Comparative Synthesis of Cu and Cu<sub>2</sub>O Nanoparticles from Different Copper Precursors in an Ionic Liquid or Propylene Carbonate

Esteban, Raquel Marcos; Meyer, Hajo; Kim, Jiyeon; Gemel, Christian; Fischer, Roland A.; Janiak, Christoph

doi:10.1002/ejic.201500969

Cited by 18 publications

(14 citation statements)

References 85 publications

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“…Spherical M‐NPs with narrow size distributions are obtained (Table ). The average diameter for the microwave‐synthesized Ni‐ and Cu‐NPs at 1.0 wt % metal dispersions in [BMIm][BF 4 ] is between 11(±3) and 14(±4) nm, respectively, as observed in previous reports for M‐NPs in this IL . The size and size dispersions of the M‐ and MF 2 ‐NPs from [BMIm][BF 4 ] are summarized in Table .…”

Section: Resultssupporting

confidence: 68%

“…[45] There are only af ew reports on the synthesis of M-NPs in organic carbonates. [46][47][48] Whereas ILs are expensive solvents, organic carbonates, such as PC,are available at low cost. [Tos],o rP C. Quantitative decomposition of the metal amidinates was then achieved by microwave heating after only 10 (IL) or 40 min(PC) by using alow powerof50Wto give an approximate temperatureo f2 40 8Ci nt he reactionm ixture (Scheme 1).…”

Section: Introductionmentioning

confidence: 99%

“…243 °C), is considered a “green solvent” of only low (eco)toxicity, and is completely biodegradable . There are only a few reports on the synthesis of M‐NPs in organic carbonates . Whereas ILs are expensive solvents, organic carbonates, such as PC, are available at low cost.…”

Section: Introductionmentioning

confidence: 99%

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Synthesis of Metal Nanoparticles and Metal Fluoride Nanoparticles from Metal Amidinate Precursors in 1-Butyl-3-Methylimidazolium Ionic Liquids and Propylene Carbonate

et al. 2016

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Decomposition of transition‐metal amidinates [M{MeC(NiPr)2}n] [M(AMD)n; M=MnII, FeII, CoII, NiII, n=2; CuI, n=1) induced by microwave heating in the ionic liquids (ILs) 1‐butyl‐3‐methylimidazolium tetrafluoroborate ([BMIm][BF4]), 1‐butyl‐3‐methylimidazolium hexafluorophosphate ([BMIm][PF6]), 1‐butyl‐3‐methylimidazolium trifluoromethanesulfonate (triflate) ([BMIm][TfO]), and 1‐butyl‐3‐methylimidazolium tosylate ([BMIm][Tos]) or in propylene carbonate (PC) gives transition‐metal nanoparticles (M‐NPs) in non‐fluorous media (e.g. [BMIm][Tos] and PC) or metal fluoride nanoparticles (MF2‐NPs) for M=Mn, Fe, and Co in [BMIm][BF4]. FeF2‐NPs can be prepared upon Fe(AMD)2 decomposition in [BMIm][BF4], [BMIm][PF6], and [BMIm][TfO]. The nanoparticles are stable in the absence of capping ligands (surfactants) for more than 6 weeks. The crystalline phases of the metal or metal fluoride synthesized in [BMIm][BF4] were identified by powder X‐ray diffraction (PXRD) to exclusively Ni‐ and Cu‐NPs or to solely MF2‐NPs for M=Mn, Fe, and Co. The size and size dispersion of the nanoparticles were determined by transmission electron microscopy (TEM) to an average diameter of 2(±2) to 14(±4) nm for the M‐NPs, except for the Cu‐NPs in PC, which were 51(±8) nm. The MF2‐NPs from [BMIm][BF4] were 15(±4) to 65(±18) nm. The average diameter from TEM is in fair agreement with the size evaluated from PXRD with the Scherrer equation. The characterization was complemented by energy‐dispersive X‐ray spectroscopy (EDX). Electrochemical investigations of the CoF2‐NPs as cathode materials for lithium‐ion batteries were simply evaluated by galvanostatic charge/discharge profiles, and the results indicated that the reversible capacity of the CoF2‐NPs was much lower than the theoretical value, which may have originated from the complex conversion reaction mechanism and residue on the surface of the nanoparticles.

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Section: Resultssupporting

confidence: 68%

Section: Introductionmentioning

confidence: 99%

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Synthesis of Metal Nanoparticles and Metal Fluoride Nanoparticles from Metal Amidinate Precursors in 1-Butyl-3-Methylimidazolium Ionic Liquids and Propylene Carbonate

et al. 2016

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“…Besides application in classic solid state chemistry, ILs can be used as reaction media to prepare (oligomeric) metal complexes, metal organic frameworks, coordination polymers [25–35] or cluster compounds incorporating main group elements [36–41] . Within SPP 1708, the synthesis of intermetallic cluster and nanoparticles, [3,42–56] the controlled synthesis of polyanions and cations, [57–61] solvent‐free chalcogenidometal‐containing materials, [62–75] deposition of nanocrystalline materials, [76–80] ionic liquids as precursors for inorganic materials, [81–83] ionic‐liquid‐modified hybrid materials, [84–87] as well as the low‐temperature synthesis of thermoelectric materials [88–92] were investigated. Moreover, theoretical [93–106] and solubility [107–114] aspects during the synthesis process were studied.…”

Section: Introductionmentioning

confidence: 99%

Pseudohalogen Chemistry in Ionic Liquids with Non‐innocent Cations and Anions

et al. 2020

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Within the second funding period of the SPP 1708 “Material Synthesis near Room Temperature”,which started in 2017, we were able to synthesize novel anionic species utilizing Ionic Liquids (ILs) both, as reaction media and reactant. ILs, bearing the decomposable and non‐innocent methyl carbonate anion [CO3Me]−, served as starting material and enabled facile access to pseudohalide salts by reaction with Me3Si−X (X=CN, N3, OCN, SCN). Starting with the synthesized Room temperature Ionic Liquid (RT‐IL) [nBu3MeN][B(OMe)3(CN)], we were able to crystallize the double salt [nBu3MeN]2[B(OMe)3(CN)](CN). Furthermore, we studied the reaction of [WCC]SCN and [WCC]CN (WCC=weakly coordinating cation) with their corresponding protic acids HX (X=SCN, CN), which resulted in formation of [H(NCS)2]− and the temperature labile solvate anions [CN(HCN)n]− (n=2, 3). In addition, the highly labile anionic HCN solvates were obtained from [PPN]X ([PPN]=μ‐nitridobis(triphenylphosphonium), X=N3, OCN, SCN and OCP) and HCN. Crystals of [PPN][X(HCN)3] (X=N3, OCN) and [PPN][SCN(HCN)2] were obtained when the crystallization was carried out at low temperatures. Interestingly, reaction of [PPN]OCP with HCN was noticed, which led to the formation of [P(CN)2]−, crystallizing as HCN disolvate [PPN][P(CN⋅HCN)2]. Furthermore, we were able to isolate the novel cyanido(halido) silicate dianions of the type [SiCl0.78(CN)5.22]2− and [SiF(CN)5]2− and the hexa‐substituted [Si(CN)6]2− by temperature controlled halide/cyanide exchange reactions. By facile neutralization reactions with the non‐innocent cation of [Et3HN]2[Si(CN)6] with MOH (M=Li, K), Li2[Si(CN)6] ⋅ 2 H2O and K2[Si(CN)6] were obtained, which form three dimensional coordination polymers. From salt metathesis processes of M2[Si(CN)6] with different imidazolium bromides, we were able to isolate new imidazolium salts and the ionic liquid [BMIm]2[Si(CN)6]. When reacting [Mes(nBu)Im]2[Si(CN)6] with an excess of the strong Lewis acid B(C6F5)3, the voluminous adduct anion {Si[CN⋅B(C6F5)3]6}2− was obtained.

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“…Transition-metal-nanoparticles (M-NPs) are very important for technological applications in several areas of science and industry, including catalysis, chemical sensors, biocatalysts and nanomaterial technology. [1][2][3][4][5][6][7][8][9] For example, silver (Ag)-nanoparticles (Ag-NPs) are potential building blocks for the creation of new materials with tailored properties for optical 10 and medical applications. [11][12][13] Particularly, Fe-NPs can be used for olefin hydrogenation reactions.…”

Section: Introductionmentioning

confidence: 99%

Use of a 4,5-dicyanoimidazolate anion based ionic liquid for the synthesis of iron and silver nanoparticles

et al. 2016

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Sixteen new ionic liquids (ILs) with tetraethylammonium, 1-butyl-3-methylimidazolium, 3-methyl-1-octylimidazolium and tetrabutylphosphonium cations paired with 2-substituted 4,5-dicyanoimidazolate anions (substituent at C2 = methyl, trifluoromethyl, pentafluoroethyl, N,N'-dimethyl amino and nitro) have been synthesized and characterized by using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA). The effects of cation and anion type and structure of the resulting ILs, including several room temperature ionic liquids (RTILs), are reflected in the crystallization, melting points and thermal decomposition of the ILs. ILs exhibited large liquid and crystallization ranges and formed glasses on cooling with glass transition temperatures in the range of -22 to -71 °C. We selected one of the newly designed ILs due to its bigger size, compared to the common conventional IL anion and high electron-withdrawing nitrile group leads to an overall stabilization anion that may stabilize the metal nanoparticles. Stable and better separated iron and silver nanoparticles are obtained by the decomposition of corresponding Fe2(CO)9 and AgPF6, respectively, under N2-atmosphere in newly designed nitrile functionalized 4,5-dicyanoimidazolate anion based IL. Very small and uniform size for Fe-nanoparticles of about 1.8 ± 0.6 nm were achieved without any additional stabilizers or capping molecules. Comparatively bigger size of Ag-nanoparticles was obtained through the reduction of AgPF6 by hydrogen gas. Additionally, the AgPF6 precursor was decomposed under microwave irradiation (MWI), fabricating nut-in-shell-like, that is, core-separated-from-shell Ag-nano-structures.

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Comparative Synthesis of Cu and Cu₂O Nanoparticles from Different Copper Precursors in an Ionic Liquid or Propylene Carbonate

Cited by 18 publications

References 85 publications

Synthesis of Metal Nanoparticles and Metal Fluoride Nanoparticles from Metal Amidinate Precursors in 1-Butyl-3-Methylimidazolium Ionic Liquids and Propylene Carbonate

Synthesis of Metal Nanoparticles and Metal Fluoride Nanoparticles from Metal Amidinate Precursors in 1-Butyl-3-Methylimidazolium Ionic Liquids and Propylene Carbonate

Pseudohalogen Chemistry in Ionic Liquids with Non‐innocent Cations and Anions

Use of a 4,5-dicyanoimidazolate anion based ionic liquid for the synthesis of iron and silver nanoparticles

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Comparative Synthesis of Cu and Cu2O Nanoparticles from Different Copper Precursors in an Ionic Liquid or Propylene Carbonate

Cited by 18 publications

References 85 publications

Synthesis of Metal Nanoparticles and Metal Fluoride Nanoparticles from Metal Amidinate Precursors in 1-Butyl-3-Methylimidazolium Ionic Liquids and Propylene Carbonate

Synthesis of Metal Nanoparticles and Metal Fluoride Nanoparticles from Metal Amidinate Precursors in 1-Butyl-3-Methylimidazolium Ionic Liquids and Propylene Carbonate

Pseudohalogen Chemistry in Ionic Liquids with Non‐innocent Cations and Anions

Use of a 4,5-dicyanoimidazolate anion based ionic liquid for the synthesis of iron and silver nanoparticles

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Comparative Synthesis of Cu and Cu₂O Nanoparticles from Different Copper Precursors in an Ionic Liquid or Propylene Carbonate