Electrodeposition of thick palladium coatings from a palladium(<scp>ii</scp>)-containing ionic liquid

Schaltin, Stijn; Brooks, Neil R.; Sniekers, Jeroen; Meervelt, Luc Van; Binnemans, Koen; Fransaer, Jan

doi:10.1039/c4cc04079a

Cited by 24 publications

(27 citation statements)

References 29 publications

(45 reference statements)

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“…[8][9][10][11][12][13] Several examples of electrodepositiono fm etals from liquid metal salts can be found in the literature. [14][15][16][17][18][19][20][21][22] Our research group has obtainedv ery promising resultsf or the electrodeposition of copper, [23][24][25] silver, [26][27][28][29][30] palladium [31] and lithium. [32] Metal coatings of ag ood quality were achieved at very high current densities,e ven withoutt he use of additives.…”

Section: Introductionmentioning

confidence: 98%

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Liquid Nickel Salts: Synthesis, Crystal Structure Determination, and Electrochemical Synthesis of Nickel Nanoparticles

Sniekers

Verguts

Brooks

et al. 2015

Chemistry A European J

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New nickel-containing ionic liquids were synthesized, characterized and their electrochemistry was investigated. In addition, a mechanism for the electrochemical synthesis of nanoparticles from these compounds is proposed. In these so-called liquid metal salts, the nickel(II) cation is octahedrally coordinated by six N-alkylimidazole ligands. The different counter anions that were used are bis(trifluoromethanesulfonyl)imide (Tf2 N(-) ), trifluoromethanesulfonate (OTf(-) ) and methanesulfonate (OMs(-) ). Several different N-alkylimidazoles were considered, with the alkyl sidechain ranging in length from methyl to dodecyl. The newly synthesized liquid metal salts were characterized by CHN analysis, FTIR, DSC, TGA and viscosity measurements. An odd-even effect was observed for the melting temperatures and viscosities of the ionic liquids, with the complexes with an even number of carbon atoms in the alkyl chain of the imidazole having a higher melting temperature and a lower viscosity than the complexes with an odd number of carbons. The crystal structures of several of the nickel(II) complexes that are not liquid at room temperature were determined. The electrochemistry of the compounds with the lowest viscosities was investigated. The nickel(II) cation could be reduced but surprisingly no nickel deposits were obtained on the electrode. Instead, nickel nanoparticles were formed at 100 % selectivity, as confirmed by TEM. The magnetic properties of these nanoparticles were investigated by SQUID measurements.

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Section: Introductionmentioning

confidence: 98%

“…This phenomenon was also found for previous liquid metal salts with copper and silver. [24][25][26][27][28][29][30][31] Upon removal of the workinge lectrode, ab lack precipitate formed around the cathode. Rinsing witha cetone andw ater completely rinsed off the precipitate and no nickel deposit was found.…”

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confidence: 99%

Liquid Nickel Salts: Synthesis, Crystal Structure Determination, and Electrochemical Synthesis of Nickel Nanoparticles

Sniekers

Verguts

Brooks

et al. 2015

Chemistry A European J

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“…The use of additives such as nicotinamide or applying pulse deposition did not significantly improve the quality of the Pd films [13]. Recently, Schaltin, et al deposited Pd from Pd-containing liquid metal salts (LMS) palladium-1-methyl-3-ethylimmidazolium (trifluoromethanesulfonyl) amide (Pd[Meim][NTf 2 ]) [14]. In their study, a Pd film of 8.3 mm thickness was fine-grained and crack-free, while a Pd film of 15.6 mm had cracks.…”

Section: Introductionmentioning

confidence: 98%

Palladium electrodeposition in 1-butyl-1-methylpyrrolidinium dicyanamide ionic liquid

Shrestha

Biddinger

2015

Electrochimica Acta

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“…22 However, these works were mostly limited to the study of Pd thin films. This limits the usability of Pd electrodeposition in ILs to the electronic and decorative industry.…”

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“…14,21 Pd-containing liquid metal salts (LMS), which are ILs with metal ions coordinated to the cations are also being explored for Pd electrodeposition. 22 However, these works were mostly limited to the study of Pd thin films. This limits the usability of Pd electrodeposition in ILs to the electronic and decorative industry.…”

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confidence: 99%

Size-Controlled Synthesis of Palladium Nanospheres by Pulse Electrodeposition in 1-Butyl-3-methylimmidazolium Chloride Ionic Liquid

Shrestha¹,

Nagib²,

Biddinger³

2015

J. Electrochem. Soc.

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Pd electrodeposition in ionic liquids has been mostly limited to the formation of thin films, which has restricted its potential application to the electronics and decorative industry only. The electrochemical synthesis of nanostructured Pd could broaden its applications to the catalyst industry as well. In 1-butyl-3-methylimmidazolium chloride, the Pd deposits reported so far have had uncontrolled growth without any well-defined morphology. In this study, we report controlled synthesis of Pd nanoparticles with well-defined morphology on pre-etched Ni electrodes. Potentiostatic pulse deposition was used to synthesize these Pd nanoparticles, which had spherical shape and unimodal size distribution. In contrast, thin film-like morphology was deposited during direct electrodeposition. The size of the Pd nanospheres was controlled by controlling the duty cycle; the size of the Pd nanospheres increased from 14.8 ± 3.5 to 30.8 ± 6.6 nm when the duty cycle decreased from 0.5 to 0.2. The size of the Pd nanospheres showed linear dependence on the duty cycle giving excellent control. X-ray diffraction analysis revealed face-centered cubic crystalline microstructure for the Pd particles. The analysis also suggested that the amount of Pd increased by decreasing the duty cycle. The surface of the Pd deposits was dominated by metallic state as revealed by X-ray photoelectron spectroscopy. Electrodeposited Pd has applications as catalysts, interconnects, jewelry and ornaments.1 Electrodeposition has also been considered for recovery of fission palladium.2 Ionic liquids (ILs) are considered promising electrolytes for Pd electrodeposition because hydrogen embrittlement, which is commonly a problem for Pd electrodeposition in aqueous systems, could be avoided by proper choice of IL. Different types of ILs have been studied for this purpose such as chloroaluminates, 20 Some of the work has also been done with the deep eutectic solvents (DES) choline chloride/urea and choline chloride/ethylene glycol.14,21 Pd-containing liquid metal salts (LMS), which are ILs with metal ions coordinated to the cations are also being explored for Pd electrodeposition. 22 However, these works were mostly limited to the study of Pd thin films. This limits the usability of Pd electrodeposition in ILs to the electronic and decorative industry.Controlled synthesis of nanostructures would make Pd electrodeposition in ILs applicable towards heterogeneous catalysis, where catalysts are usually metal nanoparticles. However, controlling size, shape and distribution of metal nanostructures are not straightforward in either aqueous-based solutions or ILs. Although significant progress has been made in aqueous-based solution regarding the synthesis of Pd nanostructures, the same could not be said for ILs. One of the issues is that the ILs behave differently than that of water; therefore, the knowledge could not be directly transferred from aqueous solutions to ILs. Another prominent issue is that each IL has unique chemistry. Despite these disadvantages, ILs hav...

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Electrodeposition of thick palladium coatings from a palladium(ii)-containing ionic liquid

Cited by 24 publications

References 29 publications

Liquid Nickel Salts: Synthesis, Crystal Structure Determination, and Electrochemical Synthesis of Nickel Nanoparticles

Liquid Nickel Salts: Synthesis, Crystal Structure Determination, and Electrochemical Synthesis of Nickel Nanoparticles

Palladium electrodeposition in 1-butyl-1-methylpyrrolidinium dicyanamide ionic liquid

Size-Controlled Synthesis of Palladium Nanospheres by Pulse Electrodeposition in 1-Butyl-3-methylimmidazolium Chloride Ionic Liquid

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