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Acta Metall Sin  2016, Vol. 52 Issue (8): 973-979    DOI: 10.11900/0412.1961.2015.00536
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Shuai JIN,Zhao CHENG,Qingsong PAN,Lei LU()
Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
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Nanotwinned metals have attracted widespread attentions recently, due to their unique overall properties, such as high strength, considerable ductility, enhanced work hardening and high electrical conductivity. The method of synthesized nanotwinned metals is an essential factor for influencing its application. To date, the direct-current electrodeposition technique is successfully used to fabricate bulk nanotwinned Cu samples. However, many parameters, such as the density of current, additive, the concentration of Cu2+, pH and temperature, influence the formation of nanoscale twins during electrodeposited process. To understand the effect of electrolyte additive on the formation of twins, in this work, gelatin with different concentrations was added into the electrolyte while other parameters are kept invariant. Bulk Cu with preferentially oriented nanoscale twins was synthesized in CuSO4 electrolyte with different concentrations of gelatin. The nanotwinned Cu sample is composed of columnar grains with high density nanoscale coherent twin boundaries, most of them are parallel to the growth surface. It is found that the concentration of the electrolyte addition plays an important role in the twin lamellar spacing of the nanotwinned Cu samples, but has little effect on grain size. No twins or twins with micro-sized spacing are detected in electrodeposited Cu without the electrolyte addition. With the concentration of gelatin increasing from 0.5 mg/L to 5 mg/L, the average twin lamellar thickness of the bulk nanotwinned Cu samples decreased from 150 nm to 30 nm. Twin boundaries also grow longer in grains with the increase of gelatin. This is because that with the increase of the concentration of gelatin, the overpotential of cathode increases and nucleation of twins becomes easier, resulting in the reduction of twin spacing.

Key words:  nanotwinned Cu      direct-current electrodeposition      twin spacing      electrolyte additive     
Fund: Supported by National Natural Science Foundation of China (Nos.51420105001, 51371171 and 51471172) and National Basic Research Program of China (No.2012CB932202)

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Fig.1  XRD spectra of columnar bulk Cu synthesized by direct current deposition with different gelation concentrations
Fig.2  SEM images of surface of the as-deposited columnar Cu under gelatin concentrations of 0.5 mg/L (a), 1 mg/L (b), 2 mg/L (c) and 5 mg/L (d)
Fig.3  Cross-sectional SEM images of the as-deposited columnar Cu under gelatin concentrations of 0.5 mg/L (a), 1 mg/L (b), 2 mg/L (c) and 5 mg/L (d)
Fig.4  Cross-sectional TEM images (a, b) and twin thickness distributions (c, d) of the as-deposited columnar nanotwinned Cu under the gelatin concentrations of 0.5 mg/L (a, c) and 2 mg/L (b, d) (Inset in Fig.4b shows the corresponding SAED pattern)
Fig.5  Open circuit potential (a), constant current polarization (b) and cathodic polarization (c) curves of direct current electrodeposited columnar nanotwinned Cu under different gelatin concentrations
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