铜基碳纳米管复合薄膜电沉积制备工艺

Preparation of copper matrix carbon nanotube composite films

为获得碳纳米管分布均匀且导电性良好的铜基碳纳米管复合材料,用超声辅助搅拌复合电沉积方法制备了Cu/MWCNT复合薄膜.采用扫描电子显微镜(SEM)、四探针电阻率仪等研究了电沉积过程中复合电镀液中碳纳米管浓度、电镀液p H值、脉冲电流密度等各项电沉积工艺参数以及不同退火温度对复合薄膜的组织形貌和电阻率的影响规律.结果表明:改变镀液中碳纳米管含量和电镀液的p H值可以改变镀层中碳纳米管的含量及分布,MWCNTs质量浓度升高到2 g/L时,复合薄膜中MWCNTs的质量分数达2.17%;改变电流密度可以细化镀层组织并改善碳纳米管在镀层中的分布,从而提高镀膜的致密度并降低镀层的电阻率;合适的热处理温度可以改善薄膜结晶度和致密度,并提高导电性.镀液中MWCNTs质量浓度为2 g/L,电镀液p H为2,电流密度为20 A/dm2,电镀时温度在25℃且加入超声辅助搅拌时,所得到的复合镀膜经400℃退火后电阻率最低.

Copper matrix carbon nanotube composite films were fabricated by an electrodeposition process using a copper plating bath containing homogeneously dispersed carbon nanotube with the aid of ultrasonic agitation.The morphologies of the composite films were observed on the scanning electron microscopy（SEM）,the electrical resistance were measured on the four-probe electric resistance meter.Technological parameters on the electrodeposition of copper matrix carbon nanotube composite films such as MWCNTs concentration in bath,p H value and current density are discussed.The MWCNTs concentration in bath and p H value affected the surface and MWCNT content in the composite films.When the MWCNTs concentration was 2 g / L,MWCNT content in the composite films reached a maximum value of 2.17 wt%.The current density affected the microstructure of the composite films and the dispersibility of MWCNTs.The heat treatment temperature affected the crystallinity and conductivity of the films.When the MWCNTs concentration is 2 g / L,while p H value is 2 and current density is about 20 A / dm2,fine grains and MWCNTs well-distributed composite film was obtained.The electrical resistance of composite film was minimized on the annealing temperature at 400 ℃.