Solvothermal Preparation and Characterization of Nano-nickel Oxide
Received date: 2019-01-19
Online published: 2019-04-22
Supported by
Project supported by the National Natural Science Foundation of China (No. 61774169), Scientific Research Foundation for the Returned overseas Chinese Scholar, Natural Science Foundation of Hunan Province (2016JJ3140) and Undergraduate student of Central South University (ZY20180866,202321009).
Nano-scale nickel oxide materials were prepared by solvothermal method using nickel acetylacetonate, oleic acid and oleylamine as raw materials, octadecene as solvent and polyvinylpyrrolidone as surfactant. The effects of the ratio of reactants ratio, insulation time, surfactant and the mass of oleylamine on the microstructure, particle size, morphology, optics and catalytic properties of the product were investigated by X-ray diffraction (XRD), transmission electron microscope (TEM), ultraviolet-visible spectroscopy (UV-Vis) spectral analysis, and Tafel test. The specific experimental operations were:the oleic acid (OA) and 1-octadecene (ODE) was added into four flasks (500 mL) with heating and stirring. Nickel acetylacetonate was added when the temperature raise to 50℃, then continuously stirring for 60 minutes at 120℃ before a certain amount of oleylamine (OAm) was added to the reaction system. The mixed solution was poured into the inner liner of the high temperature reactor. The reactor was covered and transferred to the electro-thermostatic blast oven for a period of time and then cooled to room temperature. The main research results were obtained:(1) The boundary of the original particles became smoothed after sintering, and the spherical particles become flake-shaped which might be attributed to the residual organic covering so the size of nickel oxide nanoparticles changed from the original 40~45 nm to 30~40 nm. (2) With the addition of PVP, the content of NiO phase increased and the particle size was controlled within 40~45 nm. The UV-Vis test showed that NiO belonged to direct band gap and the band gap width was 3.5~3.7 eV. (3) The Tafel analysis showed that the best catalytic activity with exchange current density J0 was 1.23×10-2 mA·cm-2, where pure NiO could be obtained when the reactant ratio of n[Ni(acac)2]:n(OA)=1:2, the additive PVP mass fraction was of 1.66%, the amount of oleylamine was of 30 mmol, and the temperature was of 200℃ for 8 h.
Chen Tian , Yang Ying , Zhao Wanyu , Pan Dequn , Zhu Congtan , Lin Feiyu , Guo Xueyi . Solvothermal Preparation and Characterization of Nano-nickel Oxide[J]. Acta Chimica Sinica, 2019 , 77(5) : 447 -454 . DOI: 10.6023/A19010033
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