The School of Chemistry and Manchester Materials Center, The University of Manchester, Oxford Road, Manchester, M13 9PL UK.
Inorg Chem. 2010 Sep 20;49(18):8495-503. doi: 10.1021/ic1011204.
The iron(III) complexes of several 1,1,5,5-tetraalkyl-2-thiobiurets [Fe(SON(CN(i)Pr(2))(2))(3) (1), Fe(2)(μ-OMe)(2)(SON(CNEt(2))(2))(2) (2), Fe(SON(CNEt(2))(2))(3) (3), and Fe(SON(CNMe(2))(2))(3) (4)] have been synthesized, and the single-crystal X-ray structures of 1, 2, and 4 have been determined. The magnetic properties of complex 2 as a function of the temperature and field were studied. Thermogravimetric analysis of complexes 1-4 showed the decomposition in one major step to iron sulfide residues. All four complexes were used as single-source precursors for the deposition of iron sulfide thin films by aerosol-assisted chemical vapor deposition. Complex 1 gave hexagonal troilite FeS films with a small amount of tetragonal pyrrhotites Fe(1-x)S at 300 °C, whereas only troilite FeS was deposited at 350, 400, or 450 °C. Complexes 2 and 3 deposited a mixture of hexagonal troilite FeS and cubic pyrite FeS(2) films at all temperatures. Complex 4 deposited very thin films of FeS at all temperatures as troilite. Scanning electron microscopy images of the films deposited from all complexes showed that the morphology consisted of plates, granules, rods, and sheets like crystallites. The size and shapes of these crystallites were dependent on the growth temperature and the precursor used. This is the first time that iron(III) thiobiuret complexes have been used as single-source precursors for iron sulfide thin films.
几种 1,1,5,5-四烷基-2-硫代双缩脲[Fe(SON(CN(i)Pr(2))(2))(3) (1)、Fe(2)(μ-OMe)(2)(SON(CNEt(2))(2))(2) (2)、Fe(SON(CNEt(2))(2))(3) (3)和 Fe(SON(CNMe(2))(2))(3) (4)]的铁(III)配合物已被合成,并确定了 1、2 和 4 的单晶 X 射线结构。研究了配合物 2 随温度和场的磁性。配合物 1-4 的热重分析表明,它们在一个主要步骤中分解为硫化铁残留物。所有四个配合物都被用作气溶胶辅助化学气相沉积法沉积硫化铁薄膜的单源前体。配合物 1 在 300°C 下得到少量四方磁黄铁矿 Fe(1-x)S 的六方硫铁矿 FeS 薄膜,而在 350、400 或 450°C 下仅沉积硫铁矿 FeS。配合物 2 和 3 在所有温度下沉积六方硫铁矿 FeS 和立方黄铁矿 FeS(2)薄膜的混合物。配合物 4 在所有温度下沉积非常薄的 FeS 薄膜,均为硫铁矿。所有配合物沉积的薄膜的扫描电子显微镜图像显示,其形态由板、颗粒、棒和片状类似晶体组成。这些晶体的大小和形状取决于生长温度和所用的前体。这是首次将铁(III)硫代双缩脲配合物用作硫化铁薄膜的单源前体。