Colloidal synthesis of metal chalcogenide nanomaterials from metal–organic precursors and capping ligand effect on electrocatalytic performance: progress, challenges and future perspectives

Khan, Malik Dilshad; Opałło, Marcin; Revaprasadu, Neerish

doi:10.1039/d1dt01742j

Cited by 27 publications

(26 citation statements)

References 88 publications

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“…Overall, the relatively similar electrochemically active surface area (ECSA) values for Sa6, Sa7 and Sa8 (Figure S28) indicate similar populations of active sites, thus the adsorption and transfer of reactants to perform the NRR follows nearly common patterns in terms of speed. Possibly the capping ligands used during the synthesis of Sa6 deteriorated the electrocatalytic activity of the sharp tips and edges of its anisotropic structure by complicating the undisturbed access of reactants on these active sites [53]. Similar FE values have been obtained also for metal dichalcogenide materials with graphene-like structures such as c-MoS2 nanosheets grown on carbon cloth by hydrothermal method or MoSe2-based composites [50,54].…”

Section: Nitrogen Reduction Reactionmentioning

confidence: 53%

Heat-Up Colloidal Synthesis of Shape-Controlled Cu-Se-S Nanostructures—Role of Precursor and Surfactant Reactivity and Performance in N2 Electroreduction

et al. 2021

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Copper selenide-sulfide nanostructures were synthesized using metal-organic chemical routes in the presence of Cu- and Se-precursors as well as S-containing compounds. Our goal was first to examine if the initial Cu/Se 1:1 molar proportion in the starting reagents would always lead to equiatomic composition in the final product, depending on other synthesis parameters which affect the reagents reactivity. Such reaction conditions were the types of precursors, surfactants and other reagents, as well as the synthesis temperature. The use of ‘hot-injection’ processes was avoided, focusing on ‘non-injection’ ones; that is, only heat-up protocols were employed, which have the advantage of simple operation and scalability. All reagents were mixed at room temperature followed by further heating to a selected high temperature. It was found that for samples with particles of bigger size and anisotropic shape the CuSe composition was favored, whereas particles with smaller size and spherical shape possessed a Cu2−xSe phase, especially when no sulfur was present. Apart from elemental Se, Al2Se3 was used as an efficient selenium source for the first time for the acquisition of copper selenide nanostructures. The use of dodecanethiol in the presence of trioctylphosphine and elemental Se promoted the incorporation of sulfur in the materials crystal lattice, leading to Cu-Se-S compositions. A variety of techniques were used to characterize the formed nanomaterials such as XRD, TEM, HRTEM, STEM-EDX, AFM and UV-Vis-NIR. Promising results, especially for thin anisotropic nanoplates for use as electrocatalysts in nitrogen reduction reaction (NRR), were obtained.

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Section: Nitrogen Reduction Reactionmentioning

confidence: 53%

Heat-Up Colloidal Synthesis of Shape-Controlled Cu-Se-S Nanostructures—Role of Precursor and Surfactant Reactivity and Performance in N2 Electroreduction

et al. 2021

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“…Still, such a negative effect depends also on the type of surfactant used. For instance, cationic surfactants are not suitable for catalysts with negative charges on their surfaces . We have previously shown that branched polyethyleneimine (PEI) allows noble metal nanostructures such as Pd and Au–Pt to exhibit remarkable catalytic and electrocatalytic performance, respectively. , Therefore, in sample Bi-S3, we kept the same conditions as in Bi-S2 with the exception of the use of PEI instead of PSS.…”

Section: Results and Discussionmentioning

confidence: 99%

Simple Bottom-Up Synthesis of Bismuthene Nanostructures with a Suitable Morphology for Competitive Performance in the Electrocatalytic Nitrogen Reduction Reaction

et al. 2022

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Nitrogen reduction to ammonia under ambient conditions has received important attention, in which high-performing catalysts are sought. A new, facile, and seedless solvothermal method based on a high-temperature reduction route has been developed in this work for the production of bismuthene nanostructures with excellent performance in the electrocatalytic nitrogen reduction reaction (NRR). Different reaction conditions were tested, such as the type of solvent, surfactant, reducing agent, reaction temperature, and time, as well as bismuth precursor source, resulting in distinct particle morphologies. Two-dimensional sheet-like structures and small particles displayed very high electrocatalytic activity, attributed to the abundance of tips, edges, and high surface area. NRR experiments resulted in an ammonia yield of 571 ± 0.1 μg h −1 cm −2 with a respective Faradaic efficiency of 7.94 ± 0.2% vs Ag/AgCl. The easy implementation of the synthetic reaction to produce Bi nanostructures facilitates its potential scale up to larger production yields.

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“…Transition-metal oxide nanocrystals are attractive for many different applications in energy conversion, storage, and photocatalysis due to their generally excellent chemical and thermal stability and their high surface area-to-volume ratio. − To advance the fundamental understanding and ultimate application of these nanomaterials, it is essential to develop synthetic methods that provide access to high-quality samples with controlled size, crystal structure, composition, and morphology . Over the last two decades, heat-up and hot-injection methods involving the reaction of precursors at elevated temperature and ambient pressure in high-boiling organic solvents have evolved to provide exquisite control over noble metal and metal chalcogenide semiconductor nanocrystals. − Ternary and alloyed materials with controlled compositions, core–shell structures, , and exceptionally high monodispersity in both isotropic and anisotropic morphologies − are all accessible for these materials. In contrast, transition-metal oxide nanomaterials, particularly ternary metal oxide nanocrystals, often cannot be made using these well-developed colloidal techniques.…”

Section: Introductionmentioning

confidence: 99%

Controlling Cation Distribution and Morphology in Colloidal Zinc Ferrite Nanocrystals

Lievanos

Knowles

2022

Chem. Mater.

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This paper describes the first synthetic method to achieve independent control over both the cation distribution (quantified by the inversion parameter x) and size of colloidal ZnFe 2 O 4 nanocrystals. Use of a heterobimetallic triangular complex of formula ZnFe 2 (μ 3 -O)(μ 2 -O 2 CCF 3 ) 6 (H 2 O) 3 as a single-source precursor, solvothermal reaction conditions, absence of hydroxyl groups from the reaction solvent, and the presence of oleylamine are required to achieve well-defined, crystalline, and monodisperse ZnFe 2 O 4 nanoparticles. The size of the ZnFe 2 O 4 nanocrystals increases as the ratio of oleic acid and oleylamine ligands to precursor increases. The inversion parameter increases with increasing solubility of the precursor in the reaction solvent, with the presence of oleic acid in the reaction mixture, and with decreasing reaction temperature. These results are consistent with a mechanism in which ligand exchange between oleic acid and carboxylate ligands bound to the precursor complex influences the degree to which the reaction produces a kinetically trapped or thermodynamically stable cation distribution. Importantly, these results indicate that preservation of the triangular Zn−O−Fe 2 core structure of the precursor in the reactive monomer species is crucial to the production of a phase-pure ZnFe 2 O 4 product and to the ability to tune the cation distribution. Overall, these results demonstrate the advantages of using a single-source precursor and solvothermal reaction conditions to achieve synthetic control over the structure of ternary spinel ferrite nanocrystals.

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Colloidal synthesis of metal chalcogenide nanomaterials from metal–organic precursors and capping ligand effect on electrocatalytic performance: progress, challenges and future perspectives

Abstract: Renewable and sustainable functional nanomaterials, which can be employed in alternative green energy sources, are highly desirable. Transition metal chalcogenides are potential catalysts for processes resulting in energy generation and...

Cited by 27 publications

References 88 publications

Heat-Up Colloidal Synthesis of Shape-Controlled Cu-Se-S Nanostructures—Role of Precursor and Surfactant Reactivity and Performance in N2 Electroreduction

Heat-Up Colloidal Synthesis of Shape-Controlled Cu-Se-S Nanostructures—Role of Precursor and Surfactant Reactivity and Performance in N2 Electroreduction

Simple Bottom-Up Synthesis of Bismuthene Nanostructures with a Suitable Morphology for Competitive Performance in the Electrocatalytic Nitrogen Reduction Reaction

Controlling Cation Distribution and Morphology in Colloidal Zinc Ferrite Nanocrystals

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