Artificial electrocatalytic ammonia (NH3) synthesis is recently becoming a research hotspot. It can couple with clean renewable electricity, which is considered an energy-efficient and sustainable approach for regulating the recirculation of nitrogen species and meanwhile promoting the growth of a circular nitrogen economy. In this Account, we review recent advances in electrocatalytic ammonia synthesis. Firstly, we briefly introduce the research background and significance of three electrochemical NH3 synthesis routes: electrocatalytic nitrogen reduction, nitric oxide reduction, and nitrate/nitrite reduction. And then we give a detailed discussion of the latest research advances in electrocatalysts for ambient NH3 synthesis, mainly involving catalytic mechanisms, theoretical advances, and electrochemical performance. Finally, the existing challenges and future research needs for artificial electrosynthesis of NH3 are also highlighted. 

Recent advances in electrocatalytic ammonia synthesis

Synergistic Enhancement of Electrocatalytic Nitrogen Reduction over Few-Layer MoSe2-Decorated Ti3C2Tx MXene

Recent advances in the synthesis and electrocatalytic application of MXene materials.

The hydrothermal dissolution-recrystallization process is a key step in the crystal structure of titania-based nanotubes and their composition. This work systematically studies the hydrothermal conditions for directly synthesizing anatase TiO2 nanotubes (ATNTs), which have not been deeply discussed elsewhere. It has been well-known that ATNTs can be synthesized by the calcination of titanate nanotubes. Herein, we found the ATNTs can be directly synthesized by optimizing the reaction temperature and time rather than calcination of titanate nanotubes, where at each temperature, there is a range of reaction times in which ATNTs can be prepared. The effect of NaOH/TiO2 ratio and starting materials was explored, and it was found that ATNTs can be prepared only if the precursor is anatase TiO2, using rutile TiO2 leads to forming titanate nanotubes. As a result, ATNTs produced directly without calcination have excellent photocatalytic CO2 reduction than titanate nanotubes and ATNTs prepared by titanate calcination.

https://pubs.acs.org/doi/pdf/10.1021/acsomega.2c04211

One-Step Hydrothermal Synthesis of Anatase TiO2 Nanotubes for Efficient Photocatalytic CO2 Reduction

Recent Advances in Ammonia Synthesis over Ruthenium Single-Atom-Embedded Catalysts: a Focused Review

https://www.cjcatal.com/EN/article/downloadArticleFile.do?attachType=PDF&id=26271

Heterostructuring 2D TiO2 nanosheets in situ grown on Ti3C2T MXene to improve the electrocatalytic nitrogen reduction

Hydrophobic treatment of the catalyst surfaces can suppress the competitive hydrogen evolution reaction (HER) during the nitrogen reduction reaction (NRR). In this work, the surface of Ti3C2Tix MXene is modified by cetyltrimethylammonium bromide (CTAB) and trimethoxy (3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl) silane (FOTS) to increase the hydrophobicity of MXenes. The ammonia (NH3) production rate and faradaic efficiency (FE) are improved from 37.62 to 54.01 μg h−1 mg−1cat. and 5.5% to 18.1% at −0.7 V vs. RHE, respectively after surface modification. 15N isotopic labeling experiment confirms that nitrogen in produced ammonia originates from N2 in the electrolyte. The excellent NRR activity of surface hydrophobic MXenes is mainly due to surfactant molecules, which inhibit the entry of water molecules and the competitive HER, which have been verified by in situ FT-IR, DFT and molecular dynamics calculations. This strategy provides an ingenious method to design more active NRR electrocatalysts. 

Surface hydrophobic modification of MXene to promote the electrochemical conversion of N2 to NH3

Electrochemical ammonia synthesis via nitrogen reduction reaction on 1T/2H mixed-phase MoSSe catalyst: Theoretical and experimental studies

Under the dual pressure of energy crisis and environmental pollution, ammonia (NH3) is an indispensable chemical product in the global economy. The electrocatalytic synthesis of NH3 directly from nitrogen (N2) and water (H2O) using renewable electricity has become one of the most attractive and important topics. The basal-plane-activated boron-doped MoS2 nanosheets (B-MoS2) as a non-noble metal catalyst with excellent performance for N2 electroreduction are synthesized by a facile one-step hydrothermal method. In 0.1 M Na2SO4 solution, MoS2 nanosheets doped with 300 mg boric acid (B-MoS2-300) obtain a charming ammonia yield rate of 75.77 µg h-1 mg-1cat. at -0.75 V vs. RHE, and an excellent Faradaic efficiency of 40.11% at -0.60 V vs. RHE. In addition, the B-MoS2-300 nanosheets show good selectivity and chemical stability, and no by-product hydrazine (N2H4) is generated during the reaction. 15N isotopic labeling experiment confirms that nitrogen in produced ammonia originates from N2 in the electrolyte. On the one hand, the high conductivity of MoS2 guarantees the electron transfer rate; on the other hand, the successful incorporation of heteroatom B enlarges the interlayer spacing of MoS2, and the B atom can act as an active site for basal plane activation, providing more active sites for NRR. Density functional theory calculation shows that the doping of B activates the base plane of 1T-MoS2, which makes the adsorption of N2 on the base plane easier and promotes the NRR process.

Basal Plane-activated Boron-doped Molybdenum Disulfide Nanosheets for Efficient Electrochemical ammonia synthesis.

Electrocatalytic nitrate reduction (NO3RR) technique has emerged as a hotspot in NH3 production, for its practicability, and a series of advanced electrocatalysts with high activity and robust stability needed to be constructed in today's era. In this work, size-tunable Cu nanoparticles on porous nitrogen-doped hexagonal carbon nanorods (Cu@NHC) were reasonably designed and served for catalyzing NO3RR in neutral media. Especially, Cu30%@NHC demonstrated a remarkable electroactivity for NH3 production as it showed a suitable grain size with massive catalytic centers and favorable d band structure with faster *NO3−-to-*NO2− catalytic dynamics. As expected, Cu30%@NHC (3628.28 µg h−1 mgcat.−1) had a much higher NH3 yield than those for Cu20%@NHC (1268.42 µg h−1 mgcat.−1) and Cu40%@NHC (725.03 µg h−1 mgcat.−1). And those collected NH3 products indeed derived from NO3RR process revealed by 15N isotope-labeling and systemic control tests. Moreover, Cu30%@NHC was also durable for NO3RR bulk electrolysis with minor loss in activity. This work offered an effective modifying tactics to boost NO3RR catalysis and could guide the design of other advanced electrocatalysts via size-induced surface engineering. 

Size-induced d band center upshift of copper for efficient nitrate reduction to ammonia

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