Heterobimetallic copper–barium complexes for deposition of composite oxide thin films
作者:Asif Ali Tahir、Muhammad Mazhar、Mazhar Hamid、Matthias Zeller、Allen D. Hunter
DOI:10.1039/b823024b
日期:——
Heterobimetallic molecular precursors [Ba(dmap)4Cu4(OAc)6·THF] (1) and [Ba(dmap)4Cu4(TFA)6·THF] (2) [dmap = N,N-dimethylaminopropanolate, OAc = acetate and TFA = trifluoroacetate] for the deposition of bariumâcopper composite oxide thin films, were prepared by the interaction of Ba(dmap)2 with Cu(OAc)2 for 1 and Cu(TFA)2 for 2, in THF. Both heterobimetallic complexes were characterized by melting point, elemental analysis, FT-IR spectroscopy, mass spectrometry and single crystal X-ray diffraction. X-Ray crystallography shows that complex 1 crystallizes in the orthorhombic space groupP212121 with the cell dimensions a = 11.2621(11) Ã
, b = 18.2768(17) Ã
and c = 24.541(2) Ã
, while complex 2 crystallizes in the monoclinic space groupC2/c with a = 23.9288(14) Ã
, b = 19.8564(12) Ã
, c = 25.5925(15) Ã
and β = 112.4390(10)°. Thermal gravimetric analysis shows that both complexes 1 and 2 undergo controlled thermal decomposition at 450 °C and 400 °C, respectively, to give mixed metal oxide composite thin films. Scanning electron microscopy (SEM), energy dispersive X-ray (EDX) and X-ray powder diffraction (XRD) analyses of the thin films suggest the formation of good quality crystalline thin films of BaCuO2âCuO composites from both 1 and 2, with average grain sizes of 105 to 175 nm and 110 to 205 nm, respectively.
双金属分子前体[Ba(dmap)4Cu4(OAc)6·THF] (1) 和 [Ba(dmap)4Cu4(TFA)6·THF] (2) [dmap = N,N-二甲基氨基丙酸盐,OAc = 醋酸盐和 TFA = 三氟乙酸盐] 用于沉积钡-铜复合氧化物薄膜,是通过在 THF 中将 Ba(dmap)2 与 Cu(OAc)2 反应制备得到 1,与 Cu(TFA)2 反应制备得到 2。这两种双金属配合物均通过熔点、元素分析、FT-IR 光谱、质谱和单晶 X 射线衍射进行了表征。X 射线晶体学显示,配合物 1 在正交空间群 P212121 中结晶,晶胞参数 a = 11.2621(11) Å,b = 18.2768(17) Å 和 c = 24.541(2) Å,而配合物 2 在单斜空间群 C2/c 中结晶,a = 23.9288(14) Å,b = 19.8564(12) Å,c = 25.5925(15) Å 和 β = 112.4390(10)°。热重分析显示,两种配合物 1 和 2 分别在 450 °C 和 400 °C 下经历受控热分解,生成混合金属氧化物复合薄膜。扫描电子显微镜 (SEM)、能量色散 X 射线 (EDX) 和 X 射线粉末衍射 (XRD) 分析显示,从 1 和 2 中均形成了高质量的 BaCuO2-CuO 复合晶体薄膜,平均晶粒尺寸分别为 105 至 175 nm 和 110 至 205 nm。