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. 2015 Oct:38:278-289.
doi: 10.1016/j.mssp.2015.04.001.

Synthesis and characterization of [Zn(acetate)2(amine)x] compounds (x = 1 or 2) and their use as precursors to ZnO

Jesse S Hyslop  1 , Amanda R Boydstun  1 , Theron R Fereday  1 , Joanna R Rusch  1 , Jennifer L Strunk  1 , Christian T Wall  1 , Cecelia C Pena  1 , Nicholas L McKibben  1 , Jerry D Harris  1 , Aaron Thurber  2 , Alex Punnoose  2 , Jason Brotherton  3 , Pamela Walker  3 , Lloyd Lowe  3 , Blake Rapp  3 , Shem Purnell  3 , William B Knowlton  3 , Seth M Hubbard  4 , Brian J Frost  5
Affiliations

Synthesis and characterization of [Zn(acetate)2(amine)x] compounds (x = 1 or 2) and their use as precursors to ZnO

Jesse S Hyslop et al. Mater Sci Semicond Process. 2015 Oct.

Abstract

As an obvious candidate for a p-type dopant in ZnO, nitrogen remains elusive in this role. Nitrogen containing precursors are a potential means to incorporate nitrogen during MOCVD growth. One class of nitrogen-containing precursors are zinc acetate amines, yet, they have received little attention. The synthesis and single crystal X-ray structure of [Zn(acetate)2(en)], and the synthesis of [Zn(acetate)2(en)2], [Zn(acetate)2(benzylamine)2], [Zn(acetate)2(butylamine)2], [Zn(acetate)2(NH3)2], and [Zn(acetate)2(tris)2], where en = ethylenediamine and tris = (tris[hydroxymethyl]aminomethane) are reported. The compounds were characterized by thermogravimetric analysis and pyrolyzed in air and inert gas to yield ZnO. These compounds are useful single source precursors to ZnO bulk powders by alkali precipitation and ZnO thin films by spray pyrolysis. The amine bound to the zinc influences the ZnO crystal size and shape and acts as a nitrogen donor for preparing nitrogen-doped ZnO during alkali precipitation. Thin films of ZnO prepared by spray pyrolysis using the precursors had a (100) preferred orientation and measured n-type to intrinsic conductivity.

Keywords: ZnO; crystal structure; single source precursors.

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Figures

Figure 1
Figure 1
The rectifying three-point probe technique. a. Three tungsten probes in which Vb is applied at probe 1 and current is measured at probe 2 while V32 is measured at probe 3. b. The circuit representation of the configuration shown in a. c. The applied bias, Vb, versus measured bias at probe 3 relative to probe 2, V32, showing the expected behavior for n-type and p-type semiconductors and data for n-type Si and p-type Si. Adapted from references [41, 42].
Figure 2
Figure 2
Thermal ellipsoid diagram of [Zn(acetate)2(ethylenediamine)] (1). Atoms are represented by ellipsoids at 50% probability.
Figure 3
Figure 3
Thermogravimetric analysis (TGA) curves for the heating of the six chemical precursor to 1000°C in dry air at a rate of 20°C/min. The figure illustrates how the amine bound to the zinc affects the ZnO formation temperature.
Figure 4
Figure 4
Thermogravimetric analysis (TGA) curves for the heating of the six chemical precursor to 1000°C in argon at a rate of 20°C/min.
Figure 5
Figure 5
Powder X-ray diffraction data for the products obtained from the pyrolysis of compounds 1-6 in air.
Figure 6
Figure 6
Powder X-ray diffraction data for the products obtained from the pyrolysis of compounds 1-6 in an inert atmosphere.
Figure 7
Figure 7
Field emission scanning electron microscopy images obtained from the pyrolysis of compounds 1-6 in dry air. The number on the image corresponds to the compound used to produce the material.
Figure 8
Figure 8
Field emission scanning electron microscopy images obtained from the pyrolysis of compounds 1-6 in an inert atmosphere.
Figure 9
Figure 9
Powder X-ray diffraction data for ZnO powders obtained by alkali precipitation of the different precursors at 75°C. Sodium hydroxide was added over the course of 25-30 minutes to precipitate the products. All products were annealed at 200°C for two hours in a nitrogen atmosphere.
Figure 10
Figure 10
Field emission scanning electron microscopy images of ZnO obtained from the alkali precipitation over the course of 30 minutes at 75°C for compounds 1 and 3-6. All samples were annealed at 200°C for two hours under nitrogen.
Figure 11
Figure 11
X-ray powder diffraction of a ZnO thin film grown using [Zn(acetate)2(NH3)2].
Figure 12
Figure 12
Representative conductivity type measurement data from several ZnO thin films – two films exhibit n-type behavior, two exhibit moderate n-type while one shows intrinsic-like behavior. Theoretical lines for n-type and p-type semiconductor are included to help guide the reader.
See this image and copyright information in PMC

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