The Preparation and Properties of Volatile Tris(N-Alkoxycarboxamidato)chromium(III) Complexes as Potential Single-Source Precursors for the MOCVD of Crystalline Chromium Oxide Thin Films

Ji Hun Kim, Da Som Song, Sunyoung Shin, Ji Yeon Ryu, Duk Young Jung, Jongsun Lim, Chang Gyoun Kim

Research output: Contribution to journalArticlepeer-review

Abstract

The synthesis, characterization, and vapor-phase growth of volatile Cr(III) complexes as single-source precursors for Cr2O3 thin films are reported. A series of Cr complexes─Cr(mdpa)3 (mdpa = N-methoxy-2,2-dimethylpropanamide) (1), Cr(edpa)3 (edpa = N-ethoxy-2,2-dimethylpropanamide) (2), Cr(empa)3 (empa = N-ethoxy-2-methylpropanamide) (3), and Cr(mpa)3 (mpa = N-methoxypropanamide) (4)─were synthesized via salt elimination reactions between CrCl3·3THF and N-alkoxy carboxamidate salts. These complexes were characterized by Fourier transform infrared spectroscopy, elemental analysis, thermogravimetric analysis (TGA), single-crystal X-ray diffraction (SC-XRD), Hirshfeld surface analysis, powder X-ray diffraction (PXRD), and vapor pressure measurement. The crystal structure of complex 1 revealed a distorted octahedral geometry with a κ2 (O,O) binding mode. TGA demonstrated that complex 1 underwent weight loss at 132 °C and no residue remained at 500 °C. The enthalpy of vaporization of 1 was estimated to be 25.58 kJ/mol, making it an optimal precursor for Cr2O3 thin films. The XRD patterns of Cr2O3 films deposited on SiO2/Si substrates confirmed their crystalline nature, showing prominent peaks at 2θ = 33.5° and 41.5°. In addition, X-ray photoelectron spectroscopy validated the target Cr/O ratio, supporting the successful formation of Cr2O3 films.

Original languageEnglish
Pages (from-to)21519-21528
Number of pages10
JournalACS Omega
Volume10
Issue number21
DOIs
StatePublished - 3 Jun 2025

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