Colloidal synthesis of nanoparticles: from bimetallic to high entropy alloys

Silva, Cora Moreira Da; Amara, Hakim; Fossard, F.; Girard, A.; Loiseau, Annick; Huc, Vincent

doi:10.1039/d2nr02478k

Cited by 19 publications

(20 citation statements)

References 60 publications

(76 reference statements)

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“…This result contrasts that for NiPdPtRhIr, which contained 19% Ni using Ni(acac) 2 under the same conditions. To incorporate more Fe and Co, we rapidly injected the precursor solution (instead of the slow injection method that was used for NiPdPtRhIr), increased the temperature to 315 °C, and held for 1 h to favor complete decomposition of the Fe(acac) 3 and Co(acac) 3 . As shown in Figure , both FePdPtRhIr and CoPdPtRhIr were synthesized as single-phase fcc HEAs, with the experimental pattern matching a reference pattern with a = 3.85 Å and a = 3.85 Å for FePdPtRhIr and CoPdPtRhIr, respectively.…”

Section: Resultsmentioning

confidence: 99%

“…Certain metal acetylacetonate salts require a higher temperature to decompose while the different reduction potentials and reduction kinetics among the constituent salts lead to poor incorporation into the alloys. 25 This result indicates that the reaction conditions need to be adjusted to account for the decomposition and reduction kinetics of the most stable salt being used in the reaction to counter the varied reduction rates and ensure the availability of monomers in solution for autocatalytic reduction pathways to take over. Analogous to NiPdPtRhIr, we studied early time points in the reactions that formed FePdPtRhIr and CoPdPtRhIr to gain insights into the pathways by which they form.…”

Section: Incorporation Of Additionalmentioning

confidence: 99%

“…However, little is known about how key reaction variables influence colloidal HEA nanoparticle formation or stability. Even less is known about the reaction pathways that lead to their formation, as well as how reaction insights from one HEA nanoparticle system can be transferred to other systems. − Some mechanistic insights into the formation of HEA nanoparticles are emerging, but they generally involve different synthetic approaches that do not map onto the types of reactions that are most commonly used to make colloidal HEAs. ,, These knowledge gaps limit the rational synthesis of colloidal HEA nanoparticles, which is a significant shortcoming given the rapidly growing interest in the properties and applications of these materials.…”

Section: Introductionmentioning

confidence: 99%

“…Solution-based colloidal syntheses are among the most powerful for nanoparticles, as they can facilitate the controlled nucleation and growth of solids through chemical or thermal triggers and can allow for exquisite control over size and shape while offering liquid dispersibility and processing, as well as the potential for scalability. , Significant advances over the past two decades have provided detailed chemical insights into the reactions that produce metal and simple alloy nanoparticles and especially noble metal systems. − As a result, it is now possible to synthesize hundreds of different types of metal and alloy nanoparticles in solution with a high degree of control over size and shape. In contrast, methods to synthesize colloidal HEA nanoparticles are only beginning to emerge. − Additionally, little is known about the reaction chemistry that leads to their formation, given the large number of elemental reagents and their range of chemical reactivities, both individually and together. − Methods that sidestep the complex reaction chemistry by predesigning heterostructured nanoparticle precursors and annealing them to form HEAs provide promising alternatives but still require the particles to be anchored on refractory supports and annealed at high temperatures. , …”

Section: Introductionmentioning

confidence: 99%

“…To date, only a small number of reports describe the direct solution synthesis of unsupported colloidal HEA nanoparticles. ,,,,,− These reports generally approach the synthesis of colloidal HEA nanoparticles by simultaneously injecting five or more metal salts into a solvent, either preheated or at room temperature prior to heating, as such methods are analogous to those used to synthesize high quality nanoparticles of the constituent metals and their simpler alloys. For these reactions, it is generally accepted that, in most cases, all of the constituent metals coreduce simultaneously and directly form HEA nanoparticles, given the high reaction temperatures and rapid kinetics.…”

Section: Introductionmentioning

confidence: 99%

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Chemical Insights into the Formation of Colloidal High Entropy Alloy Nanoparticles

et al. 2023

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Nanoparticles of high entropy alloys (HEAs) have distinct properties that result from their high surface-tovolume ratios coupled with synergistic interactions among their five or more constituent elements, which are randomly distributed throughout a crystalline lattice. Methods to synthesize HEA nanoparticles are emerging, including solution approaches that yield colloidal products. However, the complex multielement compositions of HEA nanoparticles make it challenging to identify and understand their reaction chemistry and the pathways by which they form, which hinders their rational synthesis. Here, we demonstrate the synthesis and elucidate the reaction pathways of seven colloidal HEA nanoparticle systems that contain various combinations of noble metals (Pd, Pt, Rh, Ir), 3d transition metals (Ni, Fe, Co), and a p-block element (Sn). The nanoparticles were synthesized by slowly injecting a solution containing all five constituent metal salts into oleylamine and octadecene at 275 °C. Using NiPdPtRhIr as a lead system, we confirmed the homogeneous colocalization of all five elements and achieved tunable compositions by varying their ratios. We also observed heterogeneities, including Pd-rich regions, in a subpopulation of the NiPdPtRhIr sample. Halting the reaction at early time points and characterizing the isolated products revealed a timedependent composition evolution from Pd-rich NiPd seeds to the final NiPdPtRhIr HEA. Similar reactions applied to FePdPtRhIr, CoPdPtRhIr, NiFePdPtIr, and NiFeCoPdPt, with modified conditions to most efficiently incorporate all five elements into each HEA, also revealed similar Pd-rich seeds with system-dependent differences in the rates and sequences of element uptake into the nanoparticles. When moving to SnPdPtRhIr and NiSnPdPtIr, the time-dependent formation pathway was more consistent with simultaneous coreduction rather than through formation of reactive seeds. These studies reveal important similarities and differences among the pathways by which different colloidal HEA nanoparticles form using the same synthetic method, as well as establish generality. The results provide guidelines for incorporating a range of different elements into HEA nanoparticles, ultimately providing fundamental knowledge about how to define and optimize synthetic protocols, expand into different HEA nanoparticle systems, and achieve high phase purity.

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Section: Resultsmentioning

confidence: 99%

Section: Incorporation Of Additionalmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Chemical Insights into the Formation of Colloidal High Entropy Alloy Nanoparticles

et al. 2023

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Insights Into Formation and Growth of Colloidal Multielement Alloy Nanoparticles in Solution through In Situ Liquid Cell TEM Study

Amiri,

Yurkiv,

Phakatkar

et al. 2024

Adv Funct Materials

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The nucleation and growth of nanoparticles are critical processes determining the size, shape, and properties of resulting nanoparticles. However, understanding the complex mechanisms guiding the formation and growth of colloidal multielement alloy nanoparticles remains incomplete due to the involvement of multiple elements with different properties. This study investigates in situ colloidal synthesis of multielement alloys using transmission electron microscopy (TEM) in a liquid cell. Two different pathways for nanoparticle formation in a solution containing Au, Pt, Ir, Cu, and Ni elements, resulting in two distinct sets of particles are observed. One set exhibits high Au and Cu content, ranging from 10 to 30 nm, while the other set is multi‐elemental, with Pt, Cu, Ir, and Ni, all less than 4 nm. The findings suggest that, besides element miscibility, metal ion characteristics, particularly reduction rates, and valence numbers, significantly impact particle composition during early formation stages. Density functional theory (DFT) simulations confirm differences in nanoparticle composition and surface properties collectively influence the unique growth behaviors in each nanoparticle set. This study illuminates mechanisms underlying the formation and growth of multielement nanoparticles by emphasizing factors responsible for chemical separation and effects of interplay between composition, surface energies, and element miscibility on final nanoparticles size and structure.

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Stabilization and anchoring of palladium‐copper alloy on murexide modified carbon nanotube as a superb nanocatalyst: Excellent performance in coupling and synthetic reactions

Mohammadlou,

Noroozi Pesyan

2023

Applied Organom Chemis

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Sketching a proper catalytic system with supplementary attributes, containing easy separation, wide surface area, supreme loading capacity, and fantastical electronic attributes, proposes an encouraging direction for efficiently using nanostructures for various applications. However, the capability to adjust the nano‐measure bimetallic particles is an adjustment for attaining superb performance in the catalytic field. Herein, an environmentally benign approach was developed for immobilizing and anchoring Pd‐Cu alloy nanoparticles on murexide (MX)‐functionalized carbon nanotubes (CNTs). Afterward, the catalytic activity of Pd2‐Cu3@MX/CNT was studied in synthesizing 2,3‐dihydro quinazoline‐4(1H)‐ones and carbon–carbon coupling reactions at sustainable reaction conditions under ultrasound irradiation. The results demonstrated that high‐affinity MX ligand and porous CNT structures than the adsorption of Pd–Cu had a unique designation in the high‐range constancy of the alloy nanoparticles and following catalytic activity. In addition, ultrasound irradiation got electrons of Pd–Cu alloy nanoparticles agitated, constructing a synergic efficacy between Cu and Pd metals for synthesis and coupling reactions. Our study represents that the designed catalyst is green, recyclable, and most suitable, providing new intuition into in high‐range constancy of bimetallic nanoparticles for broad applications.

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Colloidal synthesis of nanoparticles: from bimetallic to high entropy alloys

Abstract: A unique approach based on the colloidal route allowing the synthesis of monodisperse bimetallic, trimetallic, tetrametallic and pentametallic nanoparticles with diameters around 5 nm as solid solutions.

Cited by 19 publications

References 60 publications

Chemical Insights into the Formation of Colloidal High Entropy Alloy Nanoparticles

Chemical Insights into the Formation of Colloidal High Entropy Alloy Nanoparticles

Insights Into Formation and Growth of Colloidal Multielement Alloy Nanoparticles in Solution through In Situ Liquid Cell TEM Study

Stabilization and anchoring of palladium‐copper alloy on murexide modified carbon nanotube as a superb nanocatalyst: Excellent performance in coupling and synthetic reactions

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