Synthesis optimization of carbon-supported ZrO2 nanoparticles from different organometallic precursors

• Published in: Journal of nanostructure in chemistry Vol. 7; no. 2; pp. 133 - 147
• Main Authors: Madkikar, Pankaj, Wang, Xiaodong, Mittermeier, Thomas, Monteverde Videla, Alessandro H. A., Denk, Christoph, Specchia, Stefania, Gasteiger, Hubert A., Piana, Michele
• Format: Journal Article
• Language: English
• Published: Berlin/Heidelberg Springer Berlin Heidelberg 01.06.2017; Springer Nature B.V
• Subjects: Carbon; Chemistry; Chemistry and Materials Science; Computer Applications in Chemistry; Heat treatment; Inorganic Chemistry; Mass spectrometry; Nanochemistry; Nanocrystals; Nanoparticles; Optimization; Organic Chemistry; Original Research; Oxidation; Oxygen; Photoelectron spectroscopy; Physical Chemistry; Polymer Sciences; Precursors; Spectroscopic analysis; Thermal decomposition; Thermal stability; Thermogravimetric analysis; Transmission electron microscopy; Tuning; X-ray diffraction; X-rays; Zirconium dioxide; X-ray diffraction; Carbon-supported zirconia nanoparticles; Transmission electron microscopy; Thermogravimetric analysis; X-ray photoelectron spectroscopy
• ISSN: 2008-9244; 2193-8865
• DOI: 10.1007/s40097-017-0225-6

We report here the synthesis of carbon-supported ZrO 2 nanoparticles from zirconium oxyphthalocyanine (ZrOPc) and acetylacetonate [Zr(acac) 4 ]. Using thermogravimetric analysis (TGA) coupled with mass spectrometry (MS), we could investigate the thermal decomposition behavior of the chosen precursors. According to those results, we chose the heat treatment temperatures ( T HT ) using partial oxidizing (PO) and reducing (RED) atmosphere. By X-ray diffraction we detected structure and size of the nanoparticles; the size was further confirmed by transmission electron microscopy. ZrO 2 formation happens at lower temperature with Zr(acac) 4 than with ZrOPc, due to the lower thermal stability and a higher oxygen amount in Zr(acac) 4 . Using ZrOPc at T HT ≥900 °C, PO conditions facilitate the crystallite growth and formation of distinct tetragonal ZrO 2 , while with Zr(acac) 4 a distinct tetragonal ZrO 2 phase is observed already at T HT ≥750 °C in both RED and PO conditions. Tuning of ZrO 2 nanocrystallite size from 5 to 9 nm by varying the precursor loading is also demonstrated. The chemical state of zirconium was analyzed by X-ray photoelectron spectroscopy, which confirms ZrO 2 formation from different synthesis routes.