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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.


Experimental result andy(α) − αstandard curves of cupric (II) tartrate. Decomposition stage I (a) 5°C ~ 25°C/min and stage II (b) 5°C/min and (c) 10°C ~ 25°C/min.
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Fig4: Experimental result andy(α) − αstandard curves of cupric (II) tartrate. Decomposition stage I (a) 5°C ~ 25°C/min and stage II (b) 5°C/min and (c) 10°C ~ 25°C/min.

Mentions: As shown in Figure 4a, there is a good fitness between the standard curve and the experimental curve for the dehydration stage. This indicates that the kinetic equation of the dehydration stage is G(α) = 1 − (1 − α)1/3 with integral form and f(α) = 3(1 − α)2/3 with differential form, respectively. On the other hand, the experimental curve for the decomposition stage keeps to the accelerated curve and does not fit with the standard curve completely under heating rate of 5°C/min (Figure 4b). The kinetic equation for the decomposition stage may be G(α) = lnα2. Under heating rates of 10°C to 25°C/min (Figure 4c), the experimental curves of the decomposition stage are the decelerated curves and fit well with the standard curve, and the kinetic equation of the decomposition stage should be G(α) = (1 − α)−1.Figure 4


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)

Experimental result andy(α) − αstandard curves of cupric (II) tartrate. Decomposition stage I (a) 5°C ~ 25°C/min and stage II (b) 5°C/min and (c) 10°C ~ 25°C/min.
© Copyright Policy - open-access
Related In: Results  -  Collection

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

Fig4: Experimental result andy(α) − αstandard curves of cupric (II) tartrate. Decomposition stage I (a) 5°C ~ 25°C/min and stage II (b) 5°C/min and (c) 10°C ~ 25°C/min.
Mentions: As shown in Figure 4a, there is a good fitness between the standard curve and the experimental curve for the dehydration stage. This indicates that the kinetic equation of the dehydration stage is G(α) = 1 − (1 − α)1/3 with integral form and f(α) = 3(1 − α)2/3 with differential form, respectively. On the other hand, the experimental curve for the decomposition stage keeps to the accelerated curve and does not fit with the standard curve completely under heating rate of 5°C/min (Figure 4b). The kinetic equation for the decomposition stage may be G(α) = lnα2. Under heating rates of 10°C to 25°C/min (Figure 4c), the experimental curves of the decomposition stage are the decelerated curves and fit well with the standard curve, and the kinetic equation of the decomposition stage should be G(α) = (1 − α)−1.Figure 4

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.