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High-purity Cu nanocrystal synthesis by a dynamic decomposition method.

Jian X, Cao Y, Chen G, Wang C, Tang H, Yin L, Luan C, Liang Y, Jiang J, Wu S, Zeng Q, Wang F, Zhang C - Nanoscale Res Lett (2014)

Bottom Line: The growth was found to be influenced by the factors of reaction temperature, protective gas, and time.High crystalline Cu nanocrystals without floccules were obtained from thermal decomposition of cupric tartrate at 271°C for 8 h under Ar.This general approach paves a way to controllable synthesis of Cu nanocrystals with high purity.

View Article: PubMed Central - PubMed

Affiliation: Clean Energy Materials and Engineering Center, School of Energy Science and Engineering, University of Electronic Science and Technology of China, No. 2006, Xiyuan Avenue, West Hi-Tech Zone, Chengdu, 611731, China, jianxian@uestc.edu.cn.

ABSTRACT
Cu nanocrystals are applied extensively in several fields, particularly in the microelectron, sensor, and catalysis. The catalytic behavior of Cu nanocrystals depends mainly on the structure and particle size. In this work, formation of high-purity Cu nanocrystals is studied using a common chemical vapor deposition precursor of cupric tartrate. This process is investigated through a combined experimental and computational approach. The decomposition kinetics is researched via differential scanning calorimetry and thermogravimetric analysis using Flynn-Wall-Ozawa, Kissinger, and Starink methods. The growth was found to be influenced by the factors of reaction temperature, protective gas, and time. And microstructural and thermal characterizations were performed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and differential scanning calorimetry. Decomposition of cupric tartrate at different temperatures was simulated by density functional theory calculations under the generalized gradient approximation. High crystalline Cu nanocrystals without floccules were obtained from thermal decomposition of cupric tartrate at 271°C for 8 h under Ar. This general approach paves a way to controllable synthesis of Cu nanocrystals with high purity.

No MeSH data available.


TEM images of copper particles obtained from the decomposition of cupric tartrate at 271°C under Ar. (a, b) 0.5 h and (c, d) 8 h.
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Fig7: TEM images of copper particles obtained from the decomposition of cupric tartrate at 271°C under Ar. (a, b) 0.5 h and (c, d) 8 h.

Mentions: In this section, we will discuss the effect of the reaction time on the properties of the Cu nanocrystals by fixing the decomposition temperature at 271°C. As shown in Figure 6, the sample produced from the decomposition at 271°C has a higher purity. At the same time, the decomposition temperature, i.e., 271°C, is lower than the temperatures which can induce serious aggregations. From the XRD patterns shown in Figure 6, the sample obtained from the decomposition at 271°C for 8 h is much higher than that obtained decomposition at 271°C for 0.5 h. With quantitative analysis of the sample after decomposition for 0.5 h by HighScore® software, the moral ratio of pure Cu nanocrystals is 93%, while that of Cu2O is 7%. When the decomposition time was elongated to 8 h, Cu2O disappears, as reflected by the XRD patterns plotted in Figure 6. Figure 7a, b, c, d shows the TEM images of the samples from the decomposition at 271°C for 0.5 and 8 h. Lattice fringe with d = 2.1 Å confirms the formation of pure Cu nanocrystals. The floccule stuff is also observed in the products as shown in Figure 7a, which is in agreement with the results of SEM characterization.Figure 7


High-purity Cu nanocrystal synthesis by a dynamic decomposition method.

Jian X, Cao Y, Chen G, Wang C, Tang H, Yin L, Luan C, Liang Y, Jiang J, Wu S, Zeng Q, Wang F, Zhang C - Nanoscale Res Lett (2014)

TEM images of copper particles obtained from the decomposition of cupric tartrate at 271°C under Ar. (a, b) 0.5 h and (c, d) 8 h.
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC4493849&req=5

Fig7: TEM images of copper particles obtained from the decomposition of cupric tartrate at 271°C under Ar. (a, b) 0.5 h and (c, d) 8 h.
Mentions: In this section, we will discuss the effect of the reaction time on the properties of the Cu nanocrystals by fixing the decomposition temperature at 271°C. As shown in Figure 6, the sample produced from the decomposition at 271°C has a higher purity. At the same time, the decomposition temperature, i.e., 271°C, is lower than the temperatures which can induce serious aggregations. From the XRD patterns shown in Figure 6, the sample obtained from the decomposition at 271°C for 8 h is much higher than that obtained decomposition at 271°C for 0.5 h. With quantitative analysis of the sample after decomposition for 0.5 h by HighScore® software, the moral ratio of pure Cu nanocrystals is 93%, while that of Cu2O is 7%. When the decomposition time was elongated to 8 h, Cu2O disappears, as reflected by the XRD patterns plotted in Figure 6. Figure 7a, b, c, d shows the TEM images of the samples from the decomposition at 271°C for 0.5 and 8 h. Lattice fringe with d = 2.1 Å confirms the formation of pure Cu nanocrystals. The floccule stuff is also observed in the products as shown in Figure 7a, which is in agreement with the results of SEM characterization.Figure 7

Bottom Line: The growth was found to be influenced by the factors of reaction temperature, protective gas, and time.High crystalline Cu nanocrystals without floccules were obtained from thermal decomposition of cupric tartrate at 271°C for 8 h under Ar.This general approach paves a way to controllable synthesis of Cu nanocrystals with high purity.

View Article: PubMed Central - PubMed

Affiliation: Clean Energy Materials and Engineering Center, School of Energy Science and Engineering, University of Electronic Science and Technology of China, No. 2006, Xiyuan Avenue, West Hi-Tech Zone, Chengdu, 611731, China, jianxian@uestc.edu.cn.

ABSTRACT
Cu nanocrystals are applied extensively in several fields, particularly in the microelectron, sensor, and catalysis. The catalytic behavior of Cu nanocrystals depends mainly on the structure and particle size. In this work, formation of high-purity Cu nanocrystals is studied using a common chemical vapor deposition precursor of cupric tartrate. This process is investigated through a combined experimental and computational approach. The decomposition kinetics is researched via differential scanning calorimetry and thermogravimetric analysis using Flynn-Wall-Ozawa, Kissinger, and Starink methods. The growth was found to be influenced by the factors of reaction temperature, protective gas, and time. And microstructural and thermal characterizations were performed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and differential scanning calorimetry. Decomposition of cupric tartrate at different temperatures was simulated by density functional theory calculations under the generalized gradient approximation. High crystalline Cu nanocrystals without floccules were obtained from thermal decomposition of cupric tartrate at 271°C for 8 h under Ar. This general approach paves a way to controllable synthesis of Cu nanocrystals with high purity.

No MeSH data available.