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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.


XRD patterns of products after the decompositions of the cupric (II) tartrate at different temperatures.
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Fig6: XRD patterns of products after the decompositions of the cupric (II) tartrate at different temperatures.

Mentions: The XRD patterns of the decomposition products at different temperatures are plotted in Figure 6. On the XRD pattern, many characteristic diffraction peaks of cupric tartrate between 13° and 55° are clearly observed, in good agreement with the standard cupric tartrate diffraction pattern (ICDD, PDF file No. 03-065-9743). After heating at 200°C, the diffraction peaks of the floccules and Cu(111) appear on the XRD pattern. As the temperature increases to 250°C, five peaks at 29.6°, 36.5°, 42.4°, 61.4°, and 73.7° are present and are attributed to Cu2O(110), Cu2O(111), Cu2O(220), Cu(111), and Cu(220), respectively. This suggests that the floccules disappear at 250°C. On the XRD pattern of the sample obtained from the decomposition processes at 350°C and 400°C, the peaks assigned to Cu2O(110), Cu2O(111), and Cu2O(220) disappear. It should be noted that there are three peaks 43.3°, 50.5°, and 74.1°, which are due to the Cu metal, on the XRD pattern of the sample formed from decomposition at 400°C. It may caused by the reduction of Cu2O by CO and C2H2 generated from the decomposition of cupric tartrate.Figure 6


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)

XRD patterns of products after the decompositions of the cupric (II) tartrate at different temperatures.
© Copyright Policy - open-access
Related In: Results  -  Collection

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

Fig6: XRD patterns of products after the decompositions of the cupric (II) tartrate at different temperatures.
Mentions: The XRD patterns of the decomposition products at different temperatures are plotted in Figure 6. On the XRD pattern, many characteristic diffraction peaks of cupric tartrate between 13° and 55° are clearly observed, in good agreement with the standard cupric tartrate diffraction pattern (ICDD, PDF file No. 03-065-9743). After heating at 200°C, the diffraction peaks of the floccules and Cu(111) appear on the XRD pattern. As the temperature increases to 250°C, five peaks at 29.6°, 36.5°, 42.4°, 61.4°, and 73.7° are present and are attributed to Cu2O(110), Cu2O(111), Cu2O(220), Cu(111), and Cu(220), respectively. This suggests that the floccules disappear at 250°C. On the XRD pattern of the sample obtained from the decomposition processes at 350°C and 400°C, the peaks assigned to Cu2O(110), Cu2O(111), and Cu2O(220) disappear. It should be noted that there are three peaks 43.3°, 50.5°, and 74.1°, which are due to the Cu metal, on the XRD pattern of the sample formed from decomposition at 400°C. It may caused by the reduction of Cu2O by CO and C2H2 generated from the decomposition of cupric tartrate.Figure 6

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.