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. 2022 Oct;12(10):1099.
doi: 10.3390/catal12101099. Epub 2022 Sep 23.

Zinc-Acetate-Amine Complexes as Precursors to ZnO and the Effect of the Amine on Nanoparticle Morphology, Size, and Photocatalytic Activity

Jerry D Harris  1 , Emily A Wade  1 , Emmaline G Ellison  1 , Cecelia C Pena  1 , Stephen C Bryant  1 , Nicholas L McKibben  1 , Allison J Christy  1 , Kevin O Laughlin  1 , Ashley E Harris  1 , Kenrik V Goettsche  1 , Chad E Larson  1 , Seth M Hubbard  2 , Jonathan E Cowen  3 , Josh Eixenberger  4 , David Estrada  4 , Jennifer R Chase  5
Affiliations

Zinc-Acetate-Amine Complexes as Precursors to ZnO and the Effect of the Amine on Nanoparticle Morphology, Size, and Photocatalytic Activity

Jerry D Harris et al. Catalysts. 2022 Oct.

Abstract

Zinc oxide is an environmentally friendly and readily synthesized semiconductor with many industrial applications. ZnO powders were prepared by alkali precipitation using different [Zn(acetate)2(amine)x] compounds to alter the particle size and aspect ratio. Slow precipitations from 95 °C solutions produced micron-scale particles with morphologies of hexagonal plates, rods, and needles, depending on the precursor used. Powders prepared at 65 °C with rapid precipitation yielded particles with minimal morphology differences, but particle size was dependent on the precursor used. The smallest particles were produced using precursors that yielded crystals with low aspect ratios during high-temperature synthesis. Particles produced during rapid synthesis had sizes ranging from 21-45 nm. The materials were characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, thermogravimetric analysis, BET, and diffuse reflectance. The materials prepared using precursors with less-volatile amines were found to retain more organic material than ZnO produced using precursors with more volatile amines. The amount of organic material associated with the nanoparticles influenced the photocatalytic activity of the ZnO, with powders containing less organic material producing faster rate constants for the decolorizing of malachite green solutions under ultraviolet illumination, independent of particle size. [Zn(acetate)2(hydrazine)2] produced ZnO with the fastest rate constant and was recycled five times for dye degradation studies that revealed minimal to no reduction in catalytic efficiency.

Keywords: alkali precipitation; diffuse reflectance; mass spectrometry; nanoparticles; photocatalyst; surface area; synthesis; thermal analysis.

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Conflict of interest statement

Conflicts of Interest: The authors declare no conflicts of interest.

Figures

Figure 1.
Figure 1.
SEM images of ZnO powders prepared from [Zn(acetate)2(amine)2] precursors at 95°C in an aqueous solution. The precursors used were (A) [Zn(acetate)2(Tris)2], (B) [Zn(acetate)2(2-thiazolamine)2], (C) [Zn(acetate)2(hydrazine)2], and (D) [Zn(acetate)2(ethylenediamine)].
Figure 2.
Figure 2.
A schematic for the synthesis of ZnO from [Zn(acetate)2(amine)x] precursors with rapid addition of NaOH to precipitate the product. This figure was created with BioRender.com.
Figure 3.
Figure 3.
TEM images of ZnO nanoparticles prepared from [Zn(acetate)2(amine)2] precursors in a water/methanol mixture with rapid NaOH addition at 65 °C. Average particle size are given for each materaial. The precursors used were (A) [Zn(acetate)2(Tris)2] (20 ± 4 nm), (B) [Zn(acetate)2(2-thiazolamine)2] (34 ± 9 nm), (C) [Zn(acetate)2(hydrazine)2] (27 ± 7 nm), and (D) [Zn(acetate)2(ethylenediamine)] (45 ± 7 nm).
Figure 4.
Figure 4.
X-ray powder diffraction data for ZnO nanomaterials prepared using [Zn(acetate)2(amine)2] precursors by alkali precipitation in water/methanol solutions at 65°C. The labels are the amine on the precursor during synthesis. The average particle size given is that observed with the TEM measurements.
Figure 5.
Figure 5.
TGA curves showing the percent weight loss during heating for ZnO powders prepared using four different precursors. The amine label by the curve corresponds to the amine used during synthesis of the ZnO.
Figure 6.
Figure 6.
Kubelka–Munk transformed diffuse reflectance spectra of annealed ZnO powders prepared by rapid precipitation. The amine in the legend corresponds to the amine used during the synthesis of each material.
Figure 7.
Figure 7.
Absorption data for the decolorization of malachite green solutions using different zinc oxide photocatalysts prepared by rapid precipitation. The amines used to make the [Zn(acetate)2(amine)2] precursors are identified by the labels in the legend. The ZnO control was prepared using Zn(NO3)2 without added amines. “No ZnO” corresponds to the decolorization of malachite green with no catalyst in solution under UVA illumination.
Figure 8.
Figure 8.
Absorption data of malachite green solutions during photodegradation by ZnO prepared by rapid precipitation. The amines used to make the [Zn(acetate)2(amine)2] precursors are identified by the labels in the legend. R2 values for all of the best fit lines exceed 0.997.
Figure 9.
Figure 9.
Reusability study for ZnO prepared using [Zn(acetate)2(hydrazine)2] under UVA illumination for two hours. A single sample of ZnO decolored five malachite green dye samples with minimal efficiency loss.
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