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Hierarchical nanostructured carbon materials derived from candle soot and graphene for high rate and high performance electrodes for automotive batteries and supercapacitors

Primary Information

Domain

Advanced Materials

Project No.

7035

Sanction and Project Initiation

Sanction No: F. No. 3-18/2015-T.S.-I (Vol IV)

Sanction Date: 08/05/2017

Project Initiation date: 19/08/2017

Project Duration: 36

Partner Ministry/Agency/Industry

Department of Heavy Industries

Role of partner:Financial support

Support from partner:50%, 130.34 Lakhs INR

Principal Investigator

PI Image

Chandra Shekhar SharmaPrimary
Indian Institute of Technology Hyderabad

Host Institute

Co-PIs

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Tata N. Rao
ARCI Hyderabad

Scope and Objectives

1. Full cell performance of the candle soot derived fractal like carbon nanoparticles
2. Fabrication and electrochemical testing of the hierarchical nanostructured carbon electrodes derived from depositing carbon soot nanoparticles and or graphene on the electro spun carbon nanofibers /particles
3. Tuning of various process parameters for as fabricated hierarchical carbon structures to optimize electrochemical performance
4. Developing a prototype rechargeable battery and supercapacitor for automotive

Deliverables

1. Full cell demonstration of candle soot derived carbon nanoparticles using coin cell prototype
2. High performance and high rate anode for LIB and supercapacitors derived from candle soot (half-cell mode and full cell mode)
3. Demonstration of the battery and supercapacitor performance at pouch cell/cylindrical cell configuration
4. Demonstrating optimal hierarchical structure for enhanced electrochemical performance by tuning the micropatterned structure aspect ratio and optimizing the other process conditions such as wt.% of graphene and candle soot deposition time.
5. Scaling up of the carbon materials upto kg level. 6. Developing the prototype for the LIB and supercapacitor using candle soot based hierarchical structure for automobile industry

Scientific Output

1. Synthesis of nitrogen doped candle soot for binder free lithium ion battery (half-cell) Nitrogen doped candle soot has been prepared by a facile modified flame synthesis. In this method, the candle wax has been treated at its melting point and urea is added in the molten state. Further, stirred for 10 min for the uniform dispersion and solidified. The urea wax ratio is maintained at 1:4. The nitrogen doped candle soot has been collected over the stainless steel current collector and used as a binder free anode in lithium ion battery. The collected soot has been physically characterized by FTIR and scanning electron microscopy. The cell has been fabricated by using nitrogen doped candle soot as anode and lithium foil as counter and reference electrode. The assembly has been carried out in high pure argon atmosphere by using LiPF6 as electrolyte and Whatman filter paper as separator. In order to explore the electrochemical behavior of the assembled cell cyclic voltammetry measurement has been carried out at 0.1 mVs-1 in the voltage window of 0.01- 3V. Fig.3 (a) shows the cyclic voltammetry of the assembled cell, the peak around 0.6 V in the first cycle indicates the formation of SEI layer and its absence in the subsequent cycles point the stability of the formed SEI. The anodic and cathodic peaks around 0.1V indicates the insertion -exertion reaction in the carbon structure. Fig.3(b) shows the galvanostatic charge-discharge profile of the cell at different C rates. The cell showed a specific capacity of 350 mAhg-1 at 0.1C rate with a columbic efficiency of 95%. The retention of the capacity at different C rates showed the stability of the formed SEI. The cell stability test has been performed at 10 C rate for 1000 cycles, exhibits a capacity 100 mAhg-1 after 1000cycles. In summary, nitrogen doped candle soot anode showed a good stability and rate capability compared to candle soot. Modified flame synthesis is a simple and effective strategy for developing the binder free electrodes for lithium ion battery. 2. Binder free and free standing carbon structures as anode material for lithium ion battery The free standing binder free electrode has been fabricated by pyrolyzing the pencil trace applied filter paper at 900 degree C. The degree of disorder in the binder free electrode has been quantified by calculating the ID/IG ratio in the Raman spectra. The ID/IG ratio of pyrolyzed filter paper and pencil applied pyrolyzed filter paper are 0.98 and 0.52 respectively. The decrement in the ID/IG ratio indicates the predominance of the G band due to retention of the pencil trace after pyrolysis. The SEM image shows the cellulose fibers along with graphite particles substantiate the retention of pencil trace on filter paper after pyrolysis. The coin cell 2032 has been fabricated by using the prepared binder free electrode as anode and lithium foil as the counter and reference electrode and the electrochemical measurement has been carried out in the potential window 0.01 V to 3V.

Results and outcome till date

1. Developed few novel ideas to fabricate low cost, large area and binder free anodes.
2. Nitrogen doped candle soot carbon based anode is also fabricated.
3. Candle soot and graphene based hierarchical electrodes are also fabricated successfully.
4. As-fabricated anodes are tested in half-cell for their electrochemical properties such as CV, charge-discharge and impedance spectroscopy.
5. Electrochemical performance in half cell configuration is exceptional in few cases. Discharge profile plateau shows its potential for commercial applications.
6. Some of these candle soot based materials are not being tested for supercapacitor applications as well.

Societal benefit and impact anticipated

The development of energy storage technology has become an essential part to sustain the growth and progress of the society. The current project aims the development of the prototype for the automotive battery as well as supercapacitors by using hierarchical nanostructured carbon electrodes by depositing conducting carbon soot nanoparticle and/or graphene on submicron electro spun polymer and/or carbon fibers. In this aspect, we systematically studied the half-cell behavior of the lithium ion battery with the developed binder free electrodes to understand the electrochemical behavior and ultimately, to fulfill the goal of full cell prototype. Proposed outcome of this project will greatly help in developing the technology in future for fabricating Li ion batteries and supercapacitors for hybrid plug-in vehicles.

Next steps

1. Full cell testing are underway based on the as-developed hierarchical carbon materials 2. Large scale synthesis of carbon soot is under progress.

Publications and reports

Manuscript under preparation 1. Mamidi Suresh, Ananya G., Chandra S. Sharma, A facile synthesis of nitrogen doped candle soot as an anode for Lithium ion battery: Binder free approach 2. Ananya G., Mamidi Suresh, Chandra S. Sharma, Paper based high performance flexible carbon electrodes for Lithium ion battery 3. Mamidi Suresh, Ananya G., Chandra S. Sharma, Three-dimensional micropatterned carbon arrays as High rate and high capacity anode for Lithium-ion Batteries

Patents

Filing In progress

Scholars and Project Staff

1 Ananya Gangadharan Postdoctoral fellow 30/10/2017-29/10/2018
2 Ravi Kali Postdoctoral fellow 6 months (15/11/2017-14/05/2018)
3 Darshana Potphode Postdoctoral fellow 03/05/2018-Till date
4 Sushree Ritu Ritanjali JRF 16/10/2017-25/12/2017
5 Omkar JRF/Ph.D. 16/11/2017-Till date
6 Shalakha Saha JRF/Ph.D. 02/07/2018-Till date
7 Shilpi Project Asst. 3 months (05/02/2018-04/05/2018)
8 Piu Trivedi Project Asst. 13/04/2018-12/10/2018
9. S. Krishna Kumar, Postdoctoral fellow, 01/10/2018-till date
10. Madhavi G., Project Assistant, 15/05/18- till date

Challenges faced

1. Timely disbursement of funds: 50% of funds for second year are still not released.
2. Too much paper work; same information is being asked multiple times in some or other format and that too on a short notice.

Other information

Nil

Financial Information

  • Total sanction: Rs. 26068000

  • Amount received: Rs. 17118000

  • Amount utilised for Equipment: Rs. 6248000

  • Amount utilised for Manpower: Rs. 2771000

  • Amount utilised for Consumables: Rs. 1387000

  • Amount utilised for Contingency: Rs. 109000

  • Amount utilised for Travel: Rs. 180000

  • Amount utilised for Other Expenses: 1001000

  • Amount utilised for Overheads: Rs. 2548000

Equipment and facilities

Glove box , Battery analyzer, Disc cutter, Hydraulic crimper, Thyristor, Weighing balance, Galvanostat/Potentiostat, 3 Phase 10 KVA UPS