Reactions of MoCl5/MoO2Cl2 with 4-phenylimidazole-2-thiol/2-thiazoline-2-thiol in CH3CNsolvent in 1:1/1:2 molar ratios have been carried out at room temperature. Products obtained MoCl3(C9H7N2S)(CH3CN), [1];MoCl2(C9H7N2S)(CH3CN), [2]; Mo2OCl4(C9H8N2S)2, [3] and Mo4O2Cl12(C9H7N2S)4, [4]; MoO2Cl3(C3H5NS2)2, [5] and Mo2O4Cl3(C3H5NS2)2, [6] have been analyzed and characterizedby elemental analysis, FTIR, 1H NMR and LC-MS techniques. Compounds being moisture and air sensitive, these have been prepared in inert atmosphere using vacuum line and liquid nitrogen cooled traps. Fragments obtained in LC-MS spectra support the formulae derived.
Trimethylsilyldiethylamine Me3SiNEt2 and MoOCl4 (1:1) undergo a free radical redox reaction in CH2Cl2 or Et2O to form MoCl3O(HNEt2). Reduction occurs even in aprotic media like CCl4 and CS2 to give MoV complexes Mo2Cl6O2(N2Et4) and Mo2Cl6O2[(SCNEt2)2S2], respectively. A 2:1 reaction in nonionizing protic solvents undergoes redox cum cleavage to provide MoCl2O(NEt2) (HNEt2) but a reaction at reflux temperature in 1,2‐dichloroethane leads to diethylammonium salt, [Et2NH2][MoCl4O(HNEt2)]. Higher molar reactions (3:1, 4:1) in CH2Cl2 or Et2O are associated with redox reaction as well as oxygen atom abstraction to form de‐oxo MoIV complex MoCl3(NEt2)(HNEt2)2, whereas, a 3:1 reaction in CS2 forms Mo2Cl4O(S2CNEt2)4. Compounds have been characterized by elemental analyses, redox titration, magnetic moment, conductance, infrared, electronic absorption and 1H‐NMR measurements.
In this paper, three kinds of Ni–20Cr coatings were deposited on SA516 substrate steel by cold-sprayed coating technique. Physical properties (such as hardness, surface roughness, and residual stress) and slurry erosion behavior (with impingement angles of 30∘ and 90∘) of cold-sprayed substrates have been evaluated. Moreover, a scanning electron microscope (SEM) examination has been performed to evaluate the morphological characterization of various coatings. It has been found that the residual stresses induced in the coated specimens exhibited compressive nature. Further, micro-hardness and surface roughness was observed to proliferate with the incorporation of titanium carbide (TiC) and rhenium (Re) in Ni–Cr coatings. Micro-hardness for Ni–20Cr+TiC and Ni–20Cr+TiC+Re was observed at 233.67 and 278.9 Hv, respectively, where Surface roughness for Ni–20Cr+TiC and Ni–20Cr+TiC+Re was observed at 9.86 and 11.68[Formula: see text][Formula: see text]m, respectively. All types of Ni–20Cr coatings were quite efficient in reducing the erosion rate of the SA516 steel as compared to uncoated SA516 and most prominent of all was Ni–20Cr+Tic+Re coating. It was observed that at 30∘, weight loss for Ni–20Cr, Ni–20Cr+TiC and Ni–20Cr+TiC+Re was up to 0.00027, 0.00015 and 0.00012 g/mm2, whereas at 90∘, weight loss was for Ni–20Cr, Ni–20Cr+TiC and Ni–20Cr+TiC+Re was up to 0.00024, 0.00014 and 0.00012 g/mm2.
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