Low-Temperature Solution-Mediated Synthesis of Polycrystalline Intermetallic Compounds from Bulk Metal Powders

Henderson, Nathaniel L.; Schaak, Raymond E.

doi:10.1021/cm800245j

Cited by 16 publications

(17 citation statements)

References 47 publications

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“…2,3,4 Foremost among such "soft" chemistry routes is polyol co-reduction, where soluble metal precursors are heated in ethylene glycol or another mildly reducing solvent, usually to produce the desired intermetallic compound. 53,54,55,56,57,58,59,60 While the use of this method is widespread, it may result in phase segregated products due to the different reduction potentials of the metals. Another synthetic method, which is a modification of the polyol approach is coined 'ship-in-a-bottle'.…”

Section: Introductionmentioning

confidence: 99%

Intermetallic Nanocatalysts from Heterobimetallic Group 10–14 Pyridine-2-thiolate Precursors

et al. 2020

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Intermetallic compounds are atomically ordered inorganic materials containing two or more transition metals and main-group elements in unique crystal structures. Intermetallics based on group 10 and group 14 metals have shown enhanced activity, selectivity, and durability in comparison to simple metals and alloys in many catalytic reactions. While high-temperature solid-state methods to prepare intermetallic compounds exist, softer synthetic methods can provide key advantages, such as enabling the preparation of metastable phases or of smaller particles with increased surface areas for catalysis. Here, we study a generalized family of heterobimetallic precursors to binary intermetallics, each containing a group 10 metal and a group 14 tetrel bonded together and supported by pincer-like pyridine-2-thiolate ligands. Upon thermal decomposition, these heterobimetallic complexes form 10-14 binary intermetallic nanocrystals. Experiments and density functional theory (DFT) computations help in better understanding the reactivity of these precursors toward the synthesis of specific intermetallic binary phases. Using Pd2Sn as an example, we demonstrate that nanoparticles made in this way can act as uniquely selective catalysts for the reduction of nitroarenes to azoxyarenes, which highlights the utility of the intermetallics made by our method. Employing heterobimetallic pincer complexes as precursors toward binary nanocrystals and other metal-rich intermetallics provides opportunities to explore the fundamental chemistry and applications of these materials.

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Section: Introductionmentioning

confidence: 99%

Intermetallic Nanocatalysts from Heterobimetallic Group 10–14 Pyridine-2-thiolate Precursors

et al. 2020

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“…Typical synthetic strategies for this kind of compounds are high‐temperature and high‐pressure routes, which are unsuitable for the synthesis of nanostructured samples. Thus it became necessary to develop and establish new routes that operate at low temperature 2,3…”

Section: Introductionmentioning

confidence: 99%

Semimetallic Paramagnetic Nano‐Bi₂Ir and Superconducting Ferromagnetic Nano‐Bi₃Ni by Microwave‐Assisted Synthesis and Room Temperature Pseudomorphosis

Boldt

Grigas

Heise

et al. 2012

Zeitschrift anorg allge chemie

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Uniform nanocrystals of the intermetallic compounds Bi 2 Ir (diameter Ն 50 nm) and Bi 3 Ni (typical size 200 ϫ 600 nm) were obtained by a microwave-assisted polyol process at 240°C. The method was also applied to the spatially confined reaction environment in the microporous exo-template SBA-15 resulting in Bi 3 Ni particles of about 6 nm. Non-crystalline bundles of parallel Bi 3 Ni nanofibres that have an individual diameter of less than 1 nm were obtained by reductive pseudomorphosis of the subiodide Bi 12 Ni 4 I 3 at room temperature. Magnetic susceptibility measurements demonstrate coexistence of ferromagnetism and superconductivity in a single phase for the nanostructured Bi 3 Ni materials. Curie temperature, coercive field, remnant magnetization, saturation moment, diamagnetic screening, and critical

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“…The polyol process is an efficient way of preparing bimetallic nanoparticles in the form of alloys [16,17] or ordered intermetallic compounds [18][19][20][21][22] at low temperature. In this method, the nanostructures are formed in suspension within the solution, ensuring stability and control of particle size [23].…”

Section: Introductionmentioning

confidence: 99%

Synthesis and Characterization of Ordered Intermetallic Nanostructured PtSn/C and PtSb/C and Evaluation as Electrodes for Alcohol Oxidation

Silva

Angelo

2010

Electrocatal

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Ordered intermetallic compounds of Pt-based metal electrocatalysts have been recently proposed as very efficient anode materials for reactions involved in low temperature fuel cells. In this work, supported ordered intermetallics nanoparticles PtSn/C and PtSb/C and supported platinum nanoparticles (Pt/C) were prepared at low temperature from their metallic precursors by a modified polyol process, using tetraethylene glycol as the solvent and reducing agent and Vulcan carbon XC-72 as the support. Powder X-ray diffraction patterns confirmed the presence of the ordered intermetallic phase and furnished lattice parameters and crystal structure. Transmission electron microscopy images show that the metal particles were highly dispersed and distributed homogeneously over the support, and energy-dispersive X-ray spectroscopy showed that the composition of the final product is within that of the desired stoichiometry. The electrocatalytic activity of these intermetallic phases toward the oxidation of methanol, ethanol, and ethylene glycol were confirmed by cyclic voltammetry and steady-state polarization curve at room temperature. The results showed that the supported intermetallic nanoparticles PtSn and PtSb are more active than the Pt/C catalyst prepared by the same method for alcohol oxidation.

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Low-Temperature Solution-Mediated Synthesis of Polycrystalline Intermetallic Compounds from Bulk Metal Powders

Cited by 16 publications

References 47 publications

Intermetallic Nanocatalysts from Heterobimetallic Group 10–14 Pyridine-2-thiolate Precursors

Intermetallic Nanocatalysts from Heterobimetallic Group 10–14 Pyridine-2-thiolate Precursors

Semimetallic Paramagnetic Nano‐Bi₂Ir and Superconducting Ferromagnetic Nano‐Bi₃Ni by Microwave‐Assisted Synthesis and Room Temperature Pseudomorphosis

Synthesis and Characterization of Ordered Intermetallic Nanostructured PtSn/C and PtSb/C and Evaluation as Electrodes for Alcohol Oxidation

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Low-Temperature Solution-Mediated Synthesis of Polycrystalline Intermetallic Compounds from Bulk Metal Powders

Cited by 16 publications

References 47 publications

Intermetallic Nanocatalysts from Heterobimetallic Group 10–14 Pyridine-2-thiolate Precursors

Intermetallic Nanocatalysts from Heterobimetallic Group 10–14 Pyridine-2-thiolate Precursors

Semimetallic Paramagnetic Nano‐Bi2Ir and Superconducting Ferromagnetic Nano‐Bi3Ni by Microwave‐Assisted Synthesis and Room Temperature Pseudomorphosis

Synthesis and Characterization of Ordered Intermetallic Nanostructured PtSn/C and PtSb/C and Evaluation as Electrodes for Alcohol Oxidation

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Product

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Semimetallic Paramagnetic Nano‐Bi₂Ir and Superconducting Ferromagnetic Nano‐Bi₃Ni by Microwave‐Assisted Synthesis and Room Temperature Pseudomorphosis