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金属学报  2016, Vol. 52 Issue (8): 973-979    DOI: 10.11900/0412.1961.2015.00536
  论文 本期目录 | 过刊浏览 |
添加剂浓度对直流电解沉积纳米孪晶Cu微观结构的影响*
金帅,程钊,潘庆松,卢磊()
中国科学院金属研究所沈阳材料科学国家(联合)实验室, 沈阳 110016
EFFECT OF ELECTROLYTE ADDITIVE CONCEN-TRATION ON MICROSTRUCTURE OF DIRECT-CURRENT ELECTRODEPOSITED NANOTWINNED Cu
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
引用本文:

金帅,程钊,潘庆松,卢磊. 添加剂浓度对直流电解沉积纳米孪晶Cu微观结构的影响*[J]. 金属学报, 2016, 52(8): 973-979.
Shuai JIN, Zhao CHENG, Qingsong PAN, Lei LU. EFFECT OF ELECTROLYTE ADDITIVE CONCEN-TRATION ON MICROSTRUCTURE OF DIRECT-CURRENT ELECTRODEPOSITED NANOTWINNED Cu[J]. Acta Metall Sin, 2016, 52(8): 973-979.

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摘要: 

采用直流电解沉积技术制备出具有高密度择优取向的纳米孪晶结构块体纯Cu样品. 利用XRD, SEM和TEM等手段研究了添加剂浓度对其微观结构的影响. 结果表明, 样品由沿沉积方向生长的微米尺寸柱状晶粒构成, 晶粒内含有高密度孪晶界, 且大部分孪晶界平行于生长表面. 添加剂(明胶)浓度对纳米孪晶Cu的孪晶片层厚度有明显影响, 但对晶粒尺寸影响不大. 无添加剂时, 纯Cu样品中存在微米量级宽大孪晶片层, 当添加剂浓度从0.5 mg/L增加到5 mg/L, 孪晶片层厚度从 150 nm减小至 30 nm, 且孪晶界生长更完整. 其原因是随着添加剂浓度增加, 阴极过电位增大, 孪晶界形核率增加, 从而使孪晶片层厚度减小.

关键词 纳米孪晶Cu直流电解沉积孪晶片层尺寸添加剂    
Abstract

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 wordsnanotwinned Cu    direct-current electrodeposition    twin spacing    electrolyte additive
    
基金资助:*国家自然科学基金项目51420105001, 51371171和51471172及国家重点基础研究发展计划项目2012CB932202资助
图1  不同明胶浓度下直流电解沉积柱状纳米孪晶Cu的XRD谱
图2  不同明胶浓度下直流电解沉积的柱状纳米孪晶Cu表面的SEM像
图3  不同明胶浓度下直流电解沉积的柱状纳米孪晶Cu的截面SEM像
图4  明胶浓度分别为0.5和2 g/L时直流电解沉积柱状纳米孪晶Cu的TEM像及孪晶片层厚度统计
图5  不同明胶浓度时直流电解沉积柱状纳米孪晶Cu的开路电位、恒电流极化及阴极极化曲线
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