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Reactivity of vanadium oxytrichloride with β-diketones and diesters as precursors for vanadium nitride and carbide

机译:氧化钒钒与β-二酮和二酯作为钒钒和碳化物的前体的反应性

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摘要

Vanadium(V) oxytrichloride was reacted with 2,4-pentanedione, diethyl malonate, and diethyl succinate under inert conditions, forming compounds: dichloro(oxo)(2,4-pentanedione) vanadium(V) [1], dichloro(oxo)(diethyl malonate) vanadium(IV) [2] and dichloro(oxo)(diethyl succinate) vanadium(IV) [3]. Compounds 1–3 are coordinated to the vanadium centre through the two carbonyl oxygen atoms of the bidentate ligand. It was determined by X-ray crystallography that the structures of the resulting complexes were significantly different, resulting in a monomeric complex (1), a tetrameric ring (2) and a 1D coordination polymer (3). Following the synthesis and isolation of 1–3, they were tested as precursors for vanadium nitride and vanadium carbide by annealing under nitrogen and argon respectively at 1200 °C for 24 h. The resulting materials were characterised by: XRD, EDS, XPS and TEM. Keywords: Vanadium oxychloride, Precursors, Ester adducts, Vanadium carbide, Vanadium nitride, Hard materials
机译:在惰性条件下与2,4-戊二酮,二乙基丙酯,二乙基亚乙酯和二乙基丁二酸二乙酯反应,形成化合物:二氯(Oxo)(2,4-戊酰胺)钒(V)[1],二氯(Oxo) (丙二酸二甲酯)钒(IV)[2]和二氯(Oxo)(琥珀酸二乙酯)钒(IV)[3]。化合物1-3通过双齿配体的两个羰基氧原子与钒中心配位。通过X射线晶体测定,所得复合物的结构显着不同,得到单体复合物(1),四聚体环(2)和1D配位聚合物(3)。在合成和分离为1-3之后,通过在1200℃下分别在氮气和氩气下退火进行氮化钒和碳化钒的前体进行测试,以在1200℃下进行24小时。所得材料的特征在于:XRD,EDS,XPS和TEM。关键词:氯氧化钒,前体,酯加合物,碳化钒,氮化钒,硬质材料

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