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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Monitoring the formation of carbide crystal phases during the thermal decomposition of 3d transition metal dicarboxylate complexes
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Monitoring the formation of carbide crystal phases during the thermal decomposition of 3d transition metal dicarboxylate complexes

机译:在3d过渡金属二羧酸盐配合物热分解过程中监测碳化物晶相的形成

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Single molecule precursors can help to simplify the synthesis of complex alloys by minimizing the amount of necessary starting reagents. However, single molecule precursors are time consuming to prepare with very few being commercially available. In this study, a simple precipitation method is used to prepare Fe, Co, and Ni fumarate and succinate complexes. These complexes were then thermally decomposed in an inert atmosphere to test their efficiency as single molecule precursors for the formation of metal carbide phases. Elevated temperature X-ray diffraction was used to identify the crystal phases produced upon decomposition of the metal dicarboxylate complexes. Thermogravimetric analysis coupled with an infrared detector was used to identify the developed gaseous decomposition products. All complexes tested showed a reduction from the starting M~(2+) oxidation state to the M~0 oxidation state, upon decomposition. Also, each complex tested showed CO_2 and H_2O as gaseous decomposition products. Nickel succinate, iron succinate, and iron fumarate complexes were found to form carbide phases upon decomposition. This proves that transition metal dicarboxylate salts can be employed as efficient single molecule precursors for the formation of metal carbide crystal phases.
机译:单分子前体可以通过减少必要的起始试剂的数量来帮助简化复杂合金的合成。但是,单分子前体的制备很耗时,很少有市售的。在这项研究中,一种简单的沉淀方法用于制备富马酸铁,钴和镍以及琥珀酸的络合物。然后将这些络合物在惰性气氛中热分解,以测试其作为单分子前体形成金属碳化物相的效率。使用高温X射线衍射来鉴定在金属二羧酸盐配合物分解时产生的晶相。热重分析与红外检测器结合使用,以鉴定所产生的气态分解产物。测试的所有配合物在分解时均显示从起始的M〜(2+)氧化态还原为M〜0氧化态。同样,每种测试的配合物都显示出CO_2和H_2O为气态分解产物。发现琥珀酸镍,琥珀酸铁和富马酸铁络合物在分解时形成碳化物相。这证明过渡金属二羧酸盐可以用作形成金属碳化物晶体相的有效单分子前体。

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