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Pietsch, T.
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article
Low Temperature Activation of Tellurium and Resource-Efficient Synthesis of AuTe2 and Ag2Te in Ionic Liquids
Abstract
<p>The low temperature syntheses of AuTe<sub>2</sub> and Ag<sub>2</sub>Te starting from the elements were investigated in the ionic liquids (ILs) [BMIm]X and [P<sub>66614</sub>]Z ([BMIm]<sup>+</sup>=1-butyl-3-methylimidazolium; X = Cl, [HSO<sub>4</sub>]<sup>−</sup>, [P<sub>66614</sub>]<sup>+</sup> = trihexyltetradecylphosphonium; Z = Cl<sup>−</sup>, Br<sup>−</sup>, dicyanamide [DCA]<sup>−</sup>, bis(trifluoromethylsulfonyl)imide [NTf<sub>2</sub>]<sup>−</sup>, decanoate [dec]<sup>−</sup>, acetate [OAc]<sup>−</sup>, bis(2,4,4-trimethylpentyl)phosphinate [BTMP]<sup>−</sup>). Powder X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy revealed that [P<sub>66614</sub>]Cl is the most promising candidate for the single phase synthesis of AuTe<sub>2</sub> at 200 °C. Ag<sub>2</sub>Te was obtained using the same ILs by reducing the temperature in the flask to 60 °C. Even at room temperature, quantitative yield was achieved by using either 2 mol % of [P<sub>66614</sub>]Cl in dichloromethane or a planetary ball mill. Diffusion experiments, <sup>31</sup>P and <sup>125</sup>Te-NMR, and mass spectroscopy revealed one of the reaction mechanisms at 60 °C. Catalytic amounts of alkylphosphanes in commercial [P<sub>66614</sub>]Cl activate tellurium and form soluble phosphane tellurides, which react on the metal surface to solid telluride and the initial phosphane. In addition, a convenient method for the purification of [P<sub>66614</sub>]Cl was developed.</p>