Abstract: The invention discloses lithium titanate (LTO) nanoparticles 200 that have a self-assembled disordered surface layer. A modified-solvothermal method 100 of preparing the LTO nanoparticles 200 is described. The method 100 inhibits the crystallization of titanium dioxide TiO2 nanoparticles by an ageing process that is performed in continuation to the solvothermal process. The nanoparticles are characterized by the absence of a peak corresponding to [101] of TiO2 at 2theta value of 25° in the X-Ray diffraction spectra. An electrochemical cell 400 having surface engineered LiMn2O4 cathode and LTO electrode 300 as anode is disclosed. The electrochemical cell 400 delivers high capacity at ultrafast rates of charge and discharge. The LTO electrode 300 delivers specific capacity of 129 mAh/g at rates of 600C and 60mAh/g at 1200C. Further the electrochemical cell has long cycling capability without compromising capacity and nominal voltage. The electrochemical cell may be employed for high-end electric vehicle applications. The invention discloses lithium titanate (LTO) nanoparticles 200 that have a self-assembled disordered surface layer. A modified-solvothermal method 100 of preparing the LTO nanoparticles 200 is described. The method 100 inhibits the crystallization of titanium dioxide TiO2 nanoparticles by an ageing process that is performed in continuation to the solvothermal process. The nanoparticles are characterized by the absence of a peak corresponding to [101] of TiO2 at 2theta value of 25° in the X-Ray diffraction spectra. An electrochemical cell 400 having surface engineered LiMn2O4 cathode and LTO electrode 300 as anode is disclosed. The electrochemical cell 400 delivers high capacity at ultrafast rates of charge and discharge. The LTO electrode 300 delivers specific capacity of 129 mAh/g at rates of 600C and 60mAh/g at 1200C. Further the electrochemical cell has long cycling capability without compromising capacity and nominal voltage. The electrochemical cell may be employed for high-end electric vehicle applications.
1. A modified-solvothermal method (100) of preparing lithium titanate (LTO) nanoparticles having self-assembled disordered surface layer, comprising the steps of: adding titanium isopropoxide precursor to a first solution comprising lithium hydroxide and a solvent to form a first mixture, wherein the ratio of lithium hydroxide to titanium isopropoxide is in the range of 3.5:5 to 4.5:5; adding ammonia to the first mixture to form a second solution; heating the second solution at a temperature between 150 and 250°C in an autoclave reactor for 36 hours or more to obtain a nanocomposite material of LTO and titania (TiC^) nanoparticles; cooling to room temperature and retaining the nanocomposite material in the autoclave for 24 hours or more; and removing the nanoparticles from the autoclave and annealing at a temperature between 400 and 600°C for 6 hours or more to obtain LTO nanoparticles having self-assembled disordered surface layer.
2. The method as claimed in claim 1, wherein the solvent is selected from ethylene glycol, diethylene glycol, deionized water or ethanol.
3. A nanoparticle composition (200) for use in an electrode, having a crystalline lithium titanate (LTO) core (210) and self-assembled disordered surface layer (220), wherein the composition is characterized by the absence of a peak corresponding to [101] of Ti02 at 2 theta value of 25° in the X-Ray diffraction spectra..
4. The nanoparticle composition as claimed in claim 3, characterized by the absence of Eg peak at 144 cm"1 in Raman shift.
5. The nanoparticle composition as claimed in claim 3, wherein the LTO nanoparticles (200) have a diffusion coëfficiënt of Li ions in the range of 10"9 cm2/s.
6. An electrode (300) comprising: 70-80 wt.% of the nanoparticle composition of claim 3; 10-20 wt.% of a carbon additive selected from carbon nanotubes (CNT) (230), graphene nanoplatelets (GNP), carbon black (CB), or a combination thereof; and 10-20 wt.% of a binder selected from polyvinylidene fluoride (PVDF), polyvinylpyrrolidone (PVP), polyacrylic acid (PAA) or a combination thereof.
7. The electrode as claimed in claim 6, wherein a first cycle specific charge capacity of the electrode is greater than 155 mAh/g at 50C discharge rate.
8. The electrode as claimed in claim 6, wherein charge retention at the end of 2000 cycles is 70% at 100C discharge rate, to 82.6% at 50C discharge rate of the first cycle specific capacity for 2000 cycles.
9. The electrode as claimed in claim 6, wherein specific charge capacity ranges from 149 mAh/g for 100C discharge rate to 60 mAh/g for 1200C discharge rate to.
10. An electrochemical cell (400) comprising: i. a lithium based cathode (420); ii. an anode (410) comprising LTO nanoparticles having a self-assembled disordered surface wherein the nanoparticles are characterized by the absence of a peak corresponding to [101] of ÜO2 at 2 theta value of 25° in the X-Ray diffraction spectra or Eg peak at 144 cm"1 in Raman shift; iii. a separator (430) comprising commercial glass fiber or polymeric placed between the anode and the cathode; and iv. a liquid electrolyte (440) in contact with the cathode, the anode and the separator.
11. The electrochemical cell as claimed in claim 10, wherein the lithium based cathode is selected from spinel LiMn204 or LiCoC>2 or LiNio.5Mn1.5O4 or LiFePC>4 or other lithium containing layered oxides and phosphates
12. The electrochemical cell as claimed in claim 10, wherein the separator (430) is commercial glass or a polymer selected from polypropylene or polyethylene.
13. The electrochemical cell as claimed in claim 10, wherein the liquid electrolyte (440) comprises LiPF6 salt dissolved in a carbonate solvent selected from ethylene carbonate, dimethyl carbonate, diethyl carbonate, propylene carbonate or combinations thereof.
14. The electrochemical cell as claimed in claim 11, wherein discharge capacity of the full cell ranges from 170 mAh/g for 25 C discharge rate to 115 for 200C discharge rate.
15. The electrochemical cell as claimed in claim 11, wherein power density is at least 76 kW/kg and energy density is 249 or more Wh/kg at 200C discharge rate based on active material weight of the anode.
16. The electrochemical cell as claimed in claim 11, wherein discharge capacity retention at 100C discharge rate is 150 to 160 mAh/g at elevated temperatures of 55°C; or 75 to 85 mAh/g at low temperatures of -10°C.
17. The electrochemical cell as claimed in claim 11, wherein specific capacity of a half cell is 100 mAh/g or above at 300C discharge rate.
WE CLAIM:
1. A modified-solvothermal method (100) of preparing lithium titanate (LTO)
nanoparticles having self-assembled disordered surface layer, comprising the steps of:
adding titanium isopropoxide precursor to a first solution comprising lithium
hydroxide and a solvent to form a first mixture, wherein the ratio of lithium
hydroxide to titanium isopropoxide is in the range of 3.5:5 to 4.5:5;
adding ammonia to the first mixture to form a second solution;
heating the second solution at a temperature between 150 and 250°C in an
autoclave reactor for 36 hours or more to obtain a nanocomposite material of LTO
and titania (TiC^) nanoparticles;
cooling to room temperature and retaining the nanocomposite material in the
autoclave for 24 hours or more; and
removing the nanoparticles from the autoclave and annealing at a temperature between 400 and 600°C for 6 hours or more to obtain LTO nanoparticles having self-assembled disordered surface layer.
2. The method as claimed in claim 1, wherein the solvent is selected from ethylene glycol, diethylene glycol, deionized water or ethanol.
3. A nanoparticle composition (200) for use in an electrode, having a crystalline lithium titanate (LTO) core (210) and self-assembled disordered surface layer (220), wherein the composition is characterized by the absence of a peak corresponding to [101] of Ti02 at 2 theta value of 25° in the X-Ray diffraction spectra..
4. The nanoparticle composition as claimed in claim 3, characterized by the absence of Eg peak at 144 cm"1 in Raman shift.
5. The nanoparticle composition as claimed in claim 3, wherein the LTO nanoparticles (200) have a diffusion coëfficiënt of Li ions in the range of 10"9 cm2/s.
6. An electrode (300) comprising:
70-80 wt.% of the nanoparticle composition of claim 3;
10-20 wt.% of a carbon additive selected from carbon nanotubes (CNT)
(230), graphene nanoplatelets (GNP), carbon black (CB), or a combination
thereof; and
10-20 wt.% of a binder selected from polyvinylidene fluoride (PVDF),
polyvinylpyrrolidone (PVP), polyacrylic acid (PAA) or a combination
thereof.
7. The electrode as claimed in claim 6, wherein a first cycle specific charge capacity of the electrode is greater than 155 mAh/g at 50C discharge rate.
8. The electrode as claimed in claim 6, wherein charge retention at the end of 2000 cycles is 70% at 100C discharge rate, to 82.6% at 50C discharge rate of the first cycle specific capacity for 2000 cycles.
9. The electrode as claimed in claim 6, wherein specific charge capacity ranges from 149 mAh/g for 100C discharge rate to 60 mAh/g for 1200C discharge rate to.
10. An electrochemical cell (400) comprising:
i. a lithium based cathode (420);
ii. an anode (410) comprising LTO nanoparticles having a self-assembled disordered surface wherein the nanoparticles are
characterized by the absence of a peak corresponding to [101] of
ÜO2 at 2 theta value of 25° in the X-Ray diffraction spectra or Eg
peak at 144 cm"1 in Raman shift; iii. a separator (430) comprising commercial glass fiber or polymeric
placed between the anode and the cathode; and iv. a liquid electrolyte (440) in contact with the cathode, the anode and
the separator.
11. The electrochemical cell as claimed in claim 10, wherein the lithium based cathode is selected from spinel LiMn204 or LiCoC>2 or LiNio.5Mn1.5O4 or LiFePC>4 or other lithium containing layered oxides and phosphates
12. The electrochemical cell as claimed in claim 10, wherein the separator (430) is commercial glass or a polymer selected from polypropylene or polyethylene.
13. The electrochemical cell as claimed in claim 10, wherein the liquid electrolyte (440) comprises LiPF6 salt dissolved in a carbonate solvent selected from ethylene carbonate, dimethyl carbonate, diethyl carbonate, propylene carbonate or combinations thereof.
14. The electrochemical cell as claimed in claim 11, wherein discharge capacity of the full cell ranges from 170 mAh/g for 25 C discharge rate to 115 for 200C discharge rate.
15. The electrochemical cell as claimed in claim 11, wherein power density is at least 76 kW/kg and energy density is 249 or more Wh/kg at 200C discharge rate based on active material weight of the anode.
16. The electrochemical cell as claimed in claim 11, wherein discharge capacity retention at 100C discharge rate is
150 to 160 mAh/g at elevated temperatures of 55°C; or 75 to 85 mAh/g at low temperatures of -10°C.
17. The electrochemical cell as claimed in claim 11, wherein specific capacity of a
half cell is 100 mAh/g or above at 300C discharge rate.
| Section | Controller | Decision Date |
|---|---|---|
| Section 15 | SUBENDU KUNDU | 2024-03-21 |
| Section 15 | SUBENDU KUNDU | 2024-03-21 |
| # | Name | Date |
|---|---|---|
| 1 | 201841035135-STATEMENT OF UNDERTAKING (FORM 3) [18-09-2018(online)].pdf | 2018-09-18 |
| 2 | 201841035135-PROVISIONAL SPECIFICATION [18-09-2018(online)].pdf | 2018-09-18 |
| 3 | 201841035135-POWER OF AUTHORITY [18-09-2018(online)].pdf | 2018-09-18 |
| 4 | 201841035135-FORM 1 [18-09-2018(online)].pdf | 2018-09-18 |
| 5 | 201841035135-FORM 18 [17-09-2019(online)].pdf | 2019-09-17 |
| 6 | 201841035135-DRAWING [17-09-2019(online)].pdf | 2019-09-17 |
| 7 | 201841035135-CORRESPONDENCE-OTHERS [17-09-2019(online)].pdf | 2019-09-17 |
| 8 | 201841035135-COMPLETE SPECIFICATION [17-09-2019(online)].pdf | 2019-09-17 |
| 9 | 201841035135-Proof of Right (MANDATORY) [18-12-2019(online)].pdf | 2019-12-18 |
| 10 | Correspondence by Agent_Form-1_23-12-2019.pdf | 2019-12-23 |
| 11 | 201841035135-RELEVANT DOCUMENTS [25-08-2021(online)].pdf | 2021-08-25 |
| 12 | 201841035135-POA [25-08-2021(online)].pdf | 2021-08-25 |
| 13 | 201841035135-FORM 13 [25-08-2021(online)].pdf | 2021-08-25 |
| 14 | 201841035135-FER.pdf | 2021-10-17 |
| 15 | 201841035135-EDUCATIONAL INSTITUTION(S) [17-12-2021(online)].pdf | 2021-12-17 |
| 16 | 201841035135-OTHERS [28-12-2021(online)].pdf | 2021-12-28 |
| 17 | 201841035135-FER_SER_REPLY [28-12-2021(online)].pdf | 2021-12-28 |
| 18 | 201841035135-CLAIMS [28-12-2021(online)].pdf | 2021-12-28 |
| 19 | 201841035135 Correspondence by Office_Atomic_06-01-2022.pdf | 2022-01-06 |
| 20 | 201841035135-US(14)-HearingNotice-(HearingDate-21-02-2022).pdf | 2022-01-20 |
| 21 | 201841035135-Correspondence to notify the Controller [16-02-2022(online)].pdf | 2022-02-16 |
| 22 | 201841035135-Written submissions and relevant documents [07-03-2022(online)].pdf | 2022-03-07 |
| 23 | 201841035135-Response to office action [07-12-2022(online)].pdf | 2022-12-07 |
| 24 | 201841035135-PatentCertificate21-03-2024.pdf | 2024-03-21 |
| 25 | 201841035135-IntimationOfGrant21-03-2024.pdf | 2024-03-21 |
| 26 | 201841035135-Reply from DAE.pdf | 2024-07-19 |
| 1 | Search_Strategy_201841035135E_29-06-2021.pdf |