In situ thermo‐TOF‐SIMS study of thermal decomposition of zinc acetate dihydrate

Abstract

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) was used for an in situ thermal decomposition study of Zn(CH 3 COO) 2 ·2H 2 O forming ZnO nanoparticles. TOF-SIMS spectra were recorded at regular temperature intervals of 25• C in positive and negative detection modes in a dynamic thermal process.Controlled heating (5 • C min −1 ) of Zn(CH 3 COO) 2 ·2H 2 O was also carried out using thermogravimetric analysis (TGA) in an oxygen atmosphere (20 ml min −1 ). Nearly spherical ZnO nanoparticles with no agglomeration and a narrow size distribution (diameter ∼50 nm) were observed, which were characterized using scanning electron microscopy, transmission electron microscopy and x-ray diffraction. In situ thermo-TOF-SIMS was used to monitor the 64 Zn + and 66 Zn + ion abundances as a function of temperature, which showed a similar profile to that observed for weight loss in TGA during decomposition. Based on the experimental results, a possible decomposition mechanism for the formation of ZnO is proposed.

Mild Synthetic Routes to High‐Surface Zinc Oxide Nanopowders

“…This fact differs from previously obtained results on thermal decomposition of ZAD, in which no weight loss was detected beyond 300-380°C. [11,29,32,33,38,39] Consequently, it could be concluded that the remaining acetate after ZnO synthesis is strongly coordinated to the powder surface, since it requires higher temperatures to be eliminated. Low-temperature nitrogen adsorption-desorption analysis shows that materials obtained by both routes have similar textural characteristics (Figure 5a).…”

Study of a sol–gel precursor and its evolution towards ZnO

“…The sol-gel deposition 2 method 6 is routinely used, but the details of the process are still controversial. Some works demonstrate the huge influence that ambient humidity 7 , precursor 8 or solvent 9 have on the pyrolysis of zinc acetate dihydrate (ZAD) and the subsequent formation of ZnO 10,11,12 . Other reports highlight the appearance of different intermediate compounds, such as hydroxyl-or anhydrous acetates 13 , oxo-acetates 14 or hydrated hydroxyl-acetates 15 when similar ZAD species degrade, giving rise to nanowires 16 , nanobelts 17 or other nanostructures 18,19,20 .…”

Effect of carrier gas species and flow rates on the properties of ZnO thin films prepared by chemical vapor deposition using zinc acetate dihydrate

“…5a-c shows SIMS depth profiles of ZnO films prepared at oxygen flow rate of 0, 40 and 100 sccm, respectively. Since the secondary ion count of ZnO À correlates with natural abundance, negative molecular ion 64 Zn 16 O À is used as the matrix signal [32]. From Fig.…”