Zinc–diethanolamine complex: synthesis, characterization, and formation mechanism of zinc oxide via thermal decomposition

• Published in: Journal of sol-gel science and technology 2018-09, Vol.87 (3), p.743-748
• Main Authors: Hayami, Ryohei, Endo, Nagato, Abe, Takayuki, Miyase, Yuta, Sagawa, Takuya, Yamamoto, Kazuki, Tsukada, Satoru, Gunji, Takahiro
• Format: Article
• Language: English
• Subjects: Absorption spectra; Ceramics; Chemical analysis; Chemical synthesis; Chemistry and Materials Science; Composites; Crystal structure; Decomposition reactions; Fourier transforms; Glass; hybrids; Infrared analysis; Infrared spectroscopy; Inorganic Chemistry; Ligands; Materials Science; Nanoparticles; Nanotechnology; Natural Materials; NMR; Nuclear magnetic resonance; Optical and Electronic Materials; Original Paper: Sol–gel; Single crystals; solution chemistries; Spectroscopic analysis; Spectrum analysis; Structural analysis; Thermal decomposition; Wurtzite; Zinc acetate; Zinc oxide; Zinc oxides
• ISSN: 0928-0707; 1573-4846
• DOI: 10.1007/s10971-018-4768-x

Zn(OAc) 2 (H 2 DEA) was synthesized by the reaction of zinc acetate dihydrate (Zn(OAc) 2 •2H 2 O) with diethanolamine (H 2 DEA), and was characterized using single-crystal X-ray structural analysis, nuclear magnetic resonance spectroscopy, Fourier-transform infrared (FT-IR) spectroscopy, and elemental analysis. Zn(OAc) 2 (H 2 DEA) had a trigonal bipyramidal geometry comprised of one zinc atom, two acetate groups, and one H 2 DEA as a neutral tridentate ligand to form two five-membered rings. The states of Zn(OAc) 2 (H 2 DEA) heated at various temperatures were determined by FT-IR spectroscopy. At 270 °C, the H 2 DEA ligand dissociated and was removed. The absorption bands assigned to Zn–O stretching vibration of Zn 4 O core such as the zinc-oxo cluster appeared. When heated at 500 °C, the absorption bands of μ 4 -oxozincate and the acetate group disappeared completely and hexagonal wurtzite structural ZnO was formed at 550 °C. A possible thermal decomposition pathway from Zn(OAc) 2 (H 2 DEA) to ZnO was proposed. The ZnO film was highly transparent and formed by the deposition of ZnO nanoparticles with size ~40 nm. Zn(OAc) 2 (H 2 DEA) was synthesized and characterized. The states of Zn(OAc) 2 (H 2 DEA) heated at various temperatures were determined by FT-IR spectroscopy, and the formation mechanism of ZnO was estimated. Highlights Zinc–diethanolamine complex was synthesized by the reaction of zinc acetate with diethanolamine. Zinc–diethanolamine complex was isolated and characterized. The formation mechanism of ZnO was estimated by FT-IR spectra.