NAnocasting SYnthesis of metal CArbide and Nitride Electrocatalysts

Project Information

NASYCANE

Grant agreement ID: 101028087

DOI

10.3030/101028087

Project closed

EC signature date 12 March 2021

Start date 18 August 2021

End date 17 August 2023

Funded under

• EXCELLENT SCIENCE - Marie Skłodowska-Curie Actions

Total cost

€ 212 933,76

EU contribution

€ 212 933,76

Coordinated by

THE UNIVERSITY OF BIRMINGHAM
United Kingdom

Periodic Reporting for period 1 - NASYCANE (NAnocasting SYnthesis of metal CArbide and Nitride Electrocatalysts)

Reporting period: 2021-08-18 to 2023-08-17

Summary of the context and overall objectives of the project

The primary objective of NASYCANE is to design and synthesize nanomaterials of transition metal carbides and nitrides using readily available starting materials and straightforward synthesis methods, aiming to achieve efficient electrochemical reduction of CO2. Addressing industrial CO2 emissions through recycling holds the potential to mitigate climate change. The pivotal focus of the project is to develop electrocatalysts utilizing abundant materials for CO2 reduction. To this end, we have explored the 'nanocasting' method to generate nanostructured materials based on transition metal (TM) carbides and nitrides.

In particular, we've delved into the 'nanocasting' approach for synthesizing molybdenum carbide using the sol-gel method. Successfully demonstrating the tuning of nanoparticle size by varying the amount of nanocasting, Mo2C nanoparticles exhibited noteworthy electrocatalytic activity for CO2 reduction at room temperature. Furthermore, we've investigated the synthesis of tungsten carbide (WC) in both cubic and hexagonal phases, elucidating how the desired phase can be attained by manipulating the carbon precursor. Additionally, the synthesis of metal nitrides using the 'nanocasting' approach has been demonstrated. These findings collectively contribute to the advancement of 'nanocasting' synthesis of metal carbides and nitrides, marking significant progress in the NASYCANE project.

Work performed from the beginning of the project to the end of the period covered by the report and main results achieved so far

The key results of the work carried out are presented below
Transition Metal Carbide Nanoparticles:
Utilizing a modified Pechini method via the sol-gel technique, we successfully synthesized molybdenum carbide nanoparticles. A groundbreaking aspect of our work is the introduction of the 'nanocasting' approach within the sol-gel method, imparting scalability advantages. Our exploration of varied nanocasting ratios showcased a substantial impact on nanoparticle size, demonstrating the efficacy of casting in size modulation. Mo2C nanoparticles exhibited noteworthy electrocatalytic activity, revealing distinct influences of structure and casting on performance.
In another study, tungsten carbide nanoparticles were synthesized from various carbon sources using sol-gel methods. The smaller nanoparticles were obtained by changing the carbon source. Interestingly, we have shown that the phase of tungsten carbide can be changed with the carbon precursor used, which lead to the establishment of a very simple method for the synthesis of cubic phase tungsten carbide. The mechanistic studies for this synthesis are underway.
Metal Nitride Nanoparticles:
In our work on metal nitride particles, we have shown the utility of ‘nanocasting’ approach for the synthesis of Iron nitride particles. The synthesis methodology can be extended to other metal nitride nanoparticles as well.
During this project, preliminary studies were carried to introduce porosity into the hard carbons using ‘nanocasting’; synthesis of molybdenum carbide from biopolymers. These materials can be potentially used as anodes in sodium ion batteries.
A significant achievement was the synthesis of carbon nanosheets. The synthesis methodology is simple and easily scalable. Carbon nanosheets possess great interest because of their potential to use in electrochemical energy applications particularly in supercapacitors.
In summary, the work performed demonstrates a successful exploration of metal carbides and nitrides and ‘nanocasting’ approach which is a simple and scalable method that also offers the advantage tuning of size of the ‘nanoparticles’.

Progress beyond the state of the art and expected potential impact (including the socio-economic impact and the wider societal implications of the project so far)

a. The successful synthesis of molybdenum carbide nanoparticles using the nanocasting approach represents a novel and innovative method for nanoparticle production. he demonstration that casting can be used to control the size of carbide nanoparticles is an advancement beyond conventional synthesis methods. Despite the challenges in synthesizing different morphologies, the project has expanded the understanding of how casting techniques can be employed to tailor the size and potentially other properties of nanoparticles. The evaluation of electrocatalytic activity for Mo2C for CO2 reduction reaction provides insights into the potential applications of these materials.
b. Tungsten carbide (WC) is a material with remarkable properties, including high hardness, high melting point, and good wear resistance. It is often used in applications where these properties are required, such as cutting tools, drill bits, and wear-resistant coatings. WC exists in two distinct phases: cubic and hexagonal. The cubic phase is less common than the hexagonal phase, hence the studies on cubic phase are limited.
In this study, we developed a simple and straightforward method for synthesizing the different phases of WC using the sol-gel route. We found that the choice of carbon precursor significantly influenced the particle size of the synthesized WC. Cubic phase nanoparticles below 10 nm were obtained when using citric acid as carbon source, while micron-sized particles in hexagonal phase were obtained when using Pluronic as carbon precursor. The development of this new method for synthesizing WC in different phases opens new possibilities for its use in diverse applications. The analysis of the data to understand mechanism of the synthesis is currently underway.
c. Tunable synthesis of nanoparticles is always of great interest. The use of 'nanocasting' approach for the synthesis of Iron nitride nanoparticles is shown. Though further studies are still needed, the present work shows the possibility of utilizing this approach which can be further extended to other metal nitride nanoparticle
Overall the project has established a facile and scalable synthesis methodologies for the development of transition metal carbides and nitrides that can be used in electrochemical applications.

Schematic representation of 'nanocasting synthesis of transition metal carbides and nitrides