Salt-templated platinum–palladium porous macrobeam synthesis

Burpo, F. John; Nagelli, Enoch A.; Mitropoulos, Alexander N.; McClure, Joshua P.; Baker, David R.; Losch, Anchor R.; Chu, Deryn

doi:10.1557/mrc.2018.217

Cited by 5 publications

(9 citation statements)

References 28 publications

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“…Energy-dispersive X-ray mapping shown in Figure S5 indicates that the spheres are composed of predominantly platinum. Similar spheres were previously observed for Pd 2+ :Pt 2− salts at a 1:1 ratio reduced with NaBH 4 [43].…”

Section: Scanning Electron Microscopy (Sem)supporting

confidence: 87%

“…In Figure 7d, the pronounced oxidation peak occurring around at +0.96 V (vs Ag/AgCl) and reduction peaks more positive than +0.58 V (vs Ag/Ag/Cl) are associated with the overall catalytic bimetallic crystal structure in the different Pt:Cu films. The oxidation of Pt-H to Pt-OH and Pt-OH to Pt-O is evident in the strong oxidation peaks at + 0.96 V (vs Ag/AgCl) and + 1.1 V (vs Ag/AgCl), respectively [43]. The overall larger current density normalized for the mass of platinum (A/g pt ) in the 2:1:1 salt ratio is a result of the contribution of catalytic current from the high atomic composition of platinum within the microtube film (as shown in the EDS and XPS results in Table 1).…”

Section: X-ray Photoelectron Spectroscopy (Xps)mentioning

confidence: 99%

“…While numerous Pt-Cu nanostructures have been demonstrated, discrete nanoparticles require post-synthesis binding into functional electrodes, and there has been limited demonstration of scalable aqueous-based synthesis of porous 3-dimensional structures.Recently rapid noble metal aerogel synthesis was demonstrated via a high concentration direct reduction approach [38,39], and salt templating was used to synthesize 2-dimensional materials [40,41]. Combining the use of high salt concentrations and salt templates, our group synthesized Pt and Pt-Pd macrobeams and porous nanomaterials from Magnus's and Vauquelin's salts and derivatives [42,43], as well as salt-templated Au-Pd and Au-Cu-Pd multi-metallic porous materials [44]. Rapid precipitation of high-aspect ratio Magnus's salts [45] and Vauquelin's salts [46] results from the combination of oppositely charged square planar platinum and palladium metal ions, respectively.…”

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confidence: 99%

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Salt-Templated Platinum-Copper Porous Macrobeams for Ethanol Oxidation

et al. 2019

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Platinum nanomaterials provide an excellent catalytic activity for diverse applications and given its high cost, platinum alloys and bi-metallic nanomaterials with transition metals are appealing for low cost and catalytic specificity. Here the synthesis of hierarchically porous Pt–Cu macrobeams and macrotubes templated from Magnus’s salt derivative needles is demonstrated. The metal composition was controlled through the combination of [PtCl4]2− with [Pt(NH3)4]2+ and [Cu(NH3)4]2+ ions in different ratios to form salt needle templates. Polycrystalline Pt–Cu porous macrotubes and macrobeams 10’ s–100’ s μm long with square cross-sections were formed through chemical reduction with dimethylamine borane (DMAB) and NaBH4, respectively. Specific capacitance as high as 20.7 F/g was demonstrated with cyclic voltammetry. For macrotubes and macrobeams synthesized from Pt2−:Pt2+:Cu2+ salt ratios of 1:1:0, 2:1:1, 3:1:2, and 1:0:1, DMAB reduced 3:1:2 macrotubes demonstrated the highest ethanol oxidation peak currents of 12.0 A/g at 0.5 mV/s and is attributed to the combination of a highly porous structure and platinum enriched surface. Salt templates with electrochemical reduction are suggested as a rapid, scalable, and tunable platform to achieve a wide range of 3-dimensional porous metal, alloy, and multi-metallic nanomaterials for catalysis, sensor, and energy storage applications.

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Section: Scanning Electron Microscopy (Sem)supporting

confidence: 87%

Section: X-ray Photoelectron Spectroscopy (Xps)mentioning

confidence: 99%

mentioning

confidence: 99%

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Salt-Templated Platinum-Copper Porous Macrobeams for Ethanol Oxidation

et al. 2019

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“…Here we demonstrate a scalable method to use the aqueous Magnus's salt structure as a sacrificial template [36][37][38][39][40] to create nanocomposite inks with platinum nanostructures dispersed in a CNT network to maximize the catalytically active surface area. This entirely aqueous scalable approach to an electrocatalyst ink uses the primary platinum nanoparticles of the sacrificial Magnus's salt templates to disperse with CNTs.…”

Section: Introductionmentioning

confidence: 99%

“…The ultrasonication of the resulting Pt macrotubes after chemical reduction of the salt templates is a unique and rapid way to form nanocomposites of Pt nanoparticles and CNTs without the need of surfactants or capping agents. The chemically reduced Magnus's salts result in Pt macrotubes that are comprised of primary nanoparticles [36][37][38][39][40]. This technique utilizes ultrasonication to break apart the macrostructure of the Pt macrotubes and disperse the high surface area primary Pt nanoparticles throughout the CNTs to form an electrocatalyst nanocomposite.…”

Section: Introductionmentioning

confidence: 99%

Scalable Carbon Nanotube/Platinum Nanoparticle Composite Inks from Salt Templates for Oxygen Reduction Reaction Electrocatalysis for PEM Fuel Cells

et al. 2020

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Platinum nanoparticles supported on multi-walled carbon nanotubes (CNTs) were synthesized by the chemical reduction of Magnus’s salt templates formed by the electrostatic stacking of oppositely charged platinum coordinated ions. The Magnus’s salt templated synthesis of platinum macrotubes, previously demonstrated, results in sidewalls made up of individual textured nanoparticles 100 nm in diameter and comprised of 5 nm diameter fibrils. Here we demonstrate a new platform method that utilizes the individual nanoparticles that make up the platinum macrotubes formed from salt templates and subsequently disperse them through a CNT network by ultrasonication to develop an electrocatalyst nanocomposite for the oxygen reduction reaction (ORR) critical for the development of proton exchange membrane (PEM) fuel cell applications. The structural morphology and composition of the nanocomposite catalysts was characterized using scanning electron microscopy (SEM), X-ray diffractometry (XRD), and Raman spectroscopy to confirm the presence of platinum nanoparticles throughout the CNT network of the nanocomposite. The electrocatalytic activity of the nanocomposite inks was verified with cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and linear sweep voltammetry (LSV) for ORR. Furthermore, this all aqueous-based and scalable approach for the synthesis and dispersion of platinum nanoparticles with CNTs can lead to a new formulation process for the production of electrocatalytic nanocomposite inks for PEM fuel cells using the nanoparticles that form within salt templates after chemical reduction.

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Noble Metal Aerogels

Burpo

2023

Springer Handbooks

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Salt-templated platinum–palladium porous macrobeam synthesis

Abstract: Abstract

Cited by 5 publications

References 28 publications

Salt-Templated Platinum-Copper Porous Macrobeams for Ethanol Oxidation

Salt-Templated Platinum-Copper Porous Macrobeams for Ethanol Oxidation

Scalable Carbon Nanotube/Platinum Nanoparticle Composite Inks from Salt Templates for Oxygen Reduction Reaction Electrocatalysis for PEM Fuel Cells

Noble Metal Aerogels

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