Pousaneh Elaheh, Rüffer Tobias, Assim Khaybar, Dzhagan Volodymyr, Noll Julian, Zahn Dietrich R T, Mertens Lutz, Mehring Michael, Schulz Stefan E, Lang Heinrich
Technische Universität Chemnitz, Faculty of Natural Sciences, Institute of Chemistry, Inorganic Chemistry D-09107 Chemnitz Germany
Technische Universität Chemnitz, Faculty of Natural Sciences, Institute of Physics, Semiconductor Physics D-09107 Chemnitz Germany.
RSC Adv. 2018 May 29;8(35):19668-19678. doi: 10.1039/c8ra01851k. eCollection 2018 May 25.
The synthesis and characterization of bis(ketoiminato)magnesium(ii) complexes of composition [Mg(OCRCHCHRNCHCHX)] (X = NMe: 3a, R = R = Me; 3b, R = Me, R = Ph. X = OMe: 3c, R = R = Me) are reported. Complexes 3a-c are accessible by the reaction of C(O)RCHCHRN(H)CHCHX (X = NMe: 1a, R = R = Me; 1b, R = Me, R = Ph. X = OMe: 1c, R = R = Me) with Mg Bu. The structure of 3b in the solid state was determined by a single crystal X-ray diffraction study, confirming that the Mg(ii) ion is hexa-coordinated by two ketoiminato ligands, while each of the latter coordinates with its two N- and one O-donor atom in an octahedral MgNO coordination environment in the -6-33 stereo-isomeric form. The thermal behavior of 3a-c was studied by TG and DSC under an atmosphere of Ar and O respectively. The respective Me-substituted complexes 3a,c decompose at lower temperatures (3a, 166 °C; 3c, 233 °C) than the phenyl derivative 3b (243 °C). PXRD studies indicate the formation of MgO. Additionally, TG-MS studies were exemplarily carried out for 3a, indicating the release of the ketoiminato ligands. Vapor pressure measurements were conducted at 80 °C, whereby 3a,c possess with 5.6 mbar (3a) and 2.0 mbar (3c) significantly higher volatilities than 3b (0.07 mbar). Complexes 3a-c were used as MOCVD precursors for the deposition of thin MgO films on silicon substrates. It was found that only with 3a,c thin, dense and rather granulated MgO layers of thicknesses between 28-147 nm were produced. The as-deposited MgO layers were characterized by SEM, EDX, and XPS measurements and the thicknesses of the as-deposited layers were measured by Ellipsometry and SEM cross-section images. Apart from magnesium and oxygen a carbon content between 3-4 mol% was determined.
报道了组成式为[Mg(OCRCHCHRNCHCHX)]（X = NMe：3a，R = R = Me；3b，R = Me，R = Ph；X = OMe：3c，R = R = Me）的双（酮亚胺基）镁（II）配合物的合成与表征。配合物3a - c可通过C(O)RCHCHRN(H)CHCHX（X = NMe：1a，R = R = Me；1b，R = Me，R = Ph；X = OMe：1c，R = R = Me）与MgBu反应制得。通过单晶X射线衍射研究确定了3b在固态下的结构，证实Mg（II）离子由两个酮亚胺基配体六配位，而每个酮亚胺基配体在 - 6 - 33立体异构形式的八面体MgNO配位环境中通过其两个N供体原子和一个O供体原子配位。分别在Ar和O气氛下通过TG和DSC研究了3a - c的热行为。各自的甲基取代配合物3a、c比苯基衍生物3b（243 °C）在更低温度下分解（3a，166 °C；3c，233 °C）。PXRD研究表明形成了MgO。此外，对3a进行了TG - MS研究示例，表明酮亚胺基配体的释放。在80 °C下进行了蒸气压测量，由此3a、c的蒸气压分别为5.6 mbar（3a）和2.0 mbar（3c），显著高于3b（0.07 mbar）。配合物3a - c用作MOCVD前驱体，用于在硅衬底上沉积MgO薄膜。发现仅使用3a、c可制备出厚度在28 - 147 nm之间的薄、致密且相当颗粒状的MgO层。通过SEM、EDX和XPS测量对沉积后的MgO层进行了表征，并通过椭偏仪和SEM横截面图像测量了沉积层的厚度。除了镁和氧之外，还测定了碳含量在3 - 4 mol%之间。
