal ions [10-11]. Various metal ions were employed to doped at Li+ or Ti4+ side to improve the electronic conductivity [12-14]. In the present work for better ionic mobility in Lithium Titanate anode Zr+4 in varying concentrations were incorporated in the lattice site of Lithium Titanate. Incorporation of Zr+4 was done based on the following stoichiometry formula; Li4Ti5-xAxO12, where A (Zr+4) represents the dopant having x = 0.1, 0.2 and 0.3 weight percent respectively. The method for preparation of the material was by solid state reaction method [15-16]. Impedance analyzer was used to measure the change in resistance at different frequency ranges for prepared sample to judge the suitability as cathode material of lithium cell. The objective of this work is to study the effect of Zr+4 ion doping of Lithium Titanate on microstructure and electrical properties such as grain size and impedance. A further objective of this work is to enhance the Li-ion mobility by decreasing its resistance at a frequency of 50Hz. 2. Experimental Base chemicals taken for preparation of lithium titanate (LT) ceramic cathode were Li2O (AR grade Loba Chemi), Ti2O (AR grade Loba Chemi) and ZrO2 (AR Grade Loba Chemi). Chemicals were taken as per stoichiometries formula Li4Ti5-xZrxO12, where x= 0.1, 0.2 & 0.3 weight percent. Flow chart for preparation of material is shown in Fig.1.Chemicals in powder form were mixed in a ball miller for an hour for better mixing. Differential Thermal analysis (DTA) characterization of green powder was done to know the thermal changes in powder as well as to determine the calcinations temperature. Mixed powder were calcined at 800oC for one hour in a muffle furnace in an air environment to get the proper phase of LT. Calcined powder was tested for phase analysis by using X-ray diffractometer (Philips make). Particle size calculation of the prepared material was carried out by using Scherer’s formula [17]. Small pellets of calcined powder of 10 mm diameter were made by applying a pressure of 2.5 ton in a cold press. Pellets were further sintered at 11000 C for two hours for optimum densification. For testing of the suitability of prepared materials as a cathode of lithium battery cell, frequency Vs resistance Z was tested for sintered pellets by using an impedance analyzer. Scanning Electron Microscopy test of sintered pellet was carried out to obtain the grain size of prepared material at a particular sintering temperature.
N. Bala et al. / Materials Today: Proceedings 18 (2019) 1459–1464
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Fig.1 Flow chart for preparation and characterization of LT by solid state reaction method 3. Result and Discussion 3.1 DTA Analysis
Thermal Analysis Result
TGA % 100.00
DSC3.tad
TGA
80.00
60.00
40.00 0.00
200.00
400.00
600.00 Temp [C]
800.00
1000.00
Fig.2: Differential Thermal Analysis (DTA) micrograph of green Li4Ti5O12 (LT) Differential Thermal Analysis (DTA) micrograph of green prepared powder of Li4Ti5O12 (LT) is shown in Fig.2. Major exothermic peaks were observed in 220oC and 280o C. These are the indication of release of present volatile impurities in the prepared sample. DTA micrograph also indicates about completion of solid state reaction at 510o C.
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N. Bala et al. / Materials Today: Proceedings 18 (2019) 1459–1464
It means the phase of LT is achieved at 510o C. After this particular temperature no exothermic or endothermic reaction was observed in the DTA micrograph [18]. 3.2 XRD Analysis
Fig 3: X-ray diffraction analysis test micrograph for Li4Ti5O12 calcined at 800O C X-Ray Diffraction test report (XRD) of calcined powder of Li4Ti5O12 (LT) is displayed as fig 3. Different intensity peaks were observed at 2θ values at 37.50 (FWHM β: 0.1994), 43.56 (FWHM β: 0.1865), 63.36 (FWHM β: 0.1270) and 63.54 (FWHM β: 0.0772). These peaks indicate presence of monoclinic phase in prepared LT. This confirms the formation of Li4Ti5O12 as reported in other works [19]. Crystallite size analysis was done by using Scherer‘s formula as given below-
With k ~ 0.89, β is full width at half maximum (FWHM). The average crystallite size was found in nm range. 3.3 Impedance analysis Measurement of resistance at varying frequency of unmodified Li4Ti5O12 ceramics and modified with Zr ions at different weight percent is shown in Fig.4. It was observed that resistance decreases with the incorporation of Zr+4 ions in the lattice site of Li4Ti5O12. It was found from the graph that with increase in frequency, the resistance increases and the maximum resistance were observed at 1000 Hz and then it started decreasing with further increases of frequency. Maximum decrease in resistance in prepared material was observed in the case of 0.2 weight percent of Zr- ion. Lowering of resistance due to incorporation of Zr–ion in lattice site of LT indicates better Li-ion mobility during the electrolytic reaction. As a result the performing capacity of Li ion cell will be enhanced [20]. There was a decrease of 28% in resistance observed in the ambient frequency range of 50 Hz in the case of 0.2 weight percent of Zr – ion [21-22].
N. Bala et al. / Materials Today: Proceedings 18 (2019) 1459–1464
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Fig 4: Variation of Resistance (ohm) with Frequency (Hz) for Li4-xZr xTi5O12, where X= 0.0, 0.1, 0.2 & 0.3 weight percent 3.4 SEM Analysis
Fig.5: SEM micrograph of 0.2 weight percent doped Li4Ti5O12 sintered at 11000 C Scanning electron microscopy (SEM) micrograph of 0.2 weight percent incorporated Li4Ti5O12 is shown in Fig.5. Spherical distinct grains can be clearly observed in the micrograph. The average grain size was observed as 10μm. Small pore channels can also be observed in the micrograph. This pores or channel formation was due to grain boundary strain due to Zr incorporation in lattice site [23]. This pore helps in increase in Li mobility during the electrolysis reaction of lithium battery.
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4. Conclusion Lithium Titanate anode material Li4Ti5O12 incorporated with Zr-ion at varying weight percent was successfully prepared by the solid state reaction method. Presence of monoclinic phase was observed in prepared material.. Crystallaite size are found nm range. DTA test results reveal low calcination temperature in the prepared Li cathode i.e. 500 degree centigrade. SEM test had clearly shown spherical grains having average size 10μm. Impedance analysis of prepared material was shown that 0.2 weight % doping of Zr-ion in Li4Ti5O12 is most appropriate as it results in a decrease of the cathode resistance by 28 %. References [1]. [2]. [3]. [4]. [5]. [6]. [7]. [8]. [9]. [10]. [11]. [12]. [13]. [14]. [15]. [16]. [17]. [18]. [19]. [20]. [21]. [22]. [23].
R. Yuan, Cai, P. Gu,Z. Shao, J. of Power Sources 195(2010)2883-2887. L. Zhao, Y.S. Hu, H. Li, Z. Wang, L. Chen, Adv. Mat. 23(2011)1385-1388. M.M. Rahman, J.-Z.Wang, M. F.Hassan, D.Wexler, and H. K.Liu, Adv. Energy Mat.l(2011)212-220. Y. Wang, H. Liu, K. Wang, H. Eiji, Y. Wang, H. Zhou,J. of Mat. Chem.19(2009)6789. K. Amine, I. Belharouak, Z. Chen et al., Adv.Mat. 22(2010)3052-3057 S.Goriparti,E.Miele,F.De Angelis,E.Di Fabrizio,R.P.Zaccaria,C.Capiglia,J.Pow.Sources 257(2014) 421-443 A.V. Chadwick, M. J. Pooley and S. L. P. Savin Physica. Status Solidi 2(2015) 302-305 J. Lee, O. Nam, B.H. Cho,J. Power Sources, 174(2007)1-348 S.Arico,P. Bruce, B.Scrosati,J.M. Tarascon,V.Schalkwijk,Nat.Mater 4(2005) 366-77. X.Li,M.Qu,Z.Yu,J. of Alloys and Comp. 487(2009)13 J. Wolfenstine and J. L. Allen, J. of PowerSources, 180(2008) 582–585. S. Huang, Z. Wen, X. Zhu, and Z. Lin, J. of PowerSources1(2007). 408–412. A. D. Robertson, L. Trevino, H. Tukamoto, and J. T. S. Irvine, J. of PowerSources1Sources, 81(1999)352–357. S. Shi, C. Ouyang, M. Lei, and W. Tang, Journal of Power Sources 171(2007) 908–912. P. Kubiak, A. Garcia, M.Womes et al., Journal of Power Sources, 119–121(2003) 626–630. Y.Lu,M.Pang,S.Shi,Q.Ye,Z Tian,T Wang, NCBI Literature,8(2014) 2981 P. Kour, Pawan Kumar, S. K. Sinha, Manoranjan Kar, Solid StateCommunications 190(2014) 33–39. I. A. Leonidov,O. N. Leonidova,L. A. Perelyaeva, R. F. Samigullina,S. A. Kovyazina,M. V. Patrakeev, Physics of the Solid State 45 (2003)2183-2188. Z.Wang,H.Xie, G.Guowei, Lijun. J.of Nanomaterials(2012). 10.1155/2012/876197. D.Juarez-Robles,C.Chen,Y.Barsukov,P.Partha,Mukherjee,.J.of the electro.soc.164(2007)A837-A847. L.Wang,Z Wang,Q.Ju,We Wang,Z.Wang,,The 8th International Conference on Applied Energy- ICAE(2016) 4444- 4449 N.Bala, S.K.Sinha, International Journal of Interdisciplinary Research Centre (IJIRC) 1(2016), ISSN: 2455-2275(E) B.Scrosati,J.Garche,J.Power Sorces195(2005)2419-2430