Bis((dialkylamino)alkylselenolato)metal complexes as precursors for microwave-assisted synthesis of semiconductor metal selenide nanoparticles of zinc and cadmium in the ionic liquid [BMIm][ BF4]

Klauke, Karsten; Hahn, Björn; Schütte, Kai; Barthel, Juri; Janiak, Christoph

doi:10.1016/j.nanoso.2015.06.001

Cited by 21 publications

(15 citation statements)

References 62 publications

(70 reference statements)

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“…[15,16] ILs are alternatives to aqueous ando rganic solvents [17,18] and are regarded as an ew liquid medium [19,20] for the preparation of inorganic materials, including M-NPs. [21][22][23][24][25][26][27][28][29] ILs have negligible vapor pressure,h igh thermals tability, high ionic conductivity, ab road liquid-state temperature range, and the ability to dissolve av ariety of materials. [30,31] M-NPsi nI Ls have been prepared from metal salts reduced by H 2 [32][33][34] or without ar eductant, [35] from organometallic metal complexes, [36] including metal carbonyls, [37] throught hermalo rp hotochemical [38] decomposition or by electroreduction/electrodeposition.…”

Section: Introductionmentioning

confidence: 99%

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: Introductionmentioning

confidence: 99%

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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“…The average particle size obtained from TEM images are in good agreement with the estimated crystallite size from the XRD profile results for both CdSe and ZnSe nanoparticles ( Table 2). At 120 kGy, the gamma radiolytic method produced CdSe and ZnSe nanoparticles with larger particle sizes compared to those synthesized by microwave [20] or hydrothermal [21,24] methods. The creation of hydrated electrons by gamma irradiation in the colloidal solution is considered constant for formation of both CdSe and ZnSe nanoparticles, but the particle size of CdSe nanoparticles is greater than that of ZnSe nanoparticles.…”

Section: Elemental Composition Analysis (Edx)mentioning

confidence: 97%

“…Particles in the size range of 2.8-3.0 nm with a band gap range of 2.76-2.95 eV have been prepared by the chemical method [19]. The microwave radiation method can produce larger particles in the size range of 10 to 19 nm with a narrow band gap of approximately 1.79 eV [20]. CdSe nanoparticles with sizes of 43 nm and a narrow band gap of 1.75 eV were prepared by the hydrothermal method [21].…”

Section: Introductionmentioning

confidence: 99%

“…CdSe nanoparticles with sizes of 43 nm and a narrow band gap of 1.75 eV were prepared by the hydrothermal method [21]. However, the narrow size ZnSe nanoparticles of approximately 4 nm with a band gap of 3.3 eV were fabricated using the microwave method [20]. ZnSe nanoparticles of 5.14 nm with a band gap of 3.2 eV have been prepared using the micro emulsion method [22].…”

Section: Introductionmentioning

confidence: 99%

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Formation of a Colloidal CdSe and ZnSe Quantum Dots via a Gamma Radiolytic Technique

et al. 2016

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Abstract:Colloidal cadmium selenide (CdSe) and zinc selenide (ZnSe) quantum dots with a hexagonal structure were synthesized by irradiating an aqueous solution containing metal precursors, poly (vinyl pyrrolidone), isopropyl alcohol, and organic solvents with 1.25-MeV gamma rays at a dose of 120 kGy. The radiolytic processes occurring in water result in the nucleation of particles, which leads to the growth of the quantum dots. The physical properties of the CdSe and ZnSe nanoparticles were measured by various characterization techniques. X-ray diffraction (XRD) was used to confirm the nanocrystalline structure, energy-dispersive X-ray spectroscopy (EDX) was used to estimate the material composition of the samples, transmission electron microscopy (TEM) was used to determine the morphologies and average particle size distribution, and UV-visible spectroscopy was used to measure the optical absorption spectra, from which the band gap of the CdSe and ZnSe nanoparticles could be deduced.

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“…ILs are alternatives to aqueous or organic solvents, [3,4] and are regarded as a new liquid medium [5,6] for the preparation of inorganic materials. [7][8][9][10][11][12][13][14] Ionic liquids are stable at high temperatures, have no vapor pressure and a high ionic conductivity. [15][16][17] Contrary to common organic solvents they are not flammable.…”

Section: Introductionmentioning

confidence: 99%

Anion Analysis of Ionic Liquids and Ionic Liquid Purity Assessment by Ion Chromatography

Rutz

Schmolke

Gvilava

et al. 2017

Zeitschrift anorg allge chemie

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The simultaneous determination of halide impurities (fluoride, chloride, bromide, and iodide) and ionic liquid (IL) anions (tetrafluoroborate, hexafluorophosphate, and triflimide) using ion chromatography was developed with a basic, non‐gradient ion chromatography system. The non‐gradient method uses the eluent Na2CO3/NaHCO3 in water/acetonitrile (70:30 v:v) on the AS 22 column to enable a rapid and simultaneous analysis of different IL and halide anions within an acceptable run‐time (22 min) and with good resolution R of larger than 2.4, a capacity k′ between 0.4 and 5.1, selectivities α between 1.3 and 2.1, and peak asymmetries As of less than 1.5. Halide impurities below 1 ppm (1 mg·L–1 of prepared sample solution) could be quantified. A range of ionic liquids with tetrafluoroborate [BF4]–, hexafluorophosphate [PF6]–, and bis(trifluoromethylsulfonyl)imide (triflimide) [NTf2]– anions combined with cations based on imidazole, pyridine, and tetrahydrothiophene could be analyzed for their anion purity. The IL‐cations do not influence the chromatographic results. With the analysis of 18 ILs differing in their cation‐anion combination we could prove the general applicability of the described method for the anion purity analysis of ionic liquids with respect to halide ions. The IL‐anion purity of most ILs was above 98 wt %. The highest IL‐anion purity was 99.8 wt %, implying anion impurities of only 0.2 wt %. The used halide anion from the synthesis route was the major anion impurity, yet with chloride also bromide and fluoride (potentially from hydrolysis of [BF4]–) were often detected. When iodide was used, at least chloride but sometimes also bromide and fluoride was present. However, even if the IL‐anion content is above 99 wt %, it does not necessarily indicate an ionic liquid devoid of other impurities. From the IC analysis, one can also deduce a possible cation impurity if one takes into account the expected (calculated) IL‐anion content. A matching experimental and theoretical IL‐anion content excludes, a higher experimental content indicates the presence of residual KBF4, NH4PF6, or LiNTf2 salt from the halide to IL‐anion exchange.

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Bis((dialkylamino)alkylselenolato)metal complexes as precursors for microwave-assisted synthesis of semiconductor metal selenide nanoparticles of zinc and cadmium in the ionic liquid [BMIm][ BF4]

Cited by 21 publications

References 62 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

Formation of a Colloidal CdSe and ZnSe Quantum Dots via a Gamma Radiolytic Technique

Anion Analysis of Ionic Liquids and Ionic Liquid Purity Assessment by Ion Chromatography

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