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Scanning electrochemical microscopy (SECM) is a probe technique employed for the efficient mapping of local electrocatalytic activity as well as instantaneous in-situ product analysis over various homogenous and heterogenous surfaces. Ultramicroelectrodes (UME) of varying tip radius (r) are used as probe for different amperometric and potentiometric measurements. The working principle of SECM comprises of four electrode system wherein microelectrode tip is brought closer to the substrate surface and the tip or substrate current is recorded as a function of the tip-to-sample separation distance, d (approach curve) or tip x–y position (imaging) which is further exploited for different SECM modes like feedback mode, generation collection mode and redox competition mode.

Localized activity by Scanning ElectroChemical Microscope (SECM)

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Publications:

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  1. “Selective Electrochemical Production of Hydrogen Peroxide from Reduction of Oxygen on Mesoporous Nitrogen Containing Carbon”, S. Mehta, D. Gupta, T. C. Nagaiah,* ChemElectroChem 2022, 9, e202101336.

  2. “Local electrocatalytic activity of PtRu supported on nitrogen-doped carbon nanotubes towards methanol oxidation by scanning electrochemical microscopy”, D. Gupta, S. Chakraborty, R. G. Amorim, R. Ahuja and T.C. Nagaiah,* J. Mater. Chem. A, 2021, 9, 21291–21301.

  3. “Tuning the MnWO  morphology and its electrocatalytic activity towards oxygen reduction reaction”, A. Tiwari, V. Singh and T. C. Nagaiah,* J. Mater. Chem. A, 2018, 6, 2681–2692.

  4. “Nitrogen containing carbon spheres as an efficient electrocatalyst for oxygen reduction: Microelectrochemical investigation and visualization” A. Tiwari, V. Singh, D. Mandal and T. C. Nagaiah,*  J. Mater. Chem. A, 2017, 5, 20014–20023.

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​Hydrogen production by H S electrolysis

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Hydrogen (H ), because of its remarkable energy density and eco-friendly nature, emerges as an ideal energy carrier for a sustainable future. In industry, 96 % of H  is from fossil fuels, and only 4 % accounted for H O electrolysis due to high potential requirements. On the other hand, H S, a potential source of H , was recognized as a noxious and environmental pollutant and required immediate attention. H S electrolysis produced pure H  and S at a very low potential than water electrolysis and offered a cost effective approach for pure hydrogen production and simultaneously removes pollutant from the environment. However, the catalyst poisoning due to sulfur accumulation hindered its practical application.


We are working on the electrocatalysts that show high H S splitting ability for longer duration and simultaneously looking for different methods to recover the powder sulfur from polysulfide solution and use the sulfur for battery application.

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Publications:

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  1. “Pure hydrogen and sulfur production from H S by an electrochemical approach using a NiCu–MoS  catalyst”, M. Kumar, and T. C. Nagaiah,* J. Mater. Chem. A, 2022, 10, 13031–13041.

  2. “Efficient production of hydrogen from H2S via electrolysis using a CoFeS  catalyst”, M. Kumar, and T. C. Nagaiah,*  J. Mater. Chem. A, 2022, 10, 7048–7057

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Production of high purity chlorine and hydrogen via HCl electrolysis

 

Chlorine production has emerged as an imperative process for chemical industries, being the primary  chemical for manufacture of essential industrial chemicals and consumer products. However, chlorine generation is an energy intensive process which makes its large-scale production expensive and challenging. HCl electrolysis employed with chlorine evolving anode (CEA) and oxygen depolarized cathode (ODC) to recover high-purity chlorine is an important area of research related to circular economy for sustainable growth of energy sector. In our research group, the development of bifunctional electrocatalysts active for Cl  evolution (CEA) and oxygen reduction (ODC) is mainly heading in the direction of overall HCl electrolysis. Our research is focused on eliminating the expensive and scarce noble-metal based benchmark catalysts for CEA and ODC by non-noble metal based catalysts with low cost and high abundance for HCl electrolysis.

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Publications:

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  1. “Recovery of High Purity Chlorine by Cu‐Doped Fe O  in Nitrogen Containing Carbon Matrix: A Bifunctional Electrocatalyst for HCl Electrolysis”, D. Gupta,† A. Kafle,† A. Chaturvedi, T. C. Nagaiah, * ChemElectroChem, 2021, 8, 2858.

  2. “In situ incorporation of cobalt nanoclusters and nitrogen into the carbon matrix: a bifunctional catalyst for the oxygen depolarized cathode and chlorine evolution in HCl electrolysis”, V. Singh and T. C. Nagaiah,* J. Mater. Chem. A, 2019, 7, 10019–10029.

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Electrochemical dinitrogen reduction for NH  synthesis

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Ammonia is a primary building element towards the synthesis of several types of commodities in various industry such as fertilizers, transportation, medicaments, explosive, dyes and resins production. Haber- Bosch process is the dominant industrial process for ammonia production, but reports about 2% of world-wide energy use (~ 34 GJ ton NH   ) and creates significant CO  emission (~ 2 ton CO ton NH   ). Electrochemical dinitrogen reduction could be one of the most appropriate choices for ecological and CO  free ammonia production. Our research is predominantly engaged towards development of electrocatalysts for electrochemical dinitrogen fixation under ambient conditions. To address this we emphasize on identification of specific catalysts among various materials including noble-metals to non-noble metals and to metal-free carbonaceous catalysts with tuned morphology, facets and active sites.

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Electrochemical CO  reduction to value-added chemicals

 

Carbon dioxide (CO ) is an important carbon source for sustainable life. However, the overreliance on fossil fuels causes the massive discharge of CO  in the environment causing global warming and scarcity of energy. Producing an anthropogenic carbon cycle by converting CO  and H O into fuels and chemicals is an appealing strategy to address the aforementioned issues. The electrochemical reduction of CO  to value-added fuels is a promising approach, wherein the development of efficient electrocatalyst plays an important role in terms of activity and selectivity/Faradaic efficiency (FE). Our research in this area involve catalyst designing and improvement of catalytic activity and selectivity by changing the compositional behaviour of electrocatalyst such as alloying, hybridizing, and controlling the sizes and shapes for selective conversion of CO  to valuable chemicals namely methanol, methane, formic acid and carbon monoxide etc.

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Oxygen electrocatalysis

 

Oxygen electrocatalysis is considered as one of the most significant research avenue in electrochemistry  due to its sluggish kinetics which governs the overall reaction rate of electrochemical systems. O  electrochemistry involves reduction (ORR) and/or evolution (OER) of molecular oxygen residing at the heart of water electrolysis, metal–air batteries and fuel cells. ORR and OER are major bottlenecks that limit the efficiency of energy conversion and storage systems despite of usage of highly active and expensive precious metal-based benchmark catalysts. Our group is extensively working on the designing of cost-effective, highly active and durable electrocatalysts for ORR and OER to pave a pathway for carbon free energy storage and conversion by renewable energy systems. We focus on research adjoining the design and synthesis of cost-effective functional and composite materials based on earth-abundant elements, with high activity and durability that operate at reduced overpotentials and universal pH conditions.

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Recent Publications:

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  1. “Multifunctional cobalt iron sulfide electrocatalyst for high performance Zn-air battery and overall water splitting”, A. Kafle, M. Kumar, D. Gupta and T. C. Nagaiah,* J. Mater. Chem. A, 2022, 10, 4720.

  2. “Selective Electrochemical Production of Hydrogen Peroxide from Reduction of Oxygen on Mesoporous Nitrogen Containing Carbon”, S. Mehta, D. Gupta, T. C. Nagaiah,* ChemElectroChem 2022, 9, e202101336.

  3. “Nickel Iron Phosphide/Phosphate as an Oxygen Bifunctional Electrocatalyst for High-Power-Density Rechargeable Zn-Air Batteries”, N. Thakur, M. Kumar, D. Mandal* and T. C. Nagaiah,* ACS Appl. Mater. Interfaces, 2021, 13, 52487-52497.

  4. “Tuning polyoxometalate composites with carbonaceous materials towards oxygen bifunctional activity”, T. C. Nagaiah,* D. Gupta, S. D. Adhikary, A. Kafle and D. Mandal,* J. Mater. Chem. A, 2021, 9, 9228.

  5. “In situ Probing of Mn O  Activation toward Oxygen Electroreduction by the Laser-Induced Current Transient Technique”, T. C. Nagaiah,* A. Tiwari, M. Kumar, D. Scieszka, and A. S. Bandarenka. ACS Appl. Energy Mater. 2020, 3, 9151−9157.

  6. “In situ incorporation of cobalt nanoclusters and nitrogen into the carbon matrix: a bifunctional catalyst for the oxygen depolarized cathode and chlorine evolution in HCl electrolysis”, V. Singh and T. C. Nagaiah,* J. Mater. Chem. A, 2019, 7, 10019–10029.

  7. “Facet-controlled morphology of cobalt disulfide towards enhanced oxygen reduction reaction”, V. Singh, A. Tiwari and T. C. Nagaiah,* J. Mater. Chem. A, 2018, 6, 22545–22554.

  8. “Tuning the MnWO  morphology and its electrocatalytic activity towards oxygen reduction reaction”, A. Tiwari, V. Singh and T. C. Nagaiah,* J. Mater. Chem. A, 2018, 6, 2681–2692.

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Water splitting

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Hydrogen (H ) production is utterly significant for renewable clean energy, but consumes a lot of non-renewable energy along with the increased carbon footprint at industrial level. Electrochemical water splitting is a promising alternative for greener H  production and extensive research is going on around the world for development of efficient and economic technologies for the same. The core target of our research lies within catalyst designing for electrochemical water splitting (oxygen and hydrogen evolution reactions; OER and HER). The objective is to develop non-expensive, active and stable electrocatalysts varying from solid-state materials to self-standing flexible electrodes operating at reduced overpotentials to carry out water splitting.

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Recent Publications:

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  1. “Multifunctional cobalt iron sulfide electrocatalyst for high performance Zn-air battery and overall water splitting”, M. Kumar and T. C. Nagaiah,* J. Mater. Chem. A, 2022, 10, 4720.

  2. “The activation-free electroless deposition of NiFe over carbon cloth as a self-standing flexible electrode towards overall water splitting”, A. Kafle, M. Kumar, D. Gupta and T. C. Nagaiah,* J. Mater. Chem. A, 2021, 9, 24299.

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